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Journal of Aerospace Technology and Management

J. Aerosp. Technol. Manag. Vol 2, N. 2, May Aug. 2010

EDITOR IN CHIEF
Francisco Cristvo Loureno de Melo Institute of Aeronautics and Space (IAE) So Jos dos Campos, SP, Brazil editor@jatm.com.br

EXECUTIVE EDITOR
Ana Marlene Freitas de Morais Institute of Aeronautics and Space (IAE) So Jos dos Campos, SP, Brazil secretary@jatm.com.br

ASSOCIATE EDITORS
Adriana Medeiros Gama Institute of Aeronautics and Space So Jos dos Campos Brazil Ana Cristina Avelar Institute of Aeronautics and Space So Jos dos Campos Brazil Andr Fenili Universidade Federal do ABC Santo Andr Brazil Angelo Pssaro Institute for Advanced Studies So Jos dos Campos Brazil Antonio Fernando Bertachini National Institute for Space Research So Jos dos Campos Brazil Antonio Pascoal DelArco Jr. Institute of Aeronautics and Space So Jos dos Campos Brazil Carlos de Moura Neto Technological Institute of Aeronautics So Jos dos Campos Brazil Cynthia C. Martins Junqueira Institute of Aeronautics and Space So Jos dos Campos Brazil Eduardo Morgado Belo University of So Paulo So Carlos Brazil Elizabeth da Costa Mattos Institute of Aeronautics and Space So Jos dos Campos Brazil Flaminio Levy Neto Federal University of Braslia Braslia Brazil Gilberto Fisch Institute of Aeronautics and Space So Jos dos Campos Brazil Joo Luiz F. Azevedo Institute of Aeronautics and Space So Jos dos Campos Brazil Jos Roberto de Frana Arruda State Universiy of Campinas Campinas Brazil Marcos Pinotti Barbosa Federal University of Minas Gerais Belo Horizonte Brazil Mischel Carmen N. Belderrain Technological Institute of Aeronautics So Jos dos Campos Brazil Paulo Tadeu de Melo Loureno Embraer So Jos dos Campos Brazil Valder Steffen Junior Federal University of Uberlndia Uberlndia Brazil Waldemar de Castro Leite Institute of Aeronautics and Space So Jos dos Campos Brazil

EDITORIAL PRODUCTION
Ana Cristina Camargo SantAnna Glauco da Silva Helena Prado de Amorim Silva Mrcia Maria Ernandes Robles Fracasso

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Editorial Board

EDITORIAL BOARD
Acir Mrcio Loredo Souza Federal University of Rio Grande do Sul Porto Alegre Brazil Adam S. Cumming Defence Science and Technology Laborator Fort Halstead UK Adrian R. Wittwer National University of the Northeast Resistencia Argentine Alain Azoulay Superior School of Eletricity Paris France Alexandre Queiroz Bracarense Federal University of Minas Gerais Belo Horizonte Brazil Antonio Henriques de Araujo Jr State University of Rio de Janeiro Rio de Janeiro Brazil Antonio Srgio Bezerra Sombra Federal University of Cear Fortaleza Brazil Bert Pluymers Catolic University of Leuven Leuven Belgium Carlos Eduardo S. Cesnik University of Michigan Ann Arbor USA Carlos Henrique Marchi Federal University of Paran Curitiba Brazil Charles Casemiro Cavalcante Federal University of Cear Fortaleza Brazil Cosme Roberto Moreira da Silva University of Braslia Braslia Brazil Edson Aparecida de A. Querido Oliveira University of Taubat Taubat Brazil Edson Cocchieri Botelho So Paulo State University Guaratinguet Brazil Fabrice Burel National Institute of Applied Sciences Lion France Fernando Luiz Bastian Federal University of Rio de Janeiro Rio de Janeiro Brazil Francisco Souza Federal University of Uberlndia Uberlndia Brazil Frederic Plourde Superior National School of Mechanics and Aerotechnics Poitiers France Gerson Marinucci Institute for Nuclear and Energy Research So Paulo Brazil Gilson da Silva National Industrial Property Institute Rio de Janeiro Brazil Hazin Ali Al Quresh Federal University of Santa Catarina Florianpolis Brazil Hugo P. Simo Princeton University Princeton USA Joo Amato Neto University of So Paulo So Paulo Brazil Joern Sesterhenn University of Munich Munich Germany Johannes Quaas Max Planck Institute for Meteorology Hamburg Germany John Cater The University of Auckland Auckland New Zealand Jorge Carlos Narciso Dutra Institute of Aeronautics and Space So Jos dos Campos Brazil Jos Alberto Cuminato So Carlos School of Engineering So Carlos Brazil Jos ngelo Gregolin Federal University of So Carlos So Carlos Brazil Jos Atlio Fritz Rocco Technological Institute of Aeronautics So Jos dos Campos Brazil Jos Carlos Gis University of Coimbra Coimbra Portugal Jos Leandro Andrade Campos University of Coimbra Coimbra Portugal Jos Maria Fonte Ferreira University of Aveiro Aveiro Portugal Jos Rubens G. Carneiro Pontifical Catholic University Belo Horizonte Brazil Juno Gallego So Paulo State University Ilha Solteira Brazil Ligia M. Souto Vieira Technological Institute of Aeronautics So Jos dos Campos Brazil Luis Fernando Figueira da Silva Pontifical Catholic University Rio de Janeiro Brazil Luiz Antonio Pessan Federal University of So Carlos So Carlos Brazil Mrcia Barbosa Henriques Mantelli University of Santa Catarina Florianpolis Brazil Maurizio Ferrante Federal University of So Carlos So Carlos Brazil Michael Gaster University of London London UK Mirabel Cerqueira Resende Institute of Aeronautics and Space So Jos dos Campos Brazil Nicolau A.S. Rodrigues Institute for Advanced Studies So Jos dos Campos Brazil Paulo Celso Greco So Carlos School of Engineering So Carlos Brazil Paulo Varoto So Carlos School of Engineering So Carlos Brazil Rita de Cssia L. Dutra Institute of Aeronautics and Space So Jos dos Campos Brazil Roberto Costa Lima Naval Research Institute Rio de Janeiro Brazil Roberto Roma Vasconcelos Institute of Aeronautics and Space So Jos dos Campos Brazil Samuel Machado Leal da Silva Army Technological Center Rio de Janeiro Brazil Selma Shin Shimizu Melnikoff University of So Paulo So Paulo Brazil Tessaleno Devezas University of Beira Interior Covilha Portugal Ulrich Teipel University of Nuremberg Nuremberg Germany Vassilis Theofilis Polytechnic University of Madrid Madrid Spain Vinicius Andr R.Henriques Institute of Aeronautics and Space So Jos dos Campos Brazil Wim P. C. de Klerk TNO Defence Rijswijk The Netherlands
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ISSN 1984-9648 ISSN 2175-9146 (online)

Journal of Aerospace Technology and Management


Vol. 02, N. 02, May. - Aug. 2010

CONTENTS
EDITORIAL 7 Walking toward the success Francisco Cristvo Loureno de Melo TECHNICAL PAPERS 127 137 145 155 163 169 183 Atmospheric flow measurements using the PIV and HWA techniques Pires, L. B. M., Roballo, S. T., Fisch, G., Avelar, A. C., Girardi, R. M., Gielow, R. Estimates of cosmic radiation dose received by aircrew of DCTAs flight test special group Federico, C. A., Pereira, H. H. C., Pereira, M. A., Gonalez, O. L., Caldas, L. V. E. Evaluation of nacelle drag using Computational Fluid Dynamics Trapp, L. G., Argentieri, H. G. Evaluation of crystallization kinetics of poly (ether-ketone-ketone) and poly (ether-ether-ketone) by DSC Vasconcelos, G. C., Mazur, R. L., Botelho, E. C., Rezende, M. C., Costa, M. L. The role of antioxidant on propellant binder reactivity during thermal aging Villar, L. D., Silva, R. F. , Diniz, M. F., Takahashi, M. F. K., Rezende, L. C. Synthesis of a boron modified phenolic resin Kawamoto, A. M., Pardini, L. C., Diniz, M. F., Loureno, V. L., Takahashi, M. F. K. Modeling elastic and thermal properties of 2.5D carbon fiber and carbon/SiC hybrid matrix composites by homogenization method Pardini, L. C., Gregori, M. L. Thermal barrier coating by electron beam-physical vapor deposition of zirconia co-doped with yttria and niobia Almeida, D. S., Cairo, C. A. A., Silva, C. R. M., Nono, M. C. A. Advances of orbital gas tungsten arc welding for Brazilian space applications experimental setup Garcia, J. A. O., Dias (in memoriam), N. S., Lima, G. L., Pereira, W. D. B., Nogueira, N. F. Characterization of titanium welded joints by the orbital gas tungsten arc welding process for aerospace application Garcia, J. A. O., Lima, G. L., Pereira, W. D. B., Guimares, V. A., Moura Neto, C., Paranhos, R. P. R.

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219 225 237

Technology roadmap for development of SiC sensors at plasma processes laboratory Fraga, M. A., Pessoa, R. S., Maciel, H. S., Massi, M., Oliveira, I. C. Analysis of technological innovation strategy for small and medium companies of the aeronautical sector Moraes, M. B., Melo, F. C. L., Oliveira, E. A. A. Q., Cabral, A. S. Proposta de um mtodo para uma atuao pr-ativa na gesto da inovao tecnolgica em uma instituio pblica de pesquisa aeroespacial Proposal of a method to a pro-active action in the technological innovation management in an aerospace public research institution Brando Neto, N., Oliveira, L. H. THESIS ABSTRACTS

247 247 247 248

Launch vehicle guidance algorithm insensitive to the dispersion of burnout time Campelo, S. P. Numerical simulation of the flow field over sounding rockets Farias, F. R. F. Analysis of fabrication and insulations of an S-30 motor case in composite Heitkoetter, R. F. Characterization and simulation of resin flow of VARTM process in the carbon/epoxy composites manufacture Gomes, P. P. Development and characterization of radar absorbing materials based on polypyrrole/epoxy Campos, R. A. M. Synthesis of poly(o-methoxyaniline) in situ with carbon black and its use as radar absorbing materials Souza Pinto, S. DSC methodology developing for high heating rate experiments Braga, C. I. Study of convergence of parameters permittivity and permeability of RAM for X-Band and experimentally obtained from simulation Paula, A. L. Correction of the launcher vehicle attitude profile as function of the apparent velocity Frana, S. M. Real time energy estimation of the third stage of the Brazilian Satellite Launch Vehicle (VLS-1) Netto, E. R. S. Vision-based control of fixed-wing Unmanned Aerial Vehicle for autonomous road-following Souza, J. P. Development and simulation of the embedded logic to the SARA recoverable orbital platform rendezvous and docking maneuvers Gentina, J. INSTRUCTIONS TO THE AUTHOR RESEARCH BRIEFS

248 249 249 249

250 250 251 251

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254 255

The Brazilian sounding rocket VSB-30 Project: 14-X hypersonic vehicle

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Francisco Cristvo Loureno de Melo

Editorial Walking toward the success

Editor in chief editor@jatm.com.br

Early 2009, we presented the first issue of Journal of Aerospace Technology and Management (JATM) after months of hard work and planning. JATM is a techno-scientific publication edited and published by the Institute of Aeronautics and Space (Instituto de Aeronutica e Espao IAE). The magazine is, so far, published every four months and the articles are selected by an Editorial Committee. This Committee is composed by researchers and technologists from IAE and also outside members of the scientific community. The main objective is to present the results of scientific and technological researches, mainly those concerned to the aerospace field, and also to provide interaction among scientific community. This Journal follows the principle of the open access to all researchers in the field. The great receptivity of this Journal has been the main reason for the change of the publishing period from every four to every three months from the next year on. The scientific community is already seeing JATM as an appropriate vehicle for high level discussion on aerospace research. We considered the following important reasons for this change: the site of JATM (www.jatm.com.br) has been accessed, in average, 900 times monthly, from different countries, such as the United States, South Africa, France, Portugal, Germany, India, China and the United Kingdom; the Journal provides public access to all of its contents, following the principle of making free access to research and generate a greater global exchange of knowledge; the amount of articles received has increased every month; the Journal is already indexed in many databases, such as Chemical Abstracts Service (CAS), Directory of Open Access Journals (DOAJ), the e-journal gateway from global literature (J-Gate), portal to free access journals (LiVRE), Google Scholar, Summaries of Brazilian Journals (Sumrios.org), Electronic Journals Library (EZB), Ulrichs Periodicals Directory (Ulrichsweb), China Educational Publications (SOCOL@R) and Sistema Regional de Informacin en Lnea para Revistas Cientficas de Amrica Latina, el Caribe, Espaa y Portugal (Latindex); all the JATM articles contain DOI numbers defined by Crossref.org; JATM is affiliated to Brazilian Association of Scientific Editors (ABEC Brazil).

For the future, some important changes are already being done from this number as such, as the creation of the Associate Editors and renovation of the Editorial Board. These are done for the better quality in evaluating the received articles.

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In quest for the best continues, we know that the work is hard, but we also know that nothing is easy if you want a high level journal. And we know we can get a journal which will be appreciated by the aerospace scientific community. JATM is here to stay and to continue towards the success among other respectable aerospace publications.

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doi:10.5028/jatm.2010.02027410

Luciana Bassi Marinho Pires*

National Institute for Space Research So Jos dos Campos Brazil lupires@uga.edu

Atmospheric flow measurements using the PIV and HWA techniques


Abstract: Alcntara Space Center (ASC) is the Brazilian gate to the space where rockets of different sizes are launched. At ASC there is a relative topographical variation, coastal cliff, which modifies the atmospheric boundary layer characteristics and can cause interference for operations of rockets. In the present work, a simplified model (mock-up) was studied in a wind tunnel. A scale factor of 1:1000 was used and the atmospheric flow was measured using the hot wire anemometer (HWA) and particle image velocimetry (PIV) techniques. Using of HWA it was possible to calculate values of average wind speed and fluctuations in a set of points of the section of tests that representing the region of the ASC. Through these measures, other meteorological parameters that represent the atmospheric flow, such as the friction velocity (u*), the roughness length (z0) from the logarithmic profile and the alpha exponent (a) of the power law were calculated. With the use of the PIVs technique, the streamlines and the vorticity fields were obtained and it was noticed that the vorticity generated downwind of the coastal cliff has a strong turbulence (vorticities around 2000 s-1). A rectangular building (simulating the mobile integration tower) was inserted at the mock-up and the downwind turbulence was similar to the one generated by the coastal cliff. Keywords: Alcantara Space Center, Wind profile, Turbulent intensity, Vorticity, Stream lines.

National Institute for Space Research So Jos dos Campos Brazil suelen.roballo@cptec.inpe.br

Suelen T. Roballo

Institute of Aeronautics and Space So Jos dos Campos Brazil gfisch@iae.cta.br

Gilberto Fisch

Institute of Aeronautics and Space So Jos dos Campos Brazil anacristina@iae.cta.br

Ana Cristina Avelar

Technological Institute of Aeronautics So Jos dos Campos Brazil giradi@ita.br

Roberto da Mota Girardi

National Institute for Space Research So Jos dos Campos Brazil ralf.gielow@cptec.inpe.br *author for correspondence

Ralf Gielow

INTRODUCTION The knowledge of the atmospheric flow at the Space Launch Centers (like Kennedy Space Center the US Space Port, and French Guiana Space Center French/Europe Port) is very important due to its influence on the research & development (R&D) of the rockets. The trajectory, guidance and control of the rockets are influenced by the wind profile, especially near the surface, as well as the wind loads at surface and upper air. Up to a height of 1000 m, 88% of the trajectory corrections are due to the winds, while there are only 3% of wind corrections above 5000 m (Fisch, 1999). Alcntara Space Center (ASC) is the Brazilian gate to the space where rockets are launched and it is located at the north coast of the state of Maranho, close to the Equator. This region has a very special topography, with a smooth surface (ocean) close to a rough surface (continent). At the border there is a step (coastal cliff) with a 50 m of height, as shown in Fig. 1. The launch pad of the rockets is located close to this border (150 m) and it suffers an intense turbulence due to the modification of the wind profile blowing from the ocean to the continent.
Received: 08/06/10 Accepted: 26/07/10 Figure 1: Alcntara coastal cliff.

Although the wind data are usually made at meteorological stations, vertical profile measurements (like an anemometric tower or mast) give a detail of the winds in certain localizations. In general, the characteristics of the wind are divided in four groups: the vertical profiles of wind characteristics, the speed, the turbulence intensity and the spectral turbulence (Liu, 1990). Johnson (2008), for example, made a complete compilation of the main climatic elements that influence rocket launchings in the United States, giving a special attention to the winds (surface and upper air). Kwon, Lee and Sung (2003) made experiment studies using a wind tunnel to analyze the
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atmospheric conditions of the island of Oenaro-Do, where the space center of South Korea is being constructed. The wind tunnels are used by micrometeorology science due to its advantage of controlling the flow, which optimizes the data collection, the sensitivity analysis and the scientific insights. In the recent applications found in the literature using wind tunnels, it can be cited simulations with the coupling between forest and atmosphere (Novak et al., 2000) that analyzed the turbulent structure of the atmosphere within and above canopy, pollutant dispersion fields immersed in obstacles (Mavroidis, Griffiths and Hall, 2003), besides simulation of the air flow for complex topography (Cao and Tamura, 2006). Recently, Abu-Mulawech (2005) carried out a detailed analysis of the influence of the forward facing-step problem related to different heights for a mixed convection (natural and forced). The objective of this work was to study the atmospheric flow in the region of ASC through experiments in wind tunnel. The analysis was performed through the wind profiles, fields of vorticity, streamlines, turbulent intensities and fluctuation of the wind speed in each point of the interest region, using data obtained with the hot wire anemometry (HWA) and the particle image velocimetry (PIV) techniques. The results were obtained from the MSc dissertation of Roballo (2007) and from the PhD thesis of Pires (2009). WIND PROFILES AT NEAR-NEUTRAL CONDITIONS Neutral stability conditions are scarce in the real atmosphere (Arya, 2001). For strong winds with mean hourly wind speed higher than 10.0 m/s, the flow is sufficient turbulent to mix vertically the atmosphere and suppress the thermal (buoyancy) effects (Loredo-Souza, Schettini and Paluch, 2004). At the near neutral conditions, the atmospheric turbulence is purely originated from the wind shear (mechanically driven) and depends on the friction of the surface and the vertical wind shear. This work assumed a neutral stability at ASC due to the strong winds, independently of the hour of day (daily cycle) for both wet and dry conditions (seasonal cycle). A complementary study using a different data set made with sonic anemometer (Magnago, Fisch and Moraes, 2010) confirmed this hypothesis. There are some theoretical and experimental laws to represent the wind profile, like logarithmic and power law, respectively (Arya, 2001). The vertical variation of the mean wind speed (U) up to approximately 100-150 m above a roughness surface can be represented as (Eq. 1):
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u z U ( z ) = * ln k z0

(1)

where: u* is the friction velocity (m/s); k is the Von Karmans constant and assumed to be 0.40; z0 is the roughness aerodynamic length (m). An observational study (Roballo and Fisch, 2008), using a wind tower (70 m height) at ASC, has obtained values of roughness aerodynamic length between the classes 0.0-0.1 m. The friction velocity was in the interval between 0.3 and 0.4 m/s for the wet period and between 0.4-0.5 m/s for the dry period. These results will be compared with the measurements made at the wind tunnel. The power or wall law is defined by the Eq. 2:

U ( zr ) zr = U ( zn ) zn

(2)

where U(z) and U(zr) are mean wind speed equivalent to a height z and a reference height zr, respectively. The value of zr is assumed to be 10 m as it is the value suggested by the World Organization of Meteorology (WMO) to represent the surface wind. The exponent alpha for the observational study by Roballo and Fisch (2008) was found to be in the range of 0.20-0.25 (dimensionless). Usually statistical means and fluctuations are used to represent the turbulent structure, but in this work the concept of the turbulence intensity was used, defined as the ratio between the standard deviation (s) and the mean wind speed (U) (Eq. 3):

I=

s U

(3)

LOCALIZATION OF THE REGION OF THE STUDY The ASC is situated at the village of Alcntara at the north coast of the state of Maranho, at geographic coordinates 219 S, 4422 W, 50 m above sea level and at a distance of 30 km to the city of So Lus. This facility is the main Brazilian Space Center where Satellite Vehicle Launcher (VLS, acronym in Portuguese) and rocket soundings (like SONDA II, SONDA III, VS30, VS40 and VSB-30) were being launched for the last 20 years. Figure 2 shows the respective localization of the ASC, the Mobile Tower

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Atmospheric flow measurements using the PIV and HWA techniques

in Portuguese), constructed for the Plint & Partners LDD Whokingham Bershire England (Serial n TE 44/5065). This wind tunnel is an opened conventional model, subsonic (Fig. 3a). The test sections have the dimensions of 0.46 m x 0.46 m with length of 1.20 m. For the first tests a canal apparatus made by wood was used (with an open lid and internal width of 0.41 m) to allow the fully development of the boundary layer profile (Fig. 3b). The air flow is produced by electric fans with the power of 30 hp. The wind generated in the tunnel is of 33 m/s, approximately equivalent to 120 km/h. The scale in this tunnel is 1:1000.

Figure 2: Geographic localization of ASC, MTI and AT.

Integration (MTI), where the rockets are launched, and the anemometric tower (AT) whose data has been used and compared with the simulations. The climate of Alcntara shows a seasonal rainfall regime divided into two different periods: a wet period from January to June and a dry period from July to December. During the wet period, the precipitation is typically around 200 mm per month, while at the dry season the rainfall is lower than 20 mm per month. The winds are very distinct between both seasons: during the wet season (March is a characteristic month), the winds are weaker and associated with the trade winds. The wind direction is from east up to 5000 m, with wind speed around 7.0 and 8.0 m/s between the levels of 1000 and 3000 m. For the dry season (September), there is a superposition between the trade winds and the sea breeze, producing stronger winds. The direction is from east up to 8000 m height, reaching maximum velocities between 10.0 and 15.0 m/s at 2000 m. The sea breeze is more intense during the dry period because the thermal difference between oceanic and continental surface. The air temperature and humidity do not present seasonality and their values are very typical of the tropics (Fisch, 1999). METODOLOGY The experiments were carried out at the wind tunnel installed at the Professor Kwein Lien Feng Laboratory in the Technological Institute of Aeronautics (ITA, acronym

Figure 3: The wind tunnel (a) and an overview of the wind tunnel with the woody extension (b).

Measurements with hot wire anemometer (HWA) The HWA used was a 5 m tungsten probe constant temperature anemometer (CTA) from Dantec (AN-1005 HWA System) with a sample rate of 1 kHz. There was no spectral information collected during the tests. The uncertainties of the measurements were computed as 0.02 m/s and were described in Roballo (2007).
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At the mock-up developed to represent the atmospheric flow in Alcntara, it was necessary to install few spires in order to simulate the atmospheric wind profile. These spires consist of triangular steel plates, which were positioned in the entrance of measurements chamber and combined with the roughness (a carpet was used) to produce the boundary layer profile for the wind flow (Santa Catarina, 1999). Figure 4 represents a lateral view of the mounted mock-up. It was also possible to observe an apparatus (to represent the coastal cliff) that was inserted after the adjustment of the boundary layer inside the wind tunnel. Some measurements were made without the apparatus step that simulates the coastal cliff in order to adjust the exponent alpha of the power law (Eq. 2) to a value of 0.15. This value is typical of smooth surface, like the ocean (Blesmann, 1973).

The measured heights were controlled by a positioning system which is able to move in three directions. The heights of measurements were: 0.006, 0.01, 0.02, 0.03, 0.04, 0.07, 0.09, 0.11, 0.13, 0.15, 0.17, 0.19 and 0.21 m, and the first six correspond to the levels of AT (Roballo and Fisch, 2008). The maximum speed obtained was close to 22.0 m/s corresponding to a Reynolds number (Re) in the order of 104. The height length considered was 50 m (equivalent to the height of the cliff). Figure 6 represents a schematic design of the measurements. A coordinate system (x,y) was used as a reference system, where the negative x values correspond to the ocean (upwind of the coastal cliff) and the positive x values correspond to the continent (downwind).

Figure 4: Lateral view of the mounted mock-up.

Figure 6: Superior view of the experimental design with the coordinates x (longitudinal) and y (lateral).

After the adjustment of the boundary layer profile, a step apparatus was inserted in order to represent the coastal cliff (Fig. 5). This coastal cliff was positioned at a distance of 1.99 m. In order to fully investigate the role of the coastal cliff in creating turbulence, besides this experiment (Experiment 1), three others experiments (2, 3 and 4) were designed and simulated at the wind tunnel:

Measurements with particle image velocimetry For the second tests, the devices used for the formation of a typical atmospheric profile were: insertion of spires, a screen (0.005 x 0.005 m) and a carpet for fine adjustment. The screen was introduced in order to reduce the length necessary to form the atmospheric profile (AP) to be at the optical access to particle image velocimetry (PIV). Techniques of generation of atmospheric profile in short test section wind tunnel were described by Pires (2009). It was formed at 1.42 m from the screen and with a height approach of 0.20 m. Figure 7 shows a schema of the experimental apparatus used.

Experiment 1

Experiment 2

Experiment 3

Experiment 4

Figure 5: Schematic representation of the experimented models investigated in the wind tunnel.

a) apparatus smooth step (90) Experiment 1; b) apparatus smooth step (70) Experiment 2; c) apparatus smooth step (70) with local vegetation (simulated by woody cubes of 0.003 m) Experiment 3; d) apparatus perpendicular step (90) with local vegetation Experiment 4.
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Figure 7: Experimental apparatus used for the experiments of the AP and of the ASC region.

Experiment 1 (Fig. 5) was reproduced using the technique of PIV. So, the MTI (represented by a wooden block of dimensions 0.01 x 0.01 x 0.05 m) was inserted and it was observed its influence on the turbulence structure. The

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Atmospheric flow measurements using the PIV and HWA techniques

MTI has the same effect in the flow as a building. A study about building amplification factors (BAF) for sources near buildings was carried out by Thompson (1993) in a wind tunnel. BAF are defined as the ratio of the maximum ground-level (or building-surface) concentration observed to the maximum observed for the same source in the absence of the building. This study described a pointsource release of no buoyant material at various positions near isolated rectangular buildings located on flat terrain, where low and high releases were analysed, and concluded that in low releases may be entrained into the buildings highly turbulent flow region and result in high pollutant concentrations on the building surface where building air intakes are located and high releases may result in increased concentrations at ground level downwind of the building as a result of the buildings influence on the mean flow field. The free wind speed (u) ranged from 27 to 30 m/s corresponding to a Re of the order 104 based on the height of the coastal cliff of 40 m. This was the maximum Re values obtained for this wind tunnel. In the atmosphere, the Re is higher basically of the order of 106. Air flow velocity fields were obtained using a two dimensional PIV system. The test section flow was seeded with smoke particles, approximately 0.005 m in diameter, using a Rosco Fog generator. An Nd-YAG, 200 mJ/pulse laser of 532 nm wavelength, was employed to illuminate the flow field. A vertical laser sheet was created using an articulated arm (Fig. 8) and a set of lenses with thickness adjustment of the laser. A 60 mm m diameter Nikkor lens (Nikon) were fitted to 12-bits high-resolution digital camera (HiSense 4M, Dantec Dynamics) that uses a CCD with 2048 x 2048 pixels and a 7.4 m pixel pitch to record the flow field. The instantaneous images were processed using the adaptive-correlation option of the commercial software Flow Manager 4.50.17, developed by Dantec Dynamics. A 32 x 32 pixels interrogation window with 50% overlap and moving average validation was used. The camera and the source of the laser were located in a three axes system positioning. As shown in Fig. 9, for the accomplishment of the measurements with PIV, the mock-up was painted in flat black color in order to minimize the reflections of the laser that intervene with the measurements. The region of the experimental apparatus was isolated to prevent accidents caused by laser reflections and to minimize the influence of the surrounding light in the measurements. RESULTS AND DISCUSSION Figures 10a and b represent, respectively, the profiles of the wind speed and the fluctuation of the wind along

Figure 8: Section of test and articulated arm.

Figure 9: Particle generator and experimental apparatus.

the central line. The heights had been normalized by the height of reference d = 0.21 m, as well as the values of wind speed had been normalized by the wind speed at this height. It is possible to observe that upstream of the step (x < 0, in Fig. 6) the mean of wind profiles had presented characteristics of uniform flow, with low values of fluctuations. In the region of the step (x = 0), it was observed that mean wind flow pattern was disturbed, with the formation of regions with high values of fluctuations. This was mainly observed close to the surface (up to the normalized height of 0.2) and for a longitudinal distance corresponding a height of 200 m from the edge. Figure 11 shows mean flow field of vorticity and velocity obtained from the PIV measurements. The mean vorticity is a measure of the turbulence was computed by (Eq. 4):
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Figure 11: (a) PIV velocity flow field. (b) Mean vorticity flow field. Figure 10: Average velocity profile (a) and fluctuating velocity profiles (b) along the central line obtained with the HWA.

z =

V U x y

(4)

The negative values is for clockwise rotation and positive values for anti-clockwise. It can be observed a separation region on the coastal cliff corner with the formation of a recirculations bubble. For this situation, the Re was 7.5 x 104. The increase of the fluctuation cited above is related to the recirculation region caused by the coastal cliff (Fig. 11a) and the highest fluctuations of the turbulence can be seen through the vorticity field (Fig. 11b), where it is possible to observe negative vorticities values (-2000 s-1), because reverse flow. The turbulent intensity (Eq. 3) was computed for the levels of the anemometric tower (6, 10, 16.3, 28.5, 43 and 70 m) and is shown in Fig. 12. It is possible to observe that I is very high
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close to the surface, especially close to edge, where values of 0.7 at level 1 were reached. There is also a significant decrease of I with height, and at the level 6 (equivalent to 70 m height) the turbulent intensity is around 0.1 for all positions along the central line. The distance of 300 m (upstream of coastal cliff edge) was estimated as the distance where the turbulence originated by the edge disappears. The values of the exponent alpha from the power law were obtained from the linearization of the Eq. 2, which resulted in Eq. 5: log (5)

These values were also obtained by plotting log (U(z)/ U(zr )) against log (z/zr ). The alpha was computed from the adjusted linear regression (angular coefficient). Figure 13 shows an example of the procedure.

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anymore. The values of alpha at x = 200 m are higher than the values founded by Roballo and Fisch (2008), although similar values are obtained at a distance of 300 m. The meteorological parameters (u* and z0) of the logarithmic law (Eq. 1) were also computed and compared with the observations of Roballo and Fisch (2008). The distributions for u* and z0 at the central line (position y = 0) are shown in Figs. 14 and 15, respectively. At the

Figure 12: Turbulence Intensity distribution along the central lane (position y = 0).

Figure 14: Distribution of u*.

Figure 13: Example of the determination of alpha by Eq. 5.

From Table 1, which summarizes the results from all experiments, it is possible to notice that the power law cannot be applied close to the border due to the region of re-circulation. Upstream the coastal cliff (at x = -200 m), all values of alpha were very close. This is an indication that the coastal cliff will not influence this position
Table 1: The alpha values for the central lane

Figure 15: Distribution of z0.

Position (m) x = -200 x = -150 x = -100 x = -50 x = 200 x = 250 x = 300

ALPHA Experiment 1 0.21 0.24 0.31 0.40 0.24 0.24 Experiment 2 0.20 0.24 0.34 0.41 0.46 0.39 0.30 Experiment 3 0.21 0.22 0.36 0.41 0.34 0.27 0.24 Experiment 4 0.22 0.22 0.28 0.41 0.35 0.28 0.28
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position of the edge (x = 0), there is an abrupt decrease of the values of u* and z0 for Experiment 1. For the others experiments, this variation is not so intense due to the higher degree of smoothness from the topography (Experiments 2 and 3) or the inclusion of the vegetation (Experiment 4). The results from the inclusion of the vegetation indicates an increase of the mixture of the vertical transports. The values of z0 at the position 200 m showed very high numbers and this situation can be associated with lower Re of 104 (instead of the typical value of 107 for real atmosphere). This situation (Fig. 12) permits the re-circulation zone to be longer (at the wind tunnel measurements) than it is in reality. At the position x = 300 m from the edge the roughness presents a value of 0.1 m, similar to the observed values obtained by Roballo and Fisch (2008). Table 2 presents the results for u* for all the experiments and the observations. The dimensionless value corresponds the ratio of u* (for experiment values at the wind tunnel as for observation values) with the characteristic velocity in the wind tunnel. This procedure was used with the purpose of to allowing a comparison between observational and the experimental results. The Experiment 2 presented the best agreement between measurements and observations. Figure 16 shows results of PIV measurements with the presence of MTI. It is possible to observe changes in the flow pattern when reaching the MTI, illustrated by the stream lines (Fig. 16a). After the MTI the flow seems to form a von Karman street vortex. The vorticity generated at the coastal cliff (Fig. 16b) has the same intensity of those generated on the MTI (-2000 s-1) and these are the zones of higher turbulence. It is possible to verify that upstream the MTI, the vorticity of flow is of approximately -900 s-1 and that downstream
Table 2: Comparisons of the values of u* for all experiments

Figure 16: (a) stream lines and (b) vorticity with the MTI.

it reaches a positive vorticity in the value of 300 s-1. A similar situation occurs very close to the coastal cliff. The negative vorticity values occurs in the recirculation regions.

Comparison of u* experiment versus observation Wind Tunnel Experiment 1 Experiment 2 Experiment 3 Experiment4 Observations Wet period Dry period

u* (m/s) 1.80 1.20 1.47 1.53 0.3-0.4 0.4-0.5

Characteristic velocity (m/s) 22 22 22 22 8 10

Dimensionless value 0.08 0.05 0.06 0.07 0.04 0.04

Re 6.52 x 104 6.52 x 104 6.52 x 104 6.52 x 104 2.37 x 107 2.92 x 107

Obs.: The magnitude order of the Reynolds number (Re) is lower in the wind tunnel due to reduction of scale of the height of the coastal cliff, which in this case is 0.05 m.
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CONCLUSIONS The HWA technique was proved to be very appropriate for mean wind profiles and fluctuations measurements at the ASC simulation in wind tunnel. Due to the limitation in the wind tunnels velocity, high Re typical of the atmosphere (order of 105 or 106) was not obtained. However, this study developed an initial procedure to understand the atmospheric flow at ASC using wind tunnel, presenting important behaviors such as the displacement, the formation of circulation bubble and the reattachment of the flow on the tunnel surface. With the PIV technique it was possible to get a general view of the flow based on streamlines and vorticity. A modification of the flow when reaching the step (coastal cliff) was verified, as well as the formation of the recirculation region. During the second tests, measurements had been conducted with the simulation of the MTI existing in the ASC, where the rockets are positioned for the launching. An alteration of the flow was observed by the streamlines in the place, forming a von Karman street vortex. The vorticity in the localization of the MTI resulted in the same one that was occurred during the passage of the flow by the coastal cliff. Comparing the results of velocity flow map and mean vorticity obtained with PIV and turbulence intensity values obtained with HWA, it was observed that the highest values of turbulence intensity occurs in the identified flow separation regions and that the lowest turbulence intensity was observed in the free stream regions, as expected. REFERENCES Abu-Mulawech, H.I., 2005, Turbulent mixed convection flow over a forward-facing step the effects of step heights. International Journal of Thermal Sciences, Vol. 44, No 2, pp. 155-162. doi: 10.1016/j.ijthermalsci.2004.08.001. Arya, S.P., 2001, Introduction to micrometeorology, 2nd edition, Elsevier ISE, Maryland Heights, MO, USA, 420 p. Blessmann, J., 1973, Simulao da estrutura do vento natural em um tnel de vento aerodinmico, Ph.D. Thesis, Instituto de Aeronutica e Espao, So Jos dos Campos, SP, Brazil. Cao, S. and Tamura, T., 2006, Experimental study on roughness effects on turbulent boundary layer flow over a two-dimensional steep hill. Journal of Wind Engineering and Industrial Aerodynamics, Vol. 94, No 1, pp. 1-19. doi: 10.1016/j.jweia.2005.10.001.

Fisch, G., 1999, Caractersticas do perfil vertical do vento no Centro de Lanamento de Foguetes de Alcntara (CLA). Revista Brasileira de Meteorologia, Vol. 14, No 1, pp. 11-21. Jonhson, D.L., 2008, Terrestrial environment (climatic) criteria guidelines for use in aerospace vehicle development. (NASA/TM-2008-215633), NASA Marshall Space Flight Center, Huntsville, AL, 472 p. Kwon, K.J., Lee, J.Y., Sung, B., 2003, PIV measurements on the boundary Layer Flow around Naro Space Center, In: Proceedings of the 5th International Symposium on Particle Image Velocimetry, Busan, Korea, pp. 22-24. Liu, H., 1990, Wind engineering: a handbook for structural engineers, Prentice Hall, Upper Saddle River, NJ, USA, 224 p. Loredo-Souza, A.M, Schettini, E.B.C, Paluch, M.J., 2004, Simulao da camada limite atmosfrica em tnel de vento, In: Mler, S.M, Silvestrini, J., Anais da IV Escola de Primavera Transio e Turbulncia, Vol. 4, Porto Alegre, Brazil, pp. 137-163. Magnago, R.O, Fisch, G., Moraes, O.L.L., 2010, Anlise Espectral do Vento no Centro de Lanamento de Alcntara (CLA). Revista Brasileira de Meteorologia, Vol. 25, No 2, in press. Mavroidis, I., Griffiths, R.F., Hall, D.J., 2003, Field and wind tunnel investigations of plume dispersion around single surface obstacles. Atmospheric Environment, Vol. 37, No 21, pp. 2903-2918. doi: 10.1016/S13522310(03)00300-5. Novak, M.D., et al., 2000. Wind tunnel and field measurements of turbulent flow in forests. Part I: Uniformly thinned stands. Boundary Layer Meteorology, Vol. 95, No 3, pp. 457-495. Pires, L.B.M., 2009, Estudo da Camada Limite Interna desenvolvida em falsias com aplicao para o Centro de Lanamento de Alcntara, Ph.D. Thesis, Instituto Nacional de Pesquisas Espaciais, So Jos dos Campos, SP, Brazil, 165p, Available at: <http://urlib.net/sid.inpe.br/ mtc-m18@80/2009/06.22.18.27>. Roballo, S.T., 2007, Estudo do escoamento atmosfrico no Centro de Lanamento de Alcntara (CLA) atravs de medidas de torre anemomtrica e em tnel de vento. (INPE-14824-TDI/1264), Master of Science dissertation, Instituto Nacional de Pesquisas Espaciais, So Jos dos Campos, SP, Brazil, 137 p, Available at: <http://urlib.net/ sid.inpe.br/mtc-m17@80/2007/06.12.18.07>

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Roballo, S.T., Fisch, G., 2008, Escoamento atmosfrico no Centro de Lanamento de Alcntara (CLA): parte I - aspectos observacionais. Revista Brasileira de Meteorologia, Vol. 23, No 4, pp. 510-519. Santa Catarina, M.F., 1999, Avaliao do escoamento no Centro de Lanamento de Foguetes de Alcntara:

estudo em tnel de vento, Relatrio Final de Atividades de Iniciao Cientifica. Instituto Tecnolgico de Aeronutica, So Jos dos Campos, SP, Brazil, 72 p. Thompson, R.S., 1993, Building amplification factors for sources near buildings: a wind-tunnel study. Atmospheric Environment, Vol. 27, No 15, pp. 2313-2325.

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doi: 10.5028/jatm.2010.02025910

Cludio Antonio Federico*

Institute for Advanced Studies So Jos dos Campos Brazil claudiofederico@ieav.cta.br

Heloisa Helena de Castilho Pereira

Institute for Advanced Studies So Jos dos Campos Brazil heloisa@ieav.cta.br

Estimates of cosmic radiation dose received by aircrew of DCTAs flight test special group
Abstract: Aircraft crews are subjected to radiation doses of cosmic origin in the regular exercise of their functions. The present paper gives an estimate of typical doses received by crews of the Flight Test Special Group of DCTA (GEEV) from July 2007 to November 2009. The dose estimates were performed using the CARI-6 and PCAIRE codes and were compared with each other and with values obtained by other authors in other regions of the globe, being analyzed from the standpoint of estimating radiobiological risk. Keywords: Cosmic radiation, Aircrew, Dosimetry.

Marlon Antonio Pereira

Institute for Advanced Studies So Jos dos Campos Brazil marlon@ieav.cta.br

Institute for Advanced Studies So Jos dos Campos Brazil odairl@ieav.cta.br

Odair Llis Gonalez

Institute for Nuclear and Energy Research So Paulo Brazil lcaldas@ipen.br *author for correspondence

Linda Viola Ehlin Caldas

INTRODUCTION Cosmic radiation (CR) is formed by several types of ionizing radiation from external sources to our planet, which interact with the Earths magnetic field, as well as with the components of the atmosphere. The composition of the CR primary field of galactic origin is very heterogeneous, including nuclei (about 98% in total, of which 87% consists of hydrogen, 12% of helium and 1% of heavy nuclei), with a small contribution of electrons and positrons (2%) (Bartlet, 2004). In addition, the contribution of the solar radiation, which is composed of protons, electrons, helium nuclei and electromagnetic radiation, is also presented. CR penetration depends on several factors, including the Earths magnetic field and the attenuation caused by the atmosphere, such that only a part of the incident CR reaches the earths surface, irradiating all living things continuously, including human beings. The particles of cosmic radiation collide with atoms in the atmosphere, causing ionization and losing their energy gradually. The process of energy loss occurs through elastic and inelastic collisions with atomic nuclei, generating a cascade of secondary radiation, as shown in Fig. 1. This secondary radiation includes neutral and charged pi mesons (o and +/-), and anti-protons and anti-neutrons (p and n ), heavy
Received: 24/03/10 Accepted: 20/04/10

mesons (K) and hyperons (Y) (Hartmann, 2005; Oliveira, 2000; Brum, 2004).

Figure 1: Representation of the reactions involved in the interaction of particles of primary cosmic rays with the atmosphere, giving rise to secondary cosmic rays.

The intensity of cosmic radiation, as well as its composition and co-products, depend on the altitude, and, at higher altitudes, the level of dose received due to cosmic radiation is greater than that at lower altitudes, as can be seen in Fig. 2. This altitude effect causes the dose to be much higher than that in other groups of workers due to cosmic radiation

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Figure 2:

Rates of effective dose due to cosmic radiation as a function of altitude (calculated by CARI-6 code for the region of So Jos dos Campos, SP, for January 2008).

This anomaly modifies the way that cosmic radiation interacts with the geomagnetic field and atmosphere. Many studies have been carried out in this region since 1968 using stratospheric balloons with instruments like scintillation counters and others (Martin, 1972; Costa, 1981; Pinto Junior, 1985). Most of these studies focused on geophysics purposes and mainly X-rays, gamma rays and charged particles fluxes were measured in the energy range from a few keV to hundred of keVs for the former ones and more than 7 MeV for the last one. These studies indicate that the SAMA modifies the radiation incidence in higher altitudes, but no modifications are detected in the aviation flight altitudes or lower. For dosimetry studies, it is known that the main dose components in aircrews at flight altitudes are the neutrons generated by the interaction of the cosmic radiation in the atmosphere, followed by the electrons, positrons and proton components (Bartlett, 2004). The energy range of these radiations in flight altitudes varies from 0.023 eV to more than 400 MeV (Federico et al., 2009) for neutrons, from tens of KeV to hundreds of MeV for the electromagnetic cascade and from tens of MeV to hundreds of GeV for the proton component. Also, the flux-to-dose radiation conversion coefficients are highly energy-dependent, varying more than two decades over the range of energy presented at these altitudes, leaving the dose determination highly dependent on the energy spectra of all particles. This wide energy range and dependence increases the importance of complementary studies with dosimetry approach, as it has been done in other countries. Besides the effects of cosmic radiation dose accumulated in the crew, another important effect, which has led to several recent studies, refers to the induction of failures in avionics by cosmic radiation interaction, a matter that will be addressed in a future work. DETERMINATION OF COSMIC RADIATION DOSE IN AIRCRAFT CREWS The complexity of the radiation field to aircrafts flight altitude makes the direct measurement of this field a difficult and expensive work, and few groups dominate this technique in the world. Equipment used for monitoring this type of radiation field must have special characteristics and be well characterized in terms of response to the various types of radiation and of the wide range of energies involved. This equipment characterization should be done in fields that reproduce in whole or in part the fields present in the cosmic radiation at flight altitudes. In addition, in case of lack of access to that type of field, it must be characterized in conventional fields, and the equipment answer should be verified and

incident on aircraft crew members, justifying studies and preventive measures that have multiplied around the world (Noll et al., 1999; Hajek, Berger and Vana, 2004; Spurn et al., 2007). The earths magnetic field also acts as a shield, deflecting the incident particles on the earth. However, there is a strong dependence of deflection on the latitude of incidence. For instance, near the poles, the dose rate, caused by cosmic rays, is two to three times higher than that in equatorial regions (Lewis et al., 2005). This deflection capacity of the particles is determined by a local characteristic of the geomagnetic field called rigidity cut-off. An important difference in the case of Brazil is that most of its area, mainly the east coast, is subjected to the effects of a magnetic anomaly whose geological origin is not fully known yet, called South Atlantic Magnetic Anomaly (SAMA) (Lauriente, Vampola and Gosier, 1995; Costa and Mendes Junior, 2004). According to Fig. 3, one can see the SAMA at an altitude of 10 km, where a large part of Brazil, mainly the east coast, is located near the center of this anomaly.

Figure 3: Earths magnetic field map at 10 km altitude, taken from SPENVIS (2008).
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extrapolated to the fields of cosmic radiation at flight by means of computer simulations. Thus, the use of monitoring as a routine for aircrews, as done in the nuclear industry workers, would be impractical and difficult to be implemented. Although the International Commission on Radiological Protection (ICRP) in its document number 60 (ICRP, 1991) recognizes and recommends the exposure control for the flight professionals critical group, such as pilots and crews, the same is recommended that this may be done through the use of codes that perform a calculation of the estimates based on interaction of cosmic radiation in space environment and atmospheric data. Moreover, the direct measurements should be taken periodically, as recommended by ICRP (1991), to assess and monitor the accuracy and applicability of computational estimates. This same recommendation was maintained and improved in details in the publications of ICRP numbers 75 (ICRP, 1998) and 103 (ICRP, 2008). Moreover, the European Union and Canada have already recognized aircrews as personnel occupationally exposed to ionizing radiation, as explained by Courades (1999), Transport Canada (2001) and Lim and Bagshaw (2009). Brazilian regulatory authorities in the nuclear area (Comisso Nacional de Energia Nuclear CNEN) and in the aeronautical area (Agncia Nacional de Aviao Civil ANAC) have not issued recommendations or standards in this respect yet, although, in both cases, they normally follow the international recommendations. In both cases, contacts of these authors with those authorities indicate a growing interest and concern on this issue. COMPUTATIONAL TOOLS There are several types of computer codes to estimate the dose received by aircrews, which may be based on computer simulations using the Monte Carlo method, the analytical solutions of the transport equation of particles in a material, or solutions provided by empirical function that fits to experimental data. In this study, CARI-6 and PCAIRE codes were used in order to perform dose estimate calculations, and both codes provide the results in terms of the effective dose quantity, which is a limiting quantity, that is, an appropriate quantity to estimate human health risk due to ionizing radiation and can be directly related to the dose limits set by regulatory authorities. The computer code CARI-6 (EURADOS, 2004), prepared by the Federal Aviation Administration (FAA), is based on the LUIN code (OBrien, 1978), which is based on an analytical solution of the general radiation transport

equation for the cosmic radiation field, and it calculates the total dose on the shortest path, considering the geodesic curve between the origin and destination airports. The code is DOS-based and require the user to input the date of the flight, the origin and destination airports, the altitudes and duration of flight at those altitudes and the ascend and descend times. The knowledge about heliocentric potential is necessary as an input for the code, so that the doses are weighted by the solar activity. The heliocentric potential values tabulated by the FAA, which represent the monthly averages, were used in this work. The calculation results are recorded in a text file for further analysis. The PCAIRE code (Lewis et al., 2005) uses a hybrid method composed of a set of fits to experimental ambient dose equivalent measured data, taken with a tissue equivalent proportional counter (TEPC) in a wide range of geomagnetic latitudes and solar cycles. The user is required to input the date of the flight, the origin and destination airports, the altitudes and duration of flight at those altitudes. A great circle route is produced between the two airports and the coordinates and the radiation dose are calculated at every minute of flight by means of an interpolation from an extensive set of data. The conversion of these results in the effective dose is done by the PCAIRE code through a relationship based on FLUKA and LUIN codes calculations. The PCAIRE code is web-based and the results are recorded in a dosimetry report for further analysis. At the time of this study, none of the codes used allowed dose calculations from solar particle events. Such events consist of sporadic emissions of particles due to large solar flares, which, in some cases, may reach the low atmosphere and significantly increase the doses, especially at higher altitudes and low geomagnetic latitudes. As an example, the greatest event of this type occurred on February 23rd 1956, increasing the dose from a normal level of about 10 Sv/h to about 4.5 mSv/h at an altitude of 9 km (Lewis, Green and Bennett, 2009). The sporadic occurrence of such event is one of the factors that highlights the importance of the experimental measurement ability of this type of radiation field. RESULTS This work was performed collecting flight data over a period of two years with the pilots and crews of the Flight Test Special Group (GEEV) of DCTA totalizing 218 flights evaluated. Data were collected through a statement delivered to the crew, which consisted of the following information needed for the evaluation of the estimated doses: origin and destination airports, flight levels, flight duration at each level, ascending and descending time as well as information on the aircraft used.
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Averages of evaluated flight altitudes are presented in the histogram in Fig. 4. According to this figure, most of the GEEV flights are performed in low altitudes, which imply lower cosmic radiation dose rates. Only a few cases of flights were at higher altitudes, with pressurized aircraft. In the case of flights made up of more than one level of altitude, the averages were calculated by weighting the time spent at each level. As the flight level, in most cases, is strongly dependent on the used aircraft, this will ultimately bring great influence on the dose rate received by the crew.

DISCUSSION Altitude dependence Referring to Fig. 6, it is observed that, as expected, there is a strong dependence of the effective dose rate on the average flight altitude. It is important to mention that the approximated effective dose rate was calculated through the quotient of the effective dose by the total flight time duration, including ascending and descending time intervals.

Figure 4: Frequency distribution of the average altitudes of 218 flights evaluated.

Figure 6: Scatterplot with histograms in the margins showing the relationship between the approximated effective dose rate and the average altitude.

The flight data were processed through the CARI-6 and PCAIRE codes, and the effective dose results obtained for each one by the code CARI-6 are presented as a histogram in Fig. 5.

Still referring to Fig. 6, it is clearly noticed that only three flight data greatly differ from the other ones, with values of approximate effective dose rates well above the others. This fact occurs because such flights were held at medium altitudes higher than 10,000 m and were long-term, so that the ascending and descending times do not contribute significantly to total path. Latitude dependence In order to analyze the behavior of the effective dose rate as a function of the latitude, a mean latitude point was calculated between the origin and the final destination for each flight. The effective dose rate in this mean latitudes and respective altitudes was plotted in Fig. 7, where only a slightly effect of latitude can be observed in the range of flights. It is clear that most of the flight data is grouped, thus not contributing so much for this type of evaluation. In the range of the latitude covered by the Brazilian territory (from about 5 N to 30 S), the effect of latitude is more relevant only for high altitudes, as can be seen in Fig. 8, where some calculations are presented for the 45.5 W longitude and latitudes varying from 0 S to 90 S.

Figure 5: Effective dose histogram for the 218 flights evaluated by the CARI-6 code.

Figure 5 shows that most of the flights received low doses, with the average standing at 0.61 Sv and the mode at 0.13 Sv. The highest value, 7.46 Sv, occurred on a flight from high altitude (12,192 m) and longer duration (2h30min).
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Campos (SP) towards Itaituba (PA) for the same month between the years 1995 to 2009, based on the mean heliocentric potential for each year. The anomaly observed in 2000 corresponds to an abnormally high solar activity over the same period in the estimative, which means that the radiation of cosmic origin is expected to decrease due to momentary interaction with the solar field. For the year 2009 and, more recently, in 2010, there was a significant increase in the incidence of radiation resulting from a period of solar minimum that persists with the lowest values of the last century (NASA, 2009).

Figure 7: 3-D view of the calculated effective dose rates as a function of the mean latitude and altitude, where the surface plane was a mean approximation for behavior viewing purposes.

Figure 9: Estimates of effective dose for flights in July from 1995 to 2009, using the CARI-6 code (lower curve) and mean solar potential (uper curve), showing its anticorrelation.

Comparison between the codes The methodological differences between the used codes cause differences between their results, as can be seen in Fig. 10. In most cases, the CARI-6 code underestimates the dose in comparison to that calculated by the PCAIRE code, as reported by other references (EURADOS, 2004). Part of these differences may be due to a fewer resolution

Figure 8: Effect of latitude in dose rates from 0 to 90, for several altitudes. The map is only present for comparison with the latitude range in Brazilian territory.

In Fig. 8, it can be observed that the flights over the pole are subjected to higher dose rates. This is of special interest for crews that make frequent flights over this region, e.g. the crew from FAB traveling to the Brazilian scientific station in Antarctica. Influence of the solar cycle The influence of the solar cycle is of great importance in the effective dose rate at flight altitudes. Figure 9 shows a simulation of a hypothetical flight from So Jos dos

Figure 10: Comparison between results from CARI-6 and PCAIRE codes.
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of the PCAIRE code, which is in units of microsieverts while the CARI-6 code has resolution of decimal of microsieverts leading to high differences as up to one microsievert region, as can be seen in Fig. 11.

and effects of exposure to high doses of radiation. These types of effects are not observable in case of exposure of aircrews to cosmic radiation, which are several orders of magnitude lower than those needed for the occurrence of such effects. In the case of stochastic effects, they are linked to the likelihood of deleterious damage arising from molecular ionization that, in the event of molecules into the cellular DNA, can cause neoplasic changes leading to the occurrence of cancer and hereditary effects, in the case of germ cells. Such effects are typical of exposures at low doses and long exposure periods, such as exposure of aircrews to cosmic radiation. The limitation to the likelihood of deleterious effects is accomplished through effective dose limits established by regulatory agencies based on biostatistics observed in irradiated large populations (such as Hiroshima and Nagasaki) and experiments with animals extrapolated to effects of long exposure in low doses.

Figure 11: CARI-6/PCAIRE code dose ratio as a function of the CARI-6 code dose.

Comparison with other results The doses calculated in this work are within the range of 0.02 Sv to 7.46 Sv for all flights, and the majority of them (93%) is in the range from 0.02 Sv to 2.00 Sv. These values are consistent with those obtained by Tommasino (1999) in routes between Rome and Rio de Janeiro (from 2.0 Sv to 2.4 Sv) which, otherwise, had been subjected to SAMA in only a part of this route and in a lower intensity radiation period also. The majority of the doses obtained in the present study lay bellow the values estimated by FAA for the US flight crew (FAA, 1990) for commercial routes, which varies from 0.2 Sv to 9.5 Sv, but the entire range of our calculated doses is consistent with FAAs range. Furthermore, the majority of the results obtained in this work lay bellow those calculated by Alves and Mairos (2007) for similar military flight crews, which varies from 1.0 Sv to 16.5 Sv. The lower altitudes and geomagnetic location of the flights of GEEV make it difficult to compare with results from other studies that were mostly made in commercial altitudes in North American or European routes. CORRELATION WITH BIOLOGICAL EFFECTS AND DOSE LIMITS Biological effects of ionizing radiation can be divided into two types: deterministic effects and stochastic effects. Deterministic effects are those caused by high doses over short periods of exposure, resulting in the so-called acute radiation syndrome, a set of characteristic symptoms
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This limitation is reflected in the primary limits on annual effective dose, which are established for individuals who usually work with ionizing radiation and have their health and doses monitored, and also for individuals who are not normally exposed, referred to as the public. The primary limits of effective dose, established in Brazil by CNEN and consistent with international recommendations (ICRP, 1991) is 20 mSv per year (averaged on 5 consecutive years) for individuals occupationally exposed and 1 mSv per year for the general public. Epidemiological studies have been conducted since 1990 with the objective of evaluating health risks of aircraft crew members (Blettner and Zeeb, 1999). Although there have been noticeable increases in the incidence of breast cancer in female crews, as well as slightly increased incidence of brain tumors and melanomas in crews of both gender, it is difficult to assess the real origin of those risks since many factors such as variation in the circadian rhythm and UV incidence work together with the incidence of cosmic radiation as possible causes. Special care has to be taken in relation to pregnant female aircrew, since the total dose of the fetus must be kept as low as possible and always below 1 mSv in the whole gestation period. This limitation must be considered in the case of frequent flyer aircrew. CONCLUSIONS The collected data show that the dose varies from 0.02 Sv up to 7.46 Sv per flight. Due to the low frequency of flights, crews which were evaluated are located in a range

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of annual cumulative dose well below the 1mSv annual limit for public individuals. For this work condition, additional controls are not justified for the GEEV aircrew. Likewise, it is possible to see that flights of longer duration and altitude, approaching the condition of commercial flights, can reach and probably exceed cumulative doses of about 8 Sv per flight. This condition implies the possibility of exceeding the annual primary limits for individuals of the public if these crews, for example, carry out more than 125 flights of this type. This frequency is easily exceeded in the case of commercial flight crews. Another aspect to be highlighted concerns the importance of the ability to measure this type of radiation during flights in order to verify and monitor the computer estimates, in accordance to the provisions in the guidelines of the ICRP. This training is being developed within the Institute for Advanced Studies (Federico et al., 2009), and has special importance due to the fact that the codes to estimate doses crews were rarely used and evaluated in confrontation with experimental measurements in the South America region. An evaluation of the codes in this region is particularly important and interesting, mainly due to the existence of the SAMA. ACKNOWLEDGEMENTS The authors are thankful to the GEEV Commander, who allowed and supported the accomplishment of this study; to the crews, who carefully filled the forms with flight data, to the National Counsel of Technological and Scientific Development (CNPq) and FINEP (Financiadora de Estudos e Projetos) for the partial financial support. REFERENCES Alves J. G., Mairos J. C., 2007, In-flight dose estimates for aircraft crew and pregnant female crew members in military transport missions, Radiation Protection Dosimetry, Vol. 125, No 1-4, pp. 433-437. Bartlett D. T., 2004, Radiation protection aspects of the cosmic radiation exposure of aircraft crew, Radiation Protection Dosimetry, Vol. 109, No 4, pp. 349-355. Blettner M., Zeeb H., 1999, Epidemiological studies among pilots and cabin crew, Radiation Protection Dosimetry, Vol. 86, No 4, pp. 269-273. Brum C. G. M., 2004, Variabilidade da absoro de rudo csmico via rimetro e modelagem numrica dos processos associados, PhD Thesis, Instituto Nacional de Pesquisas Espaciais, So Jos dos Campos.

Costa A.M., Mendes Junior O., 2004, Anomalia magntica do atlntico sul e a radiao csmica sobre a costa do Brasil, Scientific American, Brasil, Vol. 2, No 23, p. 20-29 (in Portuguese). Costa J.M., 1981, Particle precipitation and atmospheric x and gama rays in the south atlantic magnetic anomaly by balloon experiments, Instituto de Pesquisas Espaciais, Report INPE-2119-RPE/343, So Jos dos Campos. Courades J.M., 1999, European legislation on protection against cosmic radiation, Radiation Protection Dosimetry, Vol. 86, No 4, pp. 7-24. European Dosimetry Group (EURADOS), 2004, Cosmic radiation exposure of aircraft crew, European Radiation Dosimetry Group Radiation Protection 140 of EURADOS Work Group 5, Directorate-General for Energy and Transport. Federal Aviation Administration (FAA), 1990, Radiation Exposure of Air Carrier Crewmembers, U.S. Department of Transportation, Advisory Circular n. 120-52. Federico, C.A., et al., 2009, Neutron spectra measurements in the south atlantic anomaly region, 11th Neutron and Ion Dosimetry Symposium, Ithemba Labs, Cape Town, South Africa. Hajek, M., Berger, T., Vana, N., 2004, A TLD-based personal dosemeter system for aircrew monitoring, Radiation Protection Dosimetry, Vol. 110, No 1-4, pp. 337-341. Hartmann, G. A., 2005, A anomalia magntica do atlntico sul: causas e efeitos, Master in Science Dissertation, Instituto de Astronomia, Geofsica e Cincias Atmosfricas da Universidade de So Paulo, So Paulo. International Commission on Radiological Protection (ICRP), 1991, Recommendations of the international commission on radiological protection, Annals of the ICRP, Vol. 21, No 1-3. International Commission on Radiological Protection (ICRP), 1998, General principles for the radiation protection of workers, Annals of the ICRP, Vol. 27, No 1. International Commission on Radiological Protection (ICRP), 2008, The 2007 recommendations of the International Commission on Radiological Protection, Annals of the ICRP, Vol. 37, No 2-4. Lauriente M., Vampola A.L., Gosier K., 1995, Experimental validation of south atlantic anomaly motion using a two-dimensional cross-relation technique,

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Workshop of Radiation Belts: Models and Standards, Belgian Institute for Space Aeronomy, Brussels, Belgium. Lewis B. J., et al., 2005, Aircrew dosimetry using predictive code for aircrew radiation exposure (PCAIRE), Radiation Protection Dosimetry, Vol. 116, No 1-4, pp. 320-326. Lewis B. J., Green A.R., Bennett L.G.I., 2009, Effect of Noisy sun conditions on aircrew radiation exposure, Advances in Space Research, Vol. 44, pp. 184-189. Lim M.K., Bagshaw M., 2009, Cosmic rays: are air crew at risk?, Occupational Environment Medicine, Vol. 59, pp. 428-432. Martin, I. M., 1972, Medidas de raios-X e clculo do fluxo adicional na regio da Anomalia Magntica do Atlntico Sul, M.Sc. Dissertation, Instituto de Pesquisas Espaciais, So Jos dos Campos. National Aeronautics and Space Administration (NASA), 2009, Deep solar minimum [cited Feb 28, 2010] Available at: http://science.nasa.gov/headlines/ y2009/01apr_deepsolarminimum.htm. Noll M., et al., 1999, Measurements of the equivalent dose at aircraft with TLDs, Radiation Protection Dosimetry, Vol. 85, No 1-4, pp. 283-286. OBrien K., 1978, LUIN, a code for the calculation of cosmic ray propagation in the atmosphere (update of

HASL-275), Environmental Measurements Laboratory Report EML-338, Springfield, VA, National Technical Information Service. Oliveira, M. A. L., 2000, Simulao de Chuveiros Atmosfricos Extensos e Mtodos de Reconstruo de seus Parmetros Fundamentais, PhD Thesis, Universidade de Campinas, Campinas. Pinto Junior, O., 1985, Estudos sobre raios-X na atmosfera da Anomalia Magntica do Atlntico Sul, PhD Thesis, Instituto de Pesquisas Espaciais, So Jos dos Campos. Space Environment Information System (SPENVIS). [cited Jun 18, 2010] Available at: http://www.spenvis. oma.be Spurn F., et al., 2007, Monitoring of onboard aircraft exposure to cosmic radiation: May-December 2005, Advances in Space Research, Vol. 40, pp. 15511557. Tommasino, L., 1999, In-flight measurements of radiation fields and doses, Radiation Protection Dosimetry, Vol. 86, No 4, pp. 297-301. Transport Canada, 2001, Measures for managing exposure to cosmic radiation of employers working on board aircraft, Commercial and Business Aviation Advisory Circular 183.

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doi: 10.5028/jatm.2010.02026410

Empresa Brasileira de Aeronutica S.A. So Jos dos Campos Brazil gustavo.trapp@embraer.com.br

Luis Gustavo Trapp*

Evaluation of nacelle drag using Computational Fluid Dynamics


Abstract: Thrust and drag components must be defined and properly accounted in order to estimate aircraft performance, and this hard task is particularty essential for propulsion system where drag components are functions of engine operating conditions. The present work describes a numerical method used to calculate the drag in different nacelles, long and short ducted. Two- and three-dimensional calculations were performed, solving the Reynolds Averaged Navier-Stokes (RANS) equations with a commercial Computational Fluid Dynamics (CFD) code. It is then possible to obtain four drag components: wave, induced, viscous and spurious drag using a far-field formulation. An expression in terms of entropy variations was shown and drag for different nacelle geometries was estimated. Keywords: CFD, Drag, Engine, Nacelle, Propulsion. transonic speeds can be separated into viscous (or profile) drag, induced drag and wave drag. Viscous drag consists of skin friction and form drag actuating inside the boundary layer due to the viscosity. Induced drag is produced by a modification on the pressure distribution due to the trailing vortex system that accompanies the lift generation. Wave drag, in transonic and supersonic flight speeds, is related to shock waves that induce changes in the boundary layer and pressure distribution over the body surface.

Empresa Brasileira de Aeronutica S.A. So Jos dos Campos Brazil henrique.argentieri@embraer.com.br *author for correspondence

Henrique Gustavo Argentieri

INTRODUCTION Evaluation of the performance of an aircraft during its development process is done using different tools. One starts with statistical databases during the conceptual phase; proceeds to CFD or analytical tools during preliminary design together with wind tunnel tests, and ends up in the certification phase, with the actual performance measurement on the aircraft. The ability to accurately predict the aerodynamic drag, more specifically the correct contribution of each drag component, could represent a strategic commercial advantage. For example, the addition of some drag counts could represent passenger limitations in some commercial airplane routes; consequently, the direct operation costs (DOC) increase, making the airplane less attractive for potential customers. The major aircraft performance parameters are drag and lift, which together with an engine deck can be used to evaluate other major aircraft characteristics: range, climb rate, maximum speed, maximum payload and so forth. When comparing lift and drag estimations using CFD, the lift can be more easily estimated given that it is one order of magnitude greater than drag. Even though some advances were made during the last decade, drag estimation using CFD still lacks behind the accuracy of a wind tunnel, with challenges like the accurate prediction of large separation regions and of laminar to turbulent boundary layer transition. The knowledge on the physical components of the drag is important for the prediction of scale effects on aircraft drag. The aerodynamic drag of an aircraft flying at
Received: 04/04/10 Accepted: 27/04/10

DRAG BOOKKEEPING The generally accepted method to obtain the installed nacelle drag is to calculate it by subtracting the clean aircraft drag from the drag of the aircraft with nacelles (Flamm and Wilcox, 1995). However, this technique does not allow the separation of the various drag components that contribute to the total installed nacelle drag, which include: interference drag (from the nacelle on the wing and from the wing on the nacelle) and the external and internal nacelle drag. According to Flamm and Wilcox (1995), another disadvantage of this technique is that the data accuracy is reduced because the strain-gauge balance must be selected to measure the drag of the entire model instead of only the nacelles. A workaround to this problem was developed by Bencze (1977) by mounting the aircraft model on a strain-gauge balance and support mechanism, whereas the nacelles were mounted on an independent balance and model support mechanism. Therefore, it was possible to determine the interference drag components after measuring the aircraft and nacelle drag separately.
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Additionally, this improves the accuracy of the nacelle drag measurements since the strain-gauge balances are sized to measure only the nacelle drag. However, this technique is limited in the sense that the nacelle pylon is not modeled. The split between internal and external nacelle drag is also important because while the propulsion specialists are busy developing an engine and measuring thrust at static conditions, aerodynamic specialists are busy developing an airframe and measuring drag at wind-on conditions, usually in separate organizations and at different locations (SAE, AIR1703). The engine streamtube usually defines what is treated as drag and what is thrust loss: the flow outside the streamtube produces drag, while what is inside the streamtube produces thrust loss (Fig. 1). Nevertheless, the exact definition of the thrust/drag bookkeeping system depends on the agreement between the engine and airframe manufacturers and on the details of the propulsion system.

illustrated the drag decomposition from CFD due the entropy variations in the flow as well as the identification of a spurious contribution due to numerical dissipation of the flow solver algorithm and a proper definition of the boundary layer and shock region. Brodersen et al. (2004) presented the drag computation with the standard near-field method integrating the surface pressure forces and shear stresses, and also a drag breakdown into its physical components, such as viscous, wave, and induced drag, applying a far-field approach so that all results are compared to experimental data. Tognaccini (2005), using a far-field formulation, proposed a thrust-drag accounting system given a numerical solution of the viscous subsonic or transonic flow around an aircraft configuration in power-on condition. A very simple and useful explanation to understand the near-field and far-field methods is to consider the aerodynamic drag as a force exerted by the flow field in the opposite direction of the body movement. In the same way, by the law of the action and reaction, the body reacts with a force with the same strength and opposite direction. The drag in the body perspective (near-field) comes from forces due to pressure distributions over the body surface and due to skin friction. Alternatively, the drag force calculated in the flow field perspective (far-field) comes from three natural phenomena: shock waves, vortex sheet and viscosity. The most common method to predict drag consists of the integration of pressure and shear stress acting on the surface analyzed, so-called near-field technique. In this method, the form drag can be successfully determined only if the pressure distribution along the surface is known with great accuracy. For numerical solutions of RANS equations, the problem is mainly related to the presence of numerical artificial dissipation, which produces a spurious drag, and this one becomes negligible only for highly dense grids. Another problem of this method is that the near-field drag only allows the distinction between pressure and friction drag. An alternative way to calculate aerodynamic forces through surface integration is to compute the forces around a surface enclosing the body. The advantage of this technique is that the shear stress contribution may be neglected if the control surface is located outside the viscous layer; however, an additional term (momentum flux) must be included in the analysis. In this method, the drag is determined from the momentum integral balance by considering fluxes evaluated on a surface far from the body. Oswatitsch (1956) derived a formula of the entropy drag considering first-order effects, in which the drag is expressed as the flux of a function depending only on entropy variations. However, this technique can bring

Figure 1: Airflow inside and around the nacelle.

Besides wind tunnel tests, another way to evaluate nacelle drag is using empirical methods and analytical correlations (based on wind tunnels tests), like ESDU 81024 Drag of axis-symmetric cowls at zero incidence for subsonic Mach numbers. However, one disadvantage of this method is that it is seldom the case in actual design to have an axisymmetric nacelle lofting and flow at null angle of attack. Another alternative is to perform the drag extraction using Computational Fluid Dynamics (CFD) tools. A lot of research has been developed on this subject and the AIAA CFD Drag Prediction Workshop (DPW) has been an opportunity for worldwide CFD researchers to share information about their drag prediction methods since 2001. Due to the many advantages of drag extraction with CFD, many authors have written about this subject: Sloof (1986) and van der Vooren and Sloof (1990) contain a review of fundamentals of physics of CFD drag extraction, while van Dam (1999) presents an extended and detailed overview of the state of the art on drag prediction methods. Chao and van Dam (1999 and 2006) presented an airfoil and wing drag prediction and decomposition with a wake integration technique which is very close to the far-field formulation. Paparone and Tognaccini (2002)

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uncertainties if the region integrated is not defined in a way that the spurious drag is eliminated from the calculation. Theoretical drag characteristics The integral of force balance in the free stream direction can be formulated as:
S =Sairc +Sin +Sout +Slat

The right-hand side integral in Eq. (2) represents the reaction forces of the airplane while the left-hand side stands for the total force exerted by the fluid. In the CFD terminology, when the integration is performed using the left-hand side integral in Eq. (2), the near-field method is employed. Conversely, when the integration of the right-hand side in Eq. (2) is computed, the far-field method is considered. Far-field formulation The far-field drag extraction method used is based on the Van der Vooren and Destarac (2004) method, which assumes that viscous and wave drag effects can be considered confined within control volumes and that all entropy changes come from these two phenomena. The key now is to transform the right-hand side of Eq. (2) into an entropy variation function and in separated drag contributions. This formulation can be borrowed from Tognaccini (2005) reference, resulting in the following equation:
2 s s r f s1 + f s 2 V dV R R Vfar

r uV + ( p p ) i t x ndS = 0

(1)

where: p: density; u: velocity component in freestream direction; V: velocity vector; p: pressure; p: freestream pressure; : viscous stress vector in freestream direction; Sairc: aircraft surface; Sin: inlet surface; Sout: outlet surface; Slat: lateral surface. Figure 2 shows a sketch of the domain and respective control volume.

Ds = V

(3)

where:

f s1 =

1 2 g M
2 1 + ( g 1) M 2 2g 2 M

(4)

fs2 =

(5)

s: s - s (entropy variation); R: gas constant; : ratio of specific heats; M: freestream Mach number. In order to perform analyses on two-dimensional nacelle geometries, the equation from Tognaccini (2005) can be simplified to an axisymmetric reference system by taking into account that dV = r.dr.dq. This leads to:
Figure 2: Integration domain.
2 s s r f s1 + f s 2 V rdr ar R R Rf

Equation (1) can be decomposed into two surface integrals as:


Sairc

Ds = 2p V

(6)

r uV + ( p p ) i t x ndS =

Sin +Sout +Slat

r uV + ( p p ) i t x ndS (2)

Where r is the distance from the engine axis of symmetry.


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Volume selection A solution to minimize the spurious drag in the far-field technique is to limit the integration volume. The definition of the integration boundaries can be made using the definition of the boundary layer and shock wave regions explained by Paparone and Tognaccini (2002). They propose a boundary layer and wake region sensor that simply relates the laminar and turbulent viscosity, defined as:

Fv =

l + t l

that can deal with arbitrary mesh types. The ReynoldsAveraged Navier-Stokes three-dimensional equations were solved for the compressible flow using implicit, secondorder interpolation, centroid-based polynomials and preconditioned relaxation. The turbulence model employed was the realizable k-e. The domain initial conditions were identical to the far-field boundary conditions, in which a characteristic-based velocity inflow/outflow was set, thereby prescribing aircraft speed, temperature, turbulence intensity and length scale. The drag extraction formulation was applied to three different cases, typically employed in the development and testing of an aircraft: 1) 2D analysis of an isolated DLR-F6 nacelle; 2) 3D analysis of a long-duct nacelle with different contraction ratios; 3) 3D analysis of a wind tunnel model internal drag.

(7)

where: l: laminar viscosity; t: turbulent or eddy viscosity.

The value of Fv is large in the boundary layer and wake while in the remaining part of the domain it is approximately equal to one. Thus the viscous region is selected by defining it with Fv > (1.1*Fv), where Fv is the free stream value of the boundary layer sensor. The selection of the shock wave region relies on a sensor based on another non-dimensional function:
Fshock V p = a p

Two-dimensional DLR-F6 nacelle drag In order to test the drag assessment procedure, the DLR F6 nacelle (AIAA, 2003) was chosen. This is a wind tunnel model, long-duct nacelle, from the wing-body-pylonnacelle configuration used on the AIAA Drag Prediction Workshops. This nacelle geometry is open to the general public and, therefore, can be used in the future to compare results from different authors. The original nacelle is a through-flow nacelle (TFN) approximately axisymmetric, which can be easily used to perform a two-dimensional analysis. Typical dimensions for the DLR-F6 wind tunnel model nacelle are given on Table 1, together with design parameters.
Table 1: DLR-F6 nacelle dimensions and design parameters

(8)

where: a: local sound speed. This sensor is negative in expansion zones (no shock waves) and positive in compression regions. Cells with negative values of Fshock are excluded from the shock wave region. By using the Rankine-Hugoniot relations, it is possible to estimate the Mach number downstream of the shock (Fcw), and this value is used as cutoff to define the shock wave region establishing the follow correlation:
Fshock > Fcw

(9)

Length Highlight diameter Inlet throat diameter Fan diameter Max diameter Exhaust diameter Diffusion ratio Contraction ratio

Dimension (mm) 180 55.1 49.4 54.8 76.2 50 1.1 1.24

CFD ANALYSES The CFD analyses were performed using CFD++, a commercial CFD code based on finite-volume formulation
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A hexahedral mesh was built around this nacelle, extending 10 nacelle lengths upstream, 20 lengths downstream and 20 fan diameters in the spanwise direction. Figure 3 shows a detail of the mesh, while Table 2 presents the mesh size.

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Figure 3: Detail of the DLR-F6 axisymmetric mesh. Table 2: Mesh size

Total nodes number Total elements number

48,969 49,489
Figure 5: DLR-F6 nacelle drag coefficients as a function of Mach number.

An analysis of different Mach numbers were made at Reynolds number equal to 3 x 106, which was the same Reynolds number at which the DPW measurements were performed. The reference area is 0.1454 m2. Figure 4 shows isocontours of entropy for the Mach 0.6 case in the integration domain, which extends from the engine axis up to 1.57 times the nacelle maximum diameter, and from the nacelle leading to trailing edge. The integration diameter has also been varied, but when there are no shock waves over the nacelle, it does not affect the drag results even with diameters as low as 5% greater than the maximum nacelle diameter. In the presence of the shock waves, the drag values were up to 0.6 drag counts lower, when reducing the integration domain.

Effect of the inlet contraction ratio on nacelle drag The drag of an isolated nacelle is influenced by four major parameters: length, maximum diameter, nozzle diameter and contraction ratio. The length is a function of the engine length and the design of the inlet expansion rate and nozzle convergence rate, as well as the exhaust mixing length. The maximum diameter is defined by the engine accessories attached to the casing, which must be enveloped by the nacelle contours. The nozzle diameter is linked to engine performance and is fixed for a given engine. The contraction ratio is the ratio between the area of the inlet throat and the area of the highlight (the area contained inside the line that connects the inlet leading edge). This ratio affects both the cruise and takeoff performances. A small ratio produces a small cruise drag, but leaves the inlet sensitive to separation with high angles of attack and during crosswind operation on the ground. In order to verify the effect of variations of the inlet contraction ratio on drag, a generic long-duct nacelle was employed and changes were made to its original geometry. Figure 6 shows the nacelle contours.

Figure 4: Isocontours of entropy on the integration domain, Mach 0.3 case.

A comparison between the near field and far-field drag methodologies for the DLR-F6 nacelle as a function of Mach number is presented on Fig. 5. The drag coefficient calculated with near field methodology is about one drag count higher than the far-field method for most speeds, while at the Mach number 0.85 both methodologies estimate approximately the same drag. At the low speeds, one of the reasons for the difference is that the nacelle has a finite trailing edge which is not accounted for in the fair field methodology. On the other hand, at Mach number 0.85 there is a shock wave on the nacelle exterior, which is more conservatively accounted for in the far-field methodology.

Figure 6: Nacelle contours.

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For all geometries, the same the throat area was maintained, while the highlight diameter was changed in order to analyze the nacelle performance. Table 3 summarizes the different Contraction Ratios used.
Table 3: Nacelle contraction ratios

Nacelle A Nacelle B Nacelle C

Contraction ratio 1.200 1.365 1.300

In this work, due to the usage of structured meshes, it was possible to use the same mesh parameters for all geometries, making the results independent of mesh variations between the geometries. The meshes resolutions are shown in Table 4.
Figure 8: Symmetry plane. Table 4: Mesh size

Total nodes number Total elements number

752,92 776,648

The Figures 7 to 9 illustrate the meshed domain and, in more details, the meshed nacelle surface and symmetry plane.

Figure 9: Nacelle mesh detail. Table 5: Flight condition

Mach number Altitude (ft) ISA

0.86 43 0

Figure 7: Full meshed domain.

The three different nacelle contraction ratio geometries were simulated and post-processed in order to estimate all the components drag in the same flow condition, characterized as a cruise flight phase of an aircraft. The flight condition simulated is summarized in Table 5. Figure 10 shows the region of the shock wave sensor and Fig. 11 shows the region selected by the boundary
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Figure 10: Shock wave sensor region.

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Figure 11: Boundary layer sensor region. Figure 12: Nacelle and the cylinder integration volume.

layer sensor. It is important to highlight that the volumes selected by both sensors overlap partially, given that part of the shock wave can be immersed in the boundary layer. Thus it is necessary to apply both sensors together to define the volume where the drag will be calculated. Figure 11 shows the external side of the nacelle with shock waves on the inlet lip, the bottom region near the maximum diameter and near the trailing edge. It also shows a cross cut of the nacelle through the symmetry plane. It can be seen that the volume does not include the internal side of the nacelle (inlet and exhaust regions), which was excluded from the domain after applying the boundary layer sensor. Given that the two-dimensional DLR-F6 nacelle integrated drag was not very much influenced by the integration volume, the drag accounting procedure was simplified and it was decided to use a cylindrical volume around the nacelle, shown on Fig. 12 in the drag computations, instead of the regions defined by the shock wave and boundary layer sensors,. A sensitivity analysis of the drag as a function of the cylinder radius was performed and the Fig. 13 shows a sensitive study with different cylinders radii and the respective drag estimation.It can be observed that there is a small increase in drag with the increase in the integration cylinder radius. Nevertheless, the differences between drag values increase by less than 1% though the integrated volume doubles from one case to the next. According to the flight conditions indicated in Table 5 and by using Eq. (3) with a cylindrical volume of radius equal to 1 m, the results are comparatively summarized in Fig. 14, where Nacelle B is the comparison basis (i.e. 100%).
Figure 13: Sensitive study of the interpolation cylinder radius effect on nacelle drag.

Figure 14: Comparative results of drag for the different geometries.

It is noted from Fig. 14 that the best drag performance of Nacelle A defines the geometry with the lowest drag and consequently contributes to the best aircraft performance. Further comparisons were made with the ESDU results and revealed that drag values agree within 10%.
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Internal drag As seen before, in turbofan engines, the nacelle drag is assumed to be that one produced outside the streamtube passing through the intake, therefore it includes the region from the inlet lip stagnation point to the nacelle trailing edge. The effect of the flow on the internal cowlings, supporting structures as well as the pylon portion scrubbed by the engine jet is regarded as a thrust loss. Additionally, when testing a wind tunnel model, it may present other structures that are not present on a real aircraft or engine test bench. Moreover, in case of shortduct nacelles, parts of the pylon will be washed by the engine stream, thus being necessary its removal from the nacelle drag. Fig. 15 shows a typical short-duct nacelle wind tunnel model.

Figure 16: Entropy isocontours on the symmetry plane of the integration volume.

Figure 17: Internal nacelle model drag coefficient as a function of Mach number. Figure 15: Typical short duct nacelle wind tunnel model. Source: Li, Li and Qin, 2000.

case, such increment is not caused by shock waves, but by the increased separation at the junction between the bifurcation and the inlet duct. CONCLUSIONS A comparison of drag methodologies was performed for a two-dimensional case nacelle. Although a fair agreement on drag was found, some important differences still exist. The far-field methodology does not account for the trailing edge and is greatly affected by shock waves when compared to the near field methodology. It remains to be checked whether these differences would be this great if a three-dimensional analysis were made. Nevertheless, this methodology can be easily employed in optimization processes, in which calculating the absolute value of drag is not as important as reaching the minimum drag. The far-field drag methodology was applied to the evaluation of nacelle drag, showing good agreement with ESDU results and enabling the calculation of more complex nacelle geometries drag. The use of sensors to split the boundary layer and shock regions from the rest of the domain allows the assessment of wave and form drag separately. However, the sensor definition impacts on the size of the integrated region, which could lead

The use of CFD and the far-field formulation present an easy way to perform the split between the external and internal drags. A CFD analysis of the engine and pylon was performed for different Mach numbers, letting the Reynolds number vary and keeping the same sea level ISA condition. The mesh used was a hybrid tetra-prism with approximately 6 million elements. The integration volume chosen included only the internal nacelle, i.e. the inlet duct the core-cowl bifurcation and the external part of the core cowl that is inside the nacelle and its internal surface. The pylon was not included as well as the core-cowl downstream of the fan nozzle. Figure 16 shows a cross cut along the nacelle symmetry plane, with isocontours of constant entropy for the Mach 0.75 case, showing the limits of the integration domain along with the main sources of internal drag. Results of internal drag for the different Mach number cases are shown in Fig. 17 and are consistent with the expected drag levels. When compared to the DLR-F6 nacelles two-dimensional results shown previously, there is a drag increase at the highest speeds. In this
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to errors on the drag value. It is worth noting, however, that the intensity of the spurious drag is small, as well as its effect on the final result, in both two- and threedimensional cases. The separation of internal drag from the overall nacelle (or aircraft) drag was shown to be easily achievable within the post-processing of the results. An identical procedure can be used to analyze the effect of other problems and phenomena on the nacelle, eg.: nacelle inlet lip ice accretion, in case of ice-protection system failure or engine failure; effect of nacelle dents and other protuberances on drag. Even in turboprop engines, a similar method can be employed, evaluating the drag of its intricate shapes, propeller-induced swirl and generally poor aerodynamics of its installations. It must be remarked that the cases analyzed were subject to completely turbulent flows, without any laminar region and that nowadays many manufacturers are researching nacelles that would allow laminar flow up to 20-30% of the nacelle length. In these cases, an additional validation of this methodology needs to be performed. REFERENCES Applied Aerodynamics TC. 2nd AIAA CFD Drag Prediction Workshop, June 21-22, 2003, Available in: http://aaac.larc. nasa.gov/tsab/cfdlarc/aiaa-dpw/Workshop2/workshop2. html Access on May 19, 2010. Bencze, D.P., 1977, Experimental Evaluation of NacelleAirframe Interference Forces and Pressures at Mach Numbers of 0.9 to 1.4, NASA Technical Memorandum X-3321, March 1977, Ames Research Center, United States. Brodersen, O. et al., 2004, Airbus, ONERA, and DLR Results from the 2nd AIAA Drag PredictionWorkshop, AIAA Paper No 2004-391, 42nd AIAA Aerospace Sciences Meeting and Exhibit, Reno, Nevada. Chao, D. D., van Dam, C. P., 1999, Airfoil Drag Prediction and Decomposition, Journal of Aircraft, Vol. 36, No. 4, pp. 675-681.

Chao, D. D., van Dam, C. P., 2006, Wing Drag Prediction and Decomposition, Journal of Aircraft, Vol. 43, No. 1, pp. 82-90. ESDU, 2004, Drag of Axisymmetry Cowls at Zero Incidence for Subsonic Mach Numbers, Item No. 81024, Engineering Sciences Data Unit. Flamm. J. D., Wilcox Jr., F. J., 1995, Drag Measurements of an Axisymmetric Nacelle Mounted on a Flat Plate at Supersonic Speeds, NASA Technical Memorandum 4660, June 1995, Langley Research Center, United States. Li, J., Li, F., Qin E., 2000, Numerical Simulation of Transonic Flow over Wing-Mounted Twin-Engine Transport Aircraft, Journal of Aircraft, Vol. 37, No. 3, May-June 2000. Oswatitsch, K., 1956, Gas Dynamics, Academic Press Inc, New York, pp. 177-210. Paparone, L., Tognaccini, R., 2002, A Method for Drag Decomposition from CFD Calculations, ICAS 2002 Congress, pp 1113.1-1113.9. Sloof, J. W., 1986, Computational Drag Analysis and Minimization; Mission Impossible?, Proceedings of the Aircraft Drag Prediction and Minimization Symposium, AGARD R-723, Addendum 1. Tognaccini, R., 2005, Drag Computation and Breakdown in Power-on Conditions, Journal of Aircraft, Vol. 42, No. 1, pp. 245-252. van Dam, C. P., 1999, Recent Experience with Different Methods of Drag Prediction, Progress in Aerospace Sciences, Vol. 35, pp. 751-798. van der Vooren, J., Destarac, D., 2004, Drag/Thrust Analysis of Jet-Propelled Transonic Transport Aircraft, Definition of Physical Drag Components, Aerospace Science and Techonolgy, Vol. 8, pp. 545-556. van der Vooren, J., Sloof, J. W., 1990, CFD-Based Drag Prediction; State of the Art, Theory, Prospects, Lectures notes prepared for the AIAA Professional Studies Series, Course on Drag-Prediction and Measurement, Portland (OR).

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doi: 10.5028/jatm.2010.02026310

Gibran da Cunha Vasconcelos

Univ. Estadual Paulista Guaratinguet Brazil mat06070@feg.unesp.br

Rogerio Lago Mazur

Univ. Estadual Paulista Guaratinguet Brazil rogermaz@uol.com.br

Evaluation of crystallization kinetics of poly (ether-ketoneketone) and poly (ether-etherketone) by DSC


Abstract: The poly (aryl ether ketones) are used as matrices in advanced composites with high performance due to its high thermal stability, excellent environmental performance and superior mechanical properties. Most of the physical, mechanical and thermodynamic properties of semi-crystalline polymers depend on the degree of crystallinity and morphology of the crystalline regions. Thus, a study on the crystallization process promotes a good prediction of how the manufacturing parameters affect the developed structure, and the properties of the final product. The objective of this work was to evaluate the thermoplastics polymers PEKK e PEEK by DSC, aiming to obtain the relationship between kinetics, content, nucleation and geometry of the crystalline phases, according to the parameters of the Avrami and Kissinger models. The analysis of the Avrami exponents obtained for the studied polymers indicates that both showed the formation of crystalline phases with heterogeneous nucleation and growth geometry of the type sticks or discs, depending on the cooling conditions. It was also found that the PEEK has a higher crystallinity than PEKK. Keywords: Crystallinity, PEKK, PEEK, DSC. These matrices have in common high mechanical resistance, thermal and chemical strength (Canevarolo, 2004; Lucas, 2001; Thornburrow, 2000). The thermoplastic and thermoset polymers differ in many ways. One difference is that it is only possible obtaining some degree of crystallinity in the thermoplastics polymers. The thermosets ones are always amorphous with very low or no crystallinity. The crystallinity consists of regions of aligned polymer chains, usually produced by a single chain bending. The relationship between crystalline and amorphous region of a polymer sample is expressed in terms of percentage of crystallinity or degree of crystallinity. The percentage of crystallinity of a polymer can be determined by differential scanning calorimetry (DSC), from a peak of exothermic crystallization (Lucas, 2001; Denault, 1996). DSC is a thermal analysis technique that measures the difference in energy provided to a sample and a reference material in function of a controlled temperature programming. This technique keeps constant the heat supplied to the sample and reference. A control system (servo system) immediately increases the energy supplied to the sample or the reference, depending on if the process involved is endothermic or exothermic. Therefore, the equipment keeps the sample and the
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Edson Cocchieri Botelho

Univ. Estadual Paulista Guaratinguet Brazil ebotelho@feg.unesp.br

Mirabel Cerqueira Rezende

Institute of Aeronautics and Space So Jos dos Campos- Brazil mirabel@iae.cta.br

Michelle Leali Costa*

Univ. Estadual Paulista Guaratinguet Brazil michelle@feg.unesp.br

* author for correspondence

LIST OF SYMBOLS x(t) k n E R T Tp f H fA


H fA 100% crystalline

(dx/dt)p

Volume fraction occupied by the crystallites Constant rate of global crystallization Avrami expoent Activate energy Gas constant Temperature Temperature of peak crystallization Ratio of the system colling Range of fusion enthalpy of a sample with unknown crystallinity percentage Range of fusion enthalpy of a sample with crystallinity of 100% Variation rate at the peak of crystallization

INTRODUCTION In recent years, the fast development in science and technology of materials has improved the production of new products in the aerospace industry. Among them the advance in polymeric composites are an example of recognized success. The most commonly used polymer matrices in the processing of structural composites are thermosetting type. However, nowadays new generations of high performance thermoplastic matrix are being developed for use in composites reinforced with carbon fibers.
Received: 01/04/10 Accepted: 20/04/10

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reference at the same temperature. The record of the DSC curve is expressed in terms of heat flow versus temperature or time (Lucas, 2001). During the manufacture of semi-crystalline thermoplastic composites, the polymers are exposed to repeated processes of melting, cooling and crystallization. The knowledge of the crystallization mechanisms of polymers presents a fundamental importance, since the degree of crystallinity influences the mechanical and thermal properties of these materials (Canevarolo, 2004; Lucas, 2001). The poly (aryl ether ketone) is used as matrices in advanced composites for high performance due to its excellent thermal and mechanical properties. Poly (ether-etherketone) (PEEK) and poly (ether-ketone-ketone) (PEKK) offer excellent chemical resistance and good chemical and physical properties at high temperatures. Recently, they have been widely used in commercial applications, where high temperatures and resistance are required (Gardner, 1990; Wang, 1997). Most physical, mechanical and thermodynamic properties of semi-crystalline polymers depend greatly on the degree of crystallinity and morphology of the crystalline regions. The higher the crystallinity, the higher are the properties of density, stiffness, dimensional stability, chemical resistance, abrasion resistance, melting temperature and glass transition temperature. Therefore, detailed knowledge of crystallization kinetics in a transformation processes is fundamental to control the final properties of the composites (Canevarolo, 2004; Lucas, 2001). Traditionally, the more widely used technique in crystallization kinetics is DSC. With different analysis parameters, DSC can provide important characteristics for the studied polymer, and it is possible to achieve different mechanical characteristics at the same polymer to different applications (Lamberti, 2006). Several researchers have been studying the crystallization kinetics of thermoplastic polymers with high structural performance. The Avrami kinetic model, developed at first from the probability theory, is simple and yet enough complete to describe the nucleation and growth until the crystals collision. The Avrami model describes the macroscopic nucleation and growth of any crystal structure as a function of time. In general development, it is assumed that the time of nucleation and crystal growth are interdependent and depend on distribution of material to areas of growth of crystallites. The final expression for isothermal crystallization is given by Eq. 1 (Lucas, 2001; Hsiao, 1991; Ferrara, 2004):

X(t)=1-exp(-kt n )

(1)

If we multiply both sides of the Eq. 1 by (ln), we get (Eq. 2):

ln(exp(-kt n )=1n(1-x(t))

(2)

Regrouping the Eq. 2 and multiplying again by (ln), we have (Eq. 3):
ln(-1n(1-x(t))=1n(k)-nln(t)

(3)

Therefore, if we plot the axis ln(-1n(1-x(t)) versus ln(t), the angular coefficient of the formed straight line gives us directly the value of the Avrami exponent. The Avrami exponent describes the crystallization and provides qualitative information about the nature of the process of nucleation and crystal growth. The relationship between the constant of crystallization kinetic and the activation energy is given by Eq. 4 (Lucas, 2001; Canevarolo, 2004):

-E k=k 0 .exp R.T

(4)

Therefore, the Avrami exponent may be calculated by (Eq. 5):


dx n= R.Tp2 .(0,37..E ) 1 dt p

(5)

The activate energy might be calculated (Eq. 6) by knowing the temperature of crystallization peak, from Eq. 5:
Tp 2 E.Tp ln cte = R

(6)

So, the crystallization percentage is calculated directly by (Eq. 7) (Lucas, 2001; Sidel, 2008):
% of crystallization H fA x100 H fA 100% cystalline

(7)

The objective of this paper was to initiate a study of the crystallization kinetics of PEEK and PEKK polymers by DSC, in order to get the relationship between the kinetics, the percentage, the nucleation and the geometry

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of crystalline phases formed, according to the parameters of Avrami and Kissinger models. METHODOLOGY Materials In this study, the semi-crystalline thermoplastic polymers PEKK and PEEK were analyzed. The used PEKK was supplied by Du Pont company in the form of granules, and PEEK was manufactured by the company ICI and negotiated by LATI thermoplastics in powder form. Study of crystallization kinetics PEKK The analysis by DSC was performed in a Perkin-Elmer Pyris 1 Model DSC, calibrated with indium and zinc, under constant flow of nitrogen (20 mL/min) and a heating rate of 20C/min. Samples of PEKK (~ 15 mg) were encapsulated in a standard sample pan of aluminum. Firstly, a dynamic analysis (30 to 380C at 20C/min, followed by cooling at the same rate) was performed in order to know the melting and crystallization temperatures of PEKK. Then, new samples were prepared and heated at a heating rate of 20C/min from ambient temperature to the thermodynamic melting temperature of PEKK (~ 340C), remaining 2 minutes at this temperature to allow complete melting of all crystals (thus eliminating that remaining crystals which act as seeds for crystallization). Subsequently, the samples were cooled under the rate of 100C/min until the desired isothermal temperatures of crystallization (305C, 307C, 310C and 311C) and were maintained in these isothermals until the formation of the exothermic peaks of crystallization. PEEK The DSC analysis was performed in an equipment SII NanoTechnology Inc. Seiko Model EXSTAR6000, previously calibrated with indium and zinc, at a heating rate of 10C/min. Samples of PEEK (~ 10 mg) were encapsulated in a standard pan sample of aluminum, and dynamic analyses were carried out at temperatures of 50C to 380C. The samples were heated in the heating rates of 5, 10, 15 and 20C/min. Subsequently, these samples were cooled at the same rates used for heating until the temperature of 50C, in order to forming exothermic

peaks which determine the existence of crystalline phases in the polymer. From these curves, it was possible to establish the kinetic parameters of crystallization, with consequent study on the type of nucleation involved in the formation of crystalline phases and the geometry of their growth. This study was based on the kinetic modeling of Avrami and Kissinger. RESULTS AND DISCUSSION PEKK In this study, the sample was heated twice in the DSC, according to the norm ASTM D3418, in order to destroy the thermal history of the polymer; only the second heating was considered for data analysis. Figure 1 shows the second dynamic heating of PEKK, where an endothermic peak can be observed in the curve at the temperature of 314C, indicating the melting of the material. The endothermic peak generated a fusion enthalpy of 6.9 J/g.

32

Heat Flow (mW)

31 30 29 28 250 270 290 310 330 350

Temperature (C)

Figure 1: DSC of the second heating cycling of PEKK on a rate of 20C/min.

According to the literature, the melting temperature of PEKK is around 305-340C; however, these values are directly related to the rate which the polymer is cooled or heated (ratio of heating, cooling, isotherms) and factors such as the processes involved in the synthesis of the polymer. This makes harder a direct comparison between the data. Even though, the melting temperature found in this study is within the range described in the literature (Hsiao, 1991; Pratte, 2002; Vries, 2006; Salek, 2005). Then, the PEKK was cooled in a rate of 100C/min, until four different temperatures, all in the melting region of PEKK. Samples were kept in the isotherms for 60

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minutes, in order to obtain the organization of polymeric macromolecules for the formation of crystalline phases. Thus, an exothermic peak on the crystallization (Tc) should be clearly observed. The crystallinity (about 5.4%) was obtained from the ratio between the fusion enthalpy of the sample (HfA) and the fusion enthalpy of 100% crystalline sample (HfA 100% crystalline) according with Eq. 7. Table 1 shows that the exothermic peaks obtained at the chosen isothermal crystallization of 305C, 307C, 310C and 311C showed low enthalpy.
Table 1: Crystallization enthalpy values of PEKK for the 305, 307, 310 and 311C isotherms

these temperatures has crystal growth geometry of disk type with heterogeneous nucleation, as suggested in the literature (Lucas, 2001).

Isotherms (C) 305 307 310 311

-H (J/g) 0.915 1.647 0.794 0.317

t1/2* (min) 0.2 0.21 0.24 0.22

Crystallization rate (%)**(min-1) 5 4.76 4.16 4.54

Figure 2: Relation between the experimental peaks and the math model (straight lines) of Avrami used.

* t1/2 is the necessary time to achieve half of crystallization, or the necessary time to achieve the peak at the crystallization curve on DSC. ** Crystallization rate (%) is defined as 1/ t1/2.

It appears that in none of the studied isothermals the crystallization was complete, since the values of enthalpy are smaller from that obtained for the dynamic fusion of PEKK. This can also be explained based on the low crystallinity of PEKK, which makes difficult the crystallization process in the crystalline melt region. The enthalpy values are very close, with the exception of the isotherm at 311C, which is the isotherm of the highest temperature and probably makes difficult the formation of crystals. The half life times obtained for each isotherm (Table 1) are also similar and show a very fast rate of crystallization: less than 0.2 minute. It must be remembered that high crystallization rate is not directly related to high degree of crystallinity (Hsiao, 1991). The highest rate was achieved in crystallization isothermal of 305C. Figure 2 shows the experimental points obtained from the isotherms (symbols) and the mathematical fit used by the regroup of Avrami equation (Eq. 3). The good correlation between the experimental points and the lines shows that the Avrami equation model fits the crystallization kinetics of PEKK. The values of Avrami exponent (n) were about 2.7 and 2.0 for the isotherms of 310 and 307C, respectively. This indicates that the PEKK at

In the 305C isotherm, we observed that the kinetic behavior of PEKK shows a double kinetic feature, where there is a primary and a secondary stage, as observed by Velisaris and Seferis (1986), among others, suggesting the existence of two active mechanisms in crystallization process. At this temperature, the first stage of crystallization has a value of n of about 1.4 and the second one has a value of 0.66 (Hsiao, 1991, Ferrara, 2004, Velisaris; Seferis, 1986). Figure 3 shows the development of relative crystallization (a in %) with the isothermal crystallization time for the temperatures of the rigid crystalline phase and variable amorphous phase between 305 and 311C. It can be observed in the deform S format of graphs that the crystallinity (%), initially zero, begins to grow rapidly

Figure 3: Development of crystallization relative to isothermal crystallization time for temperatures from 305 to 311C.

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in the first few moments of crystallization, achieving quickly 100% of crystallization for this material remembering that PEKK has low crystallinity (< 6%) (Wang, 1997). It appears that, with the increasing of temperature, the isothermal crystallization process becomes greatly accelerated in reaching complete crystallization in less than 30 seconds. This fact makes difficult the study of isothermal crystallization kinetics for PEKK, since the control of crystallinity of the material is complex due to the high spontaneous crystallization process. PEEK The PEEK was first heated until its melting and then cooled at the rates of 5, 10, 15 and 20C/min. Figure 4 shows the exothermic peaks formed during the cooling of PEEK, and the values of enthalpy of crystallization for these peaks are shown in Table 2. It can be observed that the greatest crystallization enthalpy for this polymer was found for the cooling rate of 20C/min. This shows that the crystallinity of this polymer is promoted by higher cooling rates.

Using the values of the crystallization temperature peak of Fig. 4, the DSC curves for various cooling rates were linearized using the method of least squares applied for Gaussian functions. The values of crystallization peak temperature for the studied cooling rates are shown in Table 3.
Table 3: Temperatures of crystallization peak found to the different cooling rates of PEEK

Cooling rate (C/min) 5 10 15 20

Crystallization peak temperature (C) 303.5 299.4 293.4 291.2

From Table 3, it was possible to obtain the curve of ln(Tp/f) versus 1000/Tp, which gives the curve fit by the least squares method, shown in Figure 5.

Figure 4: DSC curves of PEEK for the following heating rates: 5, 10, 15 and 20C/min.

Figure 5: Graph of ln(Tp/f) versus 1000/Tp to the heating rates of 5, 10, 15 and 20 C/min to the PEEK.

Table 2:

Enthalpy values found to the different cooling rates of PEEK

Cooling rates (C/min) 5 10 15 20

H (J/g) -45.8 -37.7 -45.5 -53.8

From Fig. 5 and Eq. 6, it was possible to calculate the activation energy (E) for crystallization of PEEK. The value of E, calculated following the Kissinger modeling, was 292.5 kJ/mol. Knowing the crystallization enthalpy, obtained from Fig. 4, the curve of the fraction of crystallized material as a function of reaction time, using Eq. 6, was possible to obtain. Figure 6 shows the required time to complete the crystallization reaction of PEEK in different ratios of cooling in which it was submitted.

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however, the growth geometry formed was the bat type (Lucas, 2001). Table 4 summarizes data from the value of n found for cooling rates studied for PEEK.
Table 4: Avrami exponent values found for the different cooling rates to PEEK

Cooling rate (C/min) 5 10


Figure 6: Crystallizated material fraction versus time to the heating rates of 5, 10, 15 and 20C/min.

Avrami exponent (n) 2.35 2.06 1.59 1.46

15 20

The crystallization rate (dx/dt) of PEEK was obtained from the fraction of crystallized material at the various cooling rates involved (Fig. 7). The growth rate shows the points where the crystallization occurred in a higher rate. The largest variation obtained for each curve is used to determine the value of n for different cooling rates in which the material was submitted.

CONCLUSIONS For the isothermal temperatures of 307 and 310C, the Avrami model fits the crystallization kinetics of PEKK, which allows the study of the crystal growth geometry in this region. The value of n is obtained in the range from 2.0 to 2.7, with heterogeneous nucleation, which indicates a growth type of disc geometry. For the isotherm of 305C, the PEKK exhibited a double kinetic behavior, with probably two active mechanisms in the process of crystallization. At this temperature, the first stage of crystallization showed a value of n of about 1.4, indicating a stick growth-type geometry with heterogeneous nucleation, but in the second stage the model does not fit the kinetics of crystallization. The deformed S shape, observed in the relation of crystallization relative to time of isothermal crystallization, shows that the accelerated crystallization process makes difficult the study of PEKK crystallization at the isothermals chosen. The PEEK showed significant crystallinity in all the studied cooling rates. Moreover, it was observed that the crystallization time for this polymer is between about 5-15 minutes. That means that, in order to promote the crystallization of this polymer, is not necessary to maintain it at high temperatures for too long. Thus, the crystallization process is not too fast, which may cause a difficulty in controlling the process and makes not possible to obtain parts with a high degree of crystallization in very short periods of time. It can be also observed that the growth geometry of disc type in PEEK is promoted by lower cooling rates. Major cooling rates promotes the growth geometry of the bat type.

Figure 7: Curves of crystallization rate versus temperature to PEEK for the heating rates: (a) 5C/min; (b) 10C/ min; (c) 15C/min; (d) 20C/min.

Knowing the value of E involved in the crystallization process, the value of n for the PEEK was calculated from Eq. 5. The value of n is related to the growth geometry of crystalline phases and also with this type of nucleation. Thus, at the cooling rates of 5 and 10C/min, the crystalline phases were formed with heterogeneous nucleation and growth geometry of disk type. For the cooling rates of 15 and 20C/min, the crystalline phases were also formed with heterogeneous nucleation;

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It was possible to obtain the correlation between the crystallization kinetics of both studied polymers. Thus, a much higher crystallinity in the case of PEEK was primarily noted. Furthermore, the formation of crystalline phases for PEKK occurred in a more spontaneous way when compared with PEEK. This suggests that there is a difficulty in controlling the crystalline fraction of PEKK, comparing to PEEK. The analysis of the obtained n values indicates that both polymers showed the formation of crystalline phases with growth geometries of bat or discs types, depending on the cooling conditions applied. The study of crystallization kinetics of PEKK was held in a restricted manner, due to the difficulty of crystallization of this polymer and its low crystallinity. Thus, it was possible to study the crystallization kinetics for this polymer only under isothermal conditions. As it was possible to obtain significant crystallinity for PEEK with relative easiness, the study of this polymer occurred in the form of dynamic tests. However, an analysis under isothermal conditions as a complement to the previous study should be also performed. Moreover, for a possible application of this polymer, its degradation kinetic should also be studied, as it would promote parameters for lifetime of the material at temperatures in which it is applied. ACKNOWLEDGEMENTS To the companies DuPont and LATI thermoplastics, for providing, respectively, the PEKK and the PEEK used in this work. To Fapesp, for the financial support contract 05/54358-7 and 08/00171-1. To CNPq for the financial support contract 104778/2008-3 and 119244/2009-8. To Capes, for financial support. REFERENCES Canevarolo Jr, S.V., 2004, Estrutura Molecular do Estado slido, Comportamento trmico dos polmeros, Comportamento mecnico dos polmeros, In: Cincia dos Polmeros, So Paulo: Artliber, pp. 67, 127-137, 157-158.

Denault, J., Guillemenet, J., 1996, Continuous carbon and glass fiber reinforced polypropylene: optimization of the compression molding process, International SAMPE Symposium, SAMPE, no. 41, pp. 1688-1700. Ferrara, J.A., 2004, Manifestations of Crystallization in the Processing of High Performance Thermoplastic Composites, Washington: University of Washington. Gardner, K.H., and Matheson, R.R.J., 1990, Polym, Sci. Lett, Vol. 28, pp. 28, 243. Hsiao, B.S.; Chang, I.Y.; Sauer, B.B., 1991, Isothermal crystallization kinetics of poly(ether ketone ketone) and its carbon-fibre-reinforced composites. Polymer, Vol. 32, No 15, pp. 2799-2805. doi: 10.1016/0032-3861(91) 90111-U. Krebs, J.; Bhattacharyya, D.; Friedrich, K., 1997, Production and evaluation of secondary composites aircraft components a comprehensive case study, Composites: part A, Vol. 28A, pp. 481-489. Lamberti, G., and Naddeo, C., 2006, Some issues on polymer crystallization kinetics studied by DSC non isothermal tests, Polymer Bulletin, Vol. 56, No 6, pp. 591-598. doi: 10.1007/s00289-006-0518-2. Lucas, E.F.; Soares, B.G.; Monteiro, E.E.C., 2001, Caracterizao de polmeros: determinao de peso molecular e anlise trmica, Rio de Janeiro: E-papers. Phillips, R.; Glauser, T.; Mnson, J.A.E., 1997, Thermal stability of PEEK/carbon fiber in air and its influence on consolidation, Polymer Composites, Vol. 18, No 4, pp.500-508. Pratte, J.F.; Bai, J.M.; Leach, D., 2002, Poly (Ether Ketone Ketone) Matrix Composites, International SAMPE Technical Conference, Baltimore, MD, USA, Vol. 34, pp. 949-958. Salek, M.H., 2005, Effects of Processing Parameters on the Mechanical Properties of Carbon/PEKK Thermoplastic Composite Materials, SAMPE 2005, Long Beach, CA. Sidel, S.M., et al. , 2008, Parmetros de cristalizao noisotrmica do sistema vtreo Li2O-TeO2-WO3, Congresso Brasileiro de Engenharia e Cincia dos Materiais, Vol. 18, Porto de Galinhas (PE), Brazil. Thornburrow, P., 2000, Design and process interactions in reinforced thermoplastics, In: Owen, A.M.J.; Midleton,

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V.; Jones, I.A. (Eds.). Integrated design and manufacture using fibre-reinforced composites. Boca Raton, USA: CRC Press. Velisaris, C.N., and Seferis, J.C., 1986, Polym, Eng. Sci., Vol. 26, p. 26. Vries, H., 2006, Influence of processing parameters on mechanical properties of PEKK/AS4, National

Aerospace Laboratory NLR, International Symposium on Composites Manufacturing Technology for Aircraft Structures, Vol. 3, Marknesse, Holland. Wang, W.; Schultz, J.M.; Hsiao, B.S., 1997, Dynamic study of crystallization- and melting-induced phase separation in PEEK/PEKK blends, Macromolecules, Vol. 30, No. 16, pp. 4544-4550. doi: 10.1021/ ma970092l.

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doi: 10.5028/jatm.2010.02027310

Instituto de Aeronutica e Espao So Jos dos Campos Brazil ldvillar@iae.cta.br

Luciene Dias Villar*

Rafael Filadelfo da Silva

Universidade de So Paulo Lorena Brazil rafael_fs1812@hotmail.com

The role of antioxidant on propellant binder reactivity during thermal aging


Abstract: Thermal aging of hydroxy-terminated polybutadiene (HTPB) stabilized with 2,6-di(tert-butyl)hydroxytoluene (BHT) was carried out at 60oC from 1 to 11 weeks. Samples of 200 mL were stored in sealed 500-mL Erlenmeyer flasks under atmospheric pressure or vacuum and periodically withdrawn for physical and chemical analysis, infrared spectroscopy characterization and measurement of HTPB/IPDI (isophorone diisocyanate) reactivity, expressed as pot life. Mechanical properties of the cured polyurethane, prepared from aged HTPB, were assayed by uniaxial tension tests. Despite the unchanged chemical structure, an increase in HTPB/IPDI binder reactivity was observed, being correlated with BHT depletion measured as color change (yellowing). Aging of HTPB showed no interference on mechanical properties of the cured polyurethane. Keywords: Antioxidant, Composite propellant, HTPB propellant, Polyurethane resin, Storage.

Instituto de Aeronutica e Espao So Jos dos Campos Brazil miltond@iae.cta.br

Milton Faria Diniz

Marta Ferreira K. Takahashi

Instituto de Aeronutica e Espao So Jos dos Campos Brazil martat@iae.cta.br

Instituto de Aeronutica e Espao So Jos dos Campos Brazil lcrezende@iae.cta.br * author for correspondence

Luis Cludio Rezende

INTRODUCTION Although there has been an increasing research effort into development of energetic polymer binders for solid rocket propulsion, hydroxy-terminated polybutadiene (HTPB) is still widely used in the formulation of composite propellant. This 1,3-butadiene homopolymer contains terminal and reactive hydroxyl groups, introduced during free radical polymerization by peroxide or azo compounds. During solid propellant processing, these hydroxyl groups react with a diisocyanate resulting in polyurethane, which acts as a binder for the solid particles of the propellant composition. Due to the unsaturated character of the repeated unit, polybutadiene is known to be sensitive to oxidation, thus being usually supplied with the addition of stabilizers (Ninan et al., 1996), namely antioxidants, especially hindered phenol compounds. The mechanisms and kinetics of HTPB oxidation have been a matter of great concern since the 1960s. More recently, Coquillat et al. (2007a, b, c) have defended the occurrence of radical addition to double bonds and allylic methylene consumption, meanwhile Guyader et al. (2006) have emphasized the mechanism of
Received: 07/06/10 Accepted: 20/06/10

epoxide formation during HTPB aging. In spite of this, both works agree that oxidation of HTPB is highly dependent on sample thickness and oxygen partial pressure, a condition hardly mentioned in previous studies (Hinney and Murphy, 1989; Pecsok et al., 1976). In one of these studies (Hinney and Murphy, 1989), the effect of HTPB aging over its reactivity with isocyanates was investigated by measuring the decrease in pot life, defined as the time necessary to reach a pre-established viscosity value. The authors attributed the increase in reactivity to the higher functionality derived from HTPB oxidation through a mechanism of hydroperoxide formation. In our study, an assessment of the influence of usual storage conditions over aging of HTPB was carried out by submitting large samples (200 mL) of this resin, stabilized with the primary antioxidant BHT, to thermal aging under stagnated atmospheric pressure or under vacuum. Physical and chemical analysis, infrared spectroscopy and pot life measurement showed that, being diffusion-dependent, the observed increase of HTPB reactivity was not due to change in its chemical structure. Instead, an overview of the concerned literature indicated that it was related to BHT depletion and conversion into quinone derivatives, which may eventually react with isocyanates to graphitize into the polyurethane.
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EXPERIMENTAL Material Samples of uncrosslinked HTPB (Mn = 2,900 g/mol) of predominant trans 1,4 structure (Takahashi and Diniz, 2002) were supplied by Petroflex (Brazil) containing 1% w/w of BHT (2,6-di(tert-butyl)hydroxytoluene, CA index name as 2,6-bis(1,1-dimethylethyl)-4-methyl-phenol). The material was maintained in tightly closed vessels at room temperature until they were used. Aging conditions Aging experiments were conducted on 200-mL samples of uncured liquid HTPB placed in sealed 500mL Erlenmeyer flasks. Flasks were placed into forced circulating air oven at 60 1oC and protected from day light exposition. Headspace of the flasks was kept either at atmospheric pressure or under 99% vacuum. Duplicated flasks were withdrawn after 1, 2, 4, 6, 9 and 11 weeks and placed for characterization at the same day of collection (pot life and physical and chemical analysis) or within a maximum of two days (mechanical properties). Samples were maintained in desiccators at room temperature until analyses were performed. Characterization Determination of pot life was made by stoichiometric reaction of HTPB with IPDI (isophorone diisocyanate, CA index name as 5-isocyanato-1-(isocyanatomethyl)1,3,3-trimethyl-cyclohexane) in the presence of 0.012% w/w of the catalyst ferric acetylacetonate (tris(2,4pentanedionato-iron). The catalyst was blended with HTPB in a mechanical stirrer. The mixture was heated for bubble removal. After addition of IPDI, the mixture was manually stirred and immediately placed for viscosity measurement at 50oC. The time required to reach 20 Pa.s was considered as the pot life. At each sampling time, an unaged sample of HTPB was also analyzed for pot life as a control. Yellowing of HTPB was measured by using a spectrometer in the visible region (PerkinElmer Lambda 3B UV/VIS). In preliminary tests, a range of wave length varying from 220 to 320 nm was evaluated. Maximum absorption was obtained at 295 nm. Samples were diluted in toluene (1:1) and analyzed in duplicate with toluene as the blank. Determination of physical and chemical properties included: hydroxyl number (Takahashi et al., 1996);
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viscosity at 25oC measured in a small sample device (Brookfield LVDV-II+ with software Wingather 2.2) and humidity (Karl Fischer Metrohm 633). Fourier transform infrared spectra (FT-IR) were collected by using a PerkinElmer Spectrum One spectrometer. HTPB was analyzed as thin films, while BHT was analyzed as potassium bromide pressed-pellet. Analyses were carried out under transmission mode at the following conditions: spectral range 4000 - 400 cm-1; 40 scans and 4 cm-1 resolution. Pot life and color change were evaluated by using the property retention index (PRI) as defined by ASTM D5870-95 (2003) for destructive tests. Determination of the PRI for each replicate exposed to aging, zi , is defined by Eq. (1).

zi =

pi , x p0

(1)

Where, Pi,x: property of the i replicate at exposure time, x, and p0: initial value of the property. Determination of the mean PRI, , is defined by Eq. (2).

Z=

z
i =1

(2)

Where, zi: PRI for each replicate exposed to aging; n: number of replicates. Mechanical properties Samples of HTPB aged for 1, 5, 8 and 10 weeks were also used to prepare polyurethane samples with 2 mm thickness and compared with polyurethane prepared from unaged HTPB. Dumbbell specimens were assayed for uniaxial tension tests, according to ASTM D412-06a in a Zwick 1474 testing machine at 500 mm/min and 25oC. Hardness was measured in circular specimens with 70 mm thickness by following ASTM D2240-05. RESULTS AND DISCUSSION Physical and chemical properties of HTPB for the unaged condition are presented in Table 1, which are in accordance

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The role of antioxidant on propellant binder reactivity during thermal aging

with recommended specifications (MIL-H-85497-81) for application of HTPB in solid propellants. Some of the properties investigated have no specified limits. In order to improve the comparison between both treatments (atmospheric pressure and vacuum), property retention index was applied to the processing property of pot life and to HTPB color changing (yellowing), as showed in Fig. 1. A remarkable decrease of pot life retention index was followed by a sigmoidal increase of color retention index during the course of the aging experiment (Fig. 1). A linear correlation between them is presented in Fig. 2, showing that the decrease in pot life is related to yellowing increase by a correlation factor of 0.90 and 0.94 for atmospheric pressure and vacuum, respectively.

Figure 2: Correlation between pot life and color change retention indexes.

Figure 1: Pot life and color change retention indexes as a function of aging time.

The values of hydroxyl number, viscosity and humidity are presented in Fig. 3. Dashed lines represent upper (UL) and lower (LL) limits (Table 1). Although some fluctuations can be observed, the investigated properties were kept under the specified limits and showed no significant variations throughout the aging assay.

Figure 3: Physical and chemical properties of HTPB as a function of aging time.


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Table 1:

Physical and chemical properties of unaged HTPB and recommended specifications

Physical and chemical property Hydroxyl number (m mol/g) Humidity (%) Acid number (mg KOH/g) Viscosity (Pa.s, 25oC) Refraction index (d) Density (20oC) ns: not specified.
Table 2:

HTPB unaged 0.75 0.01 0.05 0.02 0.16 0.01 6.8 0.1 1.516 0.001 (20oC) 0.902 0.001

MIL-H 85497-81 type I 0.75 to 0.85 0.10 max. ns 4.0 to 8.0 ns ns

Mechanical properties of cured polyurethane obtained from aged and unaged HTPB

Aging time (weeks) 0 1 5 8 10

Tensile strength [MPa] 1.3 0.1 1.3 0.1 1.4 0.1 1.2 0.1 1.3 0.1

Mechanical properties Tensile modulus [MPa] 2.1 0.1 2.1 0.1 2.0 0.1 2.1 0.1 2.3 0.1

Hardness [ShA] 41 1 40 1 41 1 40 2 43 1

Infrared spectra were obtained on samples of HTPB exposed to 0, 1, 2, 4, 6, 9, and 11 weeks under thermal aging at both pressure conditions. For practical reasons, only the first and the last exposure time spectra are presented in Fig. 4. Aged and unaged HTPB

samples presented similar spectra for both atmosphere conditions investigated. Increase in the absorption at the region of 3394 cm-1(nOH), which could account for increase in functionality, was not observed. Additionally, the absorption at the region of 1639 cm-1 (nC=C olefinic) remained unchanged, indicating no radical addition to double bonds up to the detection level of this technique. The absence of absorptions at the regions around 1740-1800 cm-1 (nC=O) and 8301000 cm-1 (nOO) in the aged samples also indicates no built-up of carbonyl or hydroperoxide groups. A BHT spectrum was also included in Fig. 4. Due to its low concentration (1%) on HTPB, peaks of BHT or its quinone derivatives were not apparent in HTPB spectra. In order to verify if the change in reactivity of the binder system could interfere in the mechanical properties of the cured polyurethane, properties of tensile strength, Young modulus and hardness (Shore A) of the HTPB/ IPDI polyurethanes were assayed. They showed not to be changed with the aging of HTPB (Table 2). Although the readily oxidative nature of HTPB is well established, Coquillat et al. (2007 a, b, c) and Guyader et al. (2006) have demonstrated its dependency on oxygen diffusion. Considering the aging testing conditions of this study, which used large samples (200 mL) exposed to mild temperature, without shaking the flasks, oxygen diffusion was quite difficult even at atmospheric pressure. In these conditions, oxidation of HTPB backbone may have hardly occurred as pointed by the

Figure 4: Infrared spectra of aged and unaged HTPB and BHT antioxidant. A: unaged HTPB; B: aged HTPB under atmospheric pressure for 11 weeks; C: aged HTPB under vacuum for 11 weeks; D: BHT.
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results of physical and chemical properties, especially hydroxyl number (Fig. 1), and by infrared spectra (Fig. 4). It is important to state that the dark condition of aging and the analysis of aged samples had minimized any effect of UV light in the results presented (Fig. 1 and 3). The unchanged values of humidity (Fig. 3) indicated that the reactivity increase cannot be attributed to the reaction between IPDI and any absorbed atmospheric humidity. In addition, the occurrence of HTPB homopolymerization or oxidative cross-linking during aging could not be verified, respectively, by the results of viscosity of uncured HTPB (Fig. 3) or by any change in the mechanical properties of the cured polyurethane (Table 2). On the other hand, the correlation between pot life decrease and color change (Fig. 2) indicated that the well-known yellowing of hindered phenol antioxidants (Vulic et al., 2002), even in the absence of oxygen (Bangee et al., 1995), may be related to the apparent change in HTPB reactivity, which was observed independently of the oxygen partial pressure. In fact, some studies (Celina et al., 2006; Dsilets and Ct, 2006; Shanina, Zaikov and Mukmeneva, 1996) have demonstrated that quinone derivatives from hindered phenol antioxidants react quite readily with isocyanates and graphitize into HTPB backbone. Based on this literature evidence, our results indicate that the apparent increase of the HTPB/IPDI binder reactivity is due to a side-reaction between BHT quinone derivatives and IPDI. CONCLUSION The observed increase of reactivity after thermal aging of HTPB was correlated to antioxidant depletion and quinone by-products formation, which was assigned the role to react with IPDI, thus resulting in the observed pot life decrease. No experimental evidence was obtained in order to correlate the change in reactivity with change in chemical structure of HTPB. ACKNOWLEDGMENTS Thanks are due to Prof. Dr. Gilmar P. Thim (ITA) for allowing the use of spectrometer UV/Vis. Technical support of the Laboratories of Chemical Division, specially PPR-I, PPM, EPE and CAQ, are recognized. Financial support from AEB is acknowledged. RFS acknowledges CNPq for the undergraduate scholarship (PIBIC-IAE).

REFERENCES Bangee, O.D. et al., 1995, Antioxidant-induced yellowing of textiles, Polymer Degradation and Stability, Vol. 50, No 3, pp. 313-317. Celina, M. et al., 2006, Correlation of antioxidant depletion and mechanical performance during thermal degradation of an HTPB elastomer, Polymer Degradation and Stability, Vol. 91, No 8, pp. 1870-1879. Coquillat, M. et al., 2007a, Thermal oxidation of polybutadiene. Part 1: effect of temperature, oxygen pressure and sample thickness on the thermal oxidation of hydroxyl-terminated polybutadiene, Polymer Degradation and Stability, Vol. 92, No 7, pp. 1326-1333. Coquillat, M. et al., 2007b, Thermal oxidation of polybutadiene. Part 2: mechanistic and kinetic schemes for additive-free non-crosslinked polybutadiene, Polymer Degradation and Stability, Vol. 92, No 7, pp. 1334-1342. Coquillat, M. et al., 2007c, Thermal oxidation of polybutadiene. Part 3: molar mass changes of additive-free non-crosslinked polybutadiene, Polymer Degradation and Stability, Vol. 92, No 7, pp. 1343-1349. Dsilets, S., Ct, S., 2006, Chemical bond between stabilizers and HTPB-binders in propellants, Propellants, Explosives, Pyrotechnics, Vol. 25, No 4, pp. 186-190. Guyader, M. et al., 2006, Epoxides in thermal oxidation of polybutadiene, Polymer Degradation and Stability, Vol. 91, No 11, pp. 2813-2815. Hinney, H.R., Murphy, J.R., 1989, Suppression of reactivity changes in poly BD R-45M resin, Proceedings of the 20th International Annual Conference of ICT, Karlsruhe, Germany, pp. 49-(1-11). Ninan, K.N. et al., 1996, Thermoanalytical investigations on the effect of atmospheric oxygen on HTPB resin. Propellants, Explosives, Pyrotechnics, Vol. 21, No 4, pp. 199-202. Pecsok, R.L. et al., 1976, Fourier transform infrared studies of the mechanism of oxidation of cis-1,4polybutadiene, Rubber Chemistry and Technology, Vol. 49, No 4, pp. 1010-1018. Shanina, E.L., Zaikov, G.E., Mukmeneva, N.A., 1996, Peculiarities of inhibiting the autooxidation of solid polypropylene with 4,4-bis(2,6-di-tert-butylphenol), Polymer Degradation and Stability, Vol. 51, No 1, pp. 51-56.
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Takahashi, M.F.K., Diniz, M.F., 2002, espectroscopia no infravermelho da de poliuretano baseado em resina hidroxilada, Ecltica Qumica, Vol. 27, 263-271.

Avaliao por microestrutura polibutadinica No special, pp.

Takahashi, M.F.K. et al., 1996, Determinao de ndices de hidroxila em polibutadienos hidroxilados e de grupos NCO em diisocianatos e pr-polmeros por espectroscopia no infravermelho com transformada de Fourier, Polmeros: Cincia e Tecnologia, Vol. 6, No 4, pp. 45-52.

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doi: 10.5028/jatm.2010.02027610

Instituto de Aeronutica e Espao So Jos dos Campos Brazil aparecidamkawamoto@hotmail.com

Aparecida M. Kawamoto

Synthesis of a boron modified phenolic resin


Abstract: Phenolic resin has long been used as matrix for composites mainly because of its flame retardant behavior and high char yield after pyrolysis, which results in a self supporting structure. The addition of ceramic powders, such as SiC and B4C, as fillers to the phenolic resin, results in better thermo-oxidative stability, but as drawbacks, it has poor homogeneity, adhesion and processing difficulties during molding of the composites. The addition of single elements, such as boron, silicon and phosphorus in the main backbone of the thermo-set resin is a new strategy to obtain special high performance resins, which results in higher mechanical properties, avoiding the drawbacks of simply adding fillers, which results in enhanced thermo-oxidative stability compared to conventional phenol-formaldehyde resins. Therefore, the product can have several applications, including the use as ablative thermal protection for thermo-structural composites. This work describes the preparation of a boron-modified phenolic resin (BPR) using salicyl alcohol and boric acid. The reaction was performed in refluxing toluene for a period of four hours, which produced a very high viscosity amber resin in 90% yield.The final structure of the compound, the boric acid double, substituted at the hydroxyl group of the aromatic ring, was determined with the help of the Infrared Spectroscopy, 1H-NMR, TGA-DSC and boron elemental analysis. The absorption band of the group B-O at 1349 cm-1 can be visualized at the FT-IR spectrum. 1H-NMR spectra showed peaks at 4.97-5.04 ppm and 3.60-3.90 ppm assigned to belong to CH2OH groups from the alcohol. The elemental analysis was also performed for boron determination.The product has also been tested in carbon and silicon fibers composite for the use in thermal structure. The results of the tests showed composites with superior mechanical properties when compared with the conventional phenolic resin. Keywords: Phenolic resin, Boron, Thermal protection, Oxidizing agents. Tc Tg TG Critical temperature Glass transition temperature Thermogravimetric analysis

Instituto de Aeronutica e Espao So Jos dos Campos Brazil pardini@iae.cta.br

Luiz Cludio Pardini*

Instituto de Aeronutica e Espao So Jos dos Campos Brazil miltond@iae.cta.br

Milton Faria Diniz

Instituto de Aeronutica e Espao So Jos dos Campos Brazil vlucia@iae.cta.br

Vera Lcia Loureno

Marta Ferreira K. Takahashi

Instituto de Aeronutica e Espao So Jos dos Campos Brazil martat@iae.cta.br *author for correspondence

LIST OF SYMBOLS Ar-H BPFR DMA DSC DTG FT-IR GPC HMTA ILSS Mn Mw NMR OH PC PF PPG PS TLC Aromatic protons Boron-containing phenol-formaldehyde resin Dynamic mechanical analysis Differential scanning calorimetry Differential thermogravimetry Fourier transform spectroscopy Gel permeation chromatography Hexamethylenetetramine Interlaminar shear strength Molecular weight (average number) Molecular weight (average weight) Nuclear magnetic resonance Hydroxyl group Polycarbonates Phenol formaldehyde resin Polypropyleneglycol Polystyrene Thin layer chromatrography

INTRODUCTION Phenolic resin was the first synthetic polymer. The processing technique was carried out firstly by A. von Bayer, in 1872, and further patented by Leo H. Baekeland in 1907 (Knop and Pilato, 1985). Since then, thermo-set phenolics have wide industrial and commercial application (Whitehouse, Pritchett and Barnett, 1968). Due to their excellent ablative properties and structural integrity, they have been used as high performance thermal protection systems, such as nose caps and exit cones for rocket nozzles (Knop and Pilato, 1985; Segal, 1967; Schmidt and Graig, 1982). They also have widely use in thermal insulation materials, molding compounds, foundry, coating material, wood products industry and in many other composite materials (Casiraghi et al., 1980). Another application is the use as precursor of solid carbon materials as a matrix for heat resistant materials (Lenghaus, Qiao and Solomon, 2000), and also as adhesives

Received: 14/06/10 Accepted: 28/06/10

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for production of wood agglomerates (Park et al., 1999). Another important application of phenolics is as a polymeric blend with other polymers, which produces materials with superior physical properties, such as tensile strength and modulus (Okoroafor, Villemaire and Agassant, 1992). Phenolic resins are synthesized by the reaction of phenol with formaldehyde. These resins can be divided into two main groups according to reaction conditions that are used, such as pH of the catalyst and the formaldehyde/ phenol ratio. Formaldehyde has a functionality of two and phenol, of three. Phenol will react with the OH group at the para and at the two ortho position. The two meta positions are un-reactive. If the reaction proceeds with excess of one or two moles of formaldehyde, the final product is a thermo-set resin. If the reaction proceeds with excess of phenol, it has sufficient functionality, but not enough cross linking molecules to be thermo-set or thermoplastic resin. Under acidic conditions, the reactions of phenol with formaldehyde with excess of phenol lead to the formation of novolac type resin (Fig. 1). The resole type resin is formed under alkaline conditions and excess of formaldehyde (Fig. 2). The main difference between novolac and resole resins is the presence of the reactive methylol groups and, occasionally,

dimethylene-ether linkage in the resoles instead of the condensation products linked with methylene bridges, as in the case of novolacs. Therefore, novolac resins are thermally cured by addition of a methylene cross linker hexamethylenetetramine (HMTA) or paraformaldehyde. Resoles are cured only by application of heat. Phenol formaldehyde resins (PF) are characterized by their capability of forming hydrogen bonds with polymers containing carbonyl or carbonate groups (Fahrenholtz and Kwei, 1981), or forming covalent bonding if the polymer contains complementary hydroxyl groups. In addition, the phenyl ring structure of phenolic resin is capable of forming secondary bonding by - overlap, which is important for building these polymers. The final properties of these materials depend on the synthesis and operating conditions. Details of the curing process are responsible for many of the physical and mechanical characteristics: the cure time and temperature influence, the resulting glass transition temperature (Tg) and the elastic modulus. Thus, structural information and explicit knowledge relevant to the curing process is important and essential for understanding and improving the synthesis process and the use of phenolic resins. The most commercially available phenolic resin has the average molecular weight (Mw) in the range of 500 to 1000 gmol-1. The molecular weight of phenolic resins depends on the formaldehyde/phenol ratio, the type of catalyst (acidic or alkaline), and the time and temperature of the reaction, but the most important factor for controlling the molecular weight of PF is the molar ratio. Figure 3 shows the resulting type of phenolic resin, resole or novolac, as a function of the formaldehyde/phenol ratio and molecular weight (Lemon, 1985).

OH OH OH OH CH2OH CH2O CH2OH OH ... OH ...

HO CH3 OH CH2 OH

OH

Figure 1: Structure of novolac resin.


OH CH2OH

OH

OH OH H2C CH2OH CH2O CH2OH CH2OH OH HOH2C CH2OH HOH2C

OH CH2OH HO CH2 OH CH2OH OH CH2OH

+ CH2O

CH2OH

Figure 2: Structure of resole resin.


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Figure 3: Curing graphic for phenolic resin forming novolac and resol (Lemon, 1985).
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Synthesis of a boron modified phenolic resin

The most common catalyst of phenol-formaldehyde novolac resin synthesis is: sodium, potassium and lithium hydroxides, and rarely hydroxides of divalent metals (magnesium, calcium or barium) (Knop and Sheib, 1979; Knop and Pilato, 1985). Carbonates (Na) and oxides (Ca or Mg) can also be used as catalyst in the synthesis (Polish Patent 109 966, 1981; Polish Patent 150 036, 1990). Tertiary amines, in particular triethylamine, were claimed recently as the catalyst for the resole resin synthesis (Russina Patent 2 028 313, 1995; US Patent 4 045 398, 1977). Knop (1979,1985) found that the substitution of phenol with formaldehyde in the ortho-position versus para-position increased in the following sequence of hydroxide catalyst metal: K < Na < Li < Ba < Sr < Ca < Mg. Grenier-Loustalot et al. (1996) concluded that the rate at which phenol disappeared from the reaction mixture depended on the metal valence in the hydroxide catalyst and on the size of the hydrated metal cation. Magnesium, calcium and barium hydroxides were found to be more effective catalyst than lithium, sodium or potassium hydroxides. Although phenolic resin has good thermo-oxidative resistance, extensive research has been done to improve their thermal properties through modification of their structure with introduction of some elements, such as boron or phosphorus and even silicon. The boron-containing phenol-formaldehyde resin (BPFR) is a modification of the phenolic resin. It is obtained with the introduction of boron in the main backbone of the phenolic resin. The BPFR resin has good heat-resistance, mechanical properties, electric properties and absorbance of neutron radiation (Abdalla, 2003). There are several works that describe the synthesis and applications of BPFR (America Patash Chem Corp, 1964; Gao and Liu, 1999; Gao and Liu, 2001). This resin is usually synthesized by the formaldehyde method, in which phenol borate synthesized from phenol and boric acid is followed by the reaction with poly-formaldehyde. Another popular method is the synthesis using the method of formalim (Gao and Liu, 1999), which consists in the reaction of phenol with formaldehyde to form the alcohol and then followed the reaction with boric acid. MATERIALS AND EXPERIMENTAL Materials Solvents, boric acid and 2-hydroxy benzyl alcohol were purchased from Aldrich, Fluka or Merck, according to their required purity, price and availability. Butanediol,

dichloromethane and epichlorhydrin were purified by distillation prior to use. Experimental Synthesis Boric acid and 2-hydroxy benzyl alcohol in a ratio of 1:2 were dissolved in toluene and placed in a four-necked round bottom flask equipped with a stirrer, thermometer, condenser and a Dean Stark system, and stirred under reflux for the period of four hours. Over this period, the amount of water collect at the Dean Stark was according to the calculated amount, and also the total disappearance of the alcohol can be observed on the TLC plate. Then, the solvent was evaporated giving a high viscous amber product in 89.4% yield. The reactions were performed by the use of the Dean Stark system with a heat controlled oil bath, and they were followed through the amount of water that were released during the reaction and also from thin layer chromatography. H-NMR, 13C-NMR analysis were conducted on a 300 MHz Brker DPX spectrometer using methyl-d6 sulfoxide as solvent. The proton and carbon chemical shifts are recorded in ppm and calibrated on the solvents as internal standard. Infrared spectroscopy has been recorded by a Magna-IR spectrometer 750 Fa. Thermo Nicolet (4000 to 400 cm-1, 40 scans).
1

Resin characterization and composite processing and characterization The characterization of boron-modified phenolic resin, uncured and cured, was performed by thermal (DSC and TG) and mechanical analysis. DSC analyses were carried out in a PerkinElmer Pyris 1 DSC analyser, at 20C/min in N2 (20 mL/min), mass of 11 mg in a tightly closed aluminium sample holder and gave information on the curing process, temperature and heat of the reaction and also the glass transition temperature for the cured resin. The glass transition was measured in the second heating. TG/DTG analysis of uncured resin were carried out in a SDT-Q600 TA Instruments analyser, using alumina pans (11 mg), under nitrogen atmosphere (100 mL/ min) and heating rate of 10C/min. TG/DTG curves under nitrogen or synthetic air (20 mL/min) of the cured boron-modified phenolic resin were produced at 10C/min using a PerkinElmer Pyris 1 TG analyser and platinum pans (11 mg). TG/DTG/DTA curves were obtained with a Seiko TG/DTA 6200 analyser,
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under synthetic air (20 mL/min) at 2.5 and 10oC/min, platinum pans (2 mg). The rheological characterization of n on cured resin was performed on a Rheometrics SR5 rheometer by using a parallel plate measuring system. The rheological characterization helps to obtain viscosity profiles as a function of time, temperature and shear rate, which in turn can be used to define the processing window of the neat resin. Thermal diffusivity measurements were carried out according to ASTM E1461-07 in the temperature range of 25 to 175C. The thermal diffusivity of a material depends on its thermal conductivity, density and heat capacity according to Equation 1. The thermal diffusivity characterizes the heat transport in material during transient regime conditions.

specimen

=6 mm

load span P/2 P/2 =3 mm

Figure 4: Dimensions of the specimens and its assembling on the equipment for performing the tests according to ASTM 2344-06.

Thermal diffusivity

.Cp

(1)

specimen were measured in the direction 1-2 of the composite, as shown in Fig. 5. In this case, the loading is parallel to the stacked layers. The test jig used for the tests is showed in Fig. 6. Accepted Iosipescu shear failure modes are mainly between the V-notches.

Where: k = thermal conductivity; = density; Cp = heat capacity. A composite material was molded in the form of a plate by using a lab-scale autoclave. The composite was molded with silica fabric fiber (650 g/m2) and the boronmodified phenolic resin. The cure schedule was made according to the cycle developed in this work. A 55% fiber volume fraction was measured in the silica fiber/ resin composite. The composite was characterized by interlaminar and Iosipescu shear tests. The interlaminar shear strength was measured according to ASTM D2344-06, using specimens with dimensions showed in Fig. 4. Accepted failure modes for interlaminar shear are characterized by tiny elongated cracks between laminae at the center of the specimen. The interlaminar shear strength is calculated according to the Equation 2.

Figure 5: Specimen geometry for Iosipescu shear tests in the 1-2 plane.

3 P average = rupture 4 A

(2)

Where: taverage: apparent interlaminar shear strengh (MPa); Prupture : ultimate load corresponding to the rupture of the sample (N); A: cross section area calculated by W (width) x t (thickness) (mm2). The Iosipescu shear test was performed according to ASTM D5379-98. The strength and modulus of composite
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Figure 6: Test jig for Iosipescu shear test, according to ASTM D5379-98.

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The Iosipescu shear strength can be calculated by the Equation 3:

OH H
+

OH
70oC NAOH

OH CH2OH
+

OH CH2OH HOH2C
+

CH2OH

C O H

Where: t: the aparent average shear strength, in MPa; Pultimate: the ultimate load of the sample at rupture N; A: the cross section area of the specimen (width x thickness), between the V-notches (mm2). RESULTS AND DISCUSSION
OH

P ultimate A

(3)
OH HOH2C CH2 OH

HOH2C

HOH2C

OH HOH2C + CH2OCH2

OH CH2OH

HOH2C

HOH2C

HOH2C

HOH2C

Scheme 1: Method for the synthesis of salicyl alcohol.

Structure of boron modified phenolic resin According to the literature (Xu, 1976; Tu and Wei, 1981; Heefel et al., 1975), the initial condensation product of salicyl alcohol and boric acid consists mainly of phenol borate and some salicyl alcohol borate as shown in Fig. 7.
OH B O O O OH B O HO
BO

+ B(OH)3

300oC

B O

+ HOB O

+ (HO)2BO

+ H2O

3
H
+ 3

2
HOH2C

C O H 3

150oC

BO HOH2C

+ BO

CH2OH 3

O HOH2C

CH2OH 3

Scheme 2: Method for synthesis of BPFR resin.

Figure 7: Condensation products from the reaction of salicyl alcohol and boric acid.

Several attempts has been done to obtain the boron resin using the formalin method, however, it was not possible to get a monomer free from side compounds and therefore the following reaction to get BPFR resin did not proceed. The alternative proposed in this project was to get the monomer starting from the available pure alcohol and reaction with boric acid. Then, the reaction was performed according to Scheme 3.

In this work, the synthesis has been done using the Formalin (Gao and Liu, 1999) method, that consists in the initial formation of salicyl alcohol (reaction of phenol with formaldehyde) that followed the reaction with boric acid. However, the reaction of phenol with formaldehyde produced a mixture of several compounds as shown in Scheme 1 (Abdalla, Ludwick and Mitchell, 2003). This mixture is difficult to separate, causing problems to follow the subsequent reaction to obtain the desired monomer. Hirohata et al. (Hirohata, Misaki and Yoshii, 1987) used the strategy of the reaction of phenol with boric acid followed reaction with formaldehyde. However, this also leads to a mixture of several compounds that is very difficult to separate, as shown in Scheme 2. However, it has been proved (Gao and Liu, 1999) that the reaction of salicyl alcohol with boric acid proceeded with the ratio of 50% in 50 minutes, while the reaction of phenol was only 4% in 150 minutes. Therefore, it is evident that the condensation product has salicyl alcohol groups attached to oxygen of boric acid (Scheme 3).

OH CH2OH

HOH2C

(1)

(3) H3BO3

O CH2OH O B O CH2OH

(3) H2O

Scheme 3: Synthesis of BPFR monomer.

In order to replace the three OH groups at boric acid to alcohol, the molar ratio of 3:1 (alcohol:acid) was used, which would produce the compound shown in Scheme 4. As it has been described at experimental part, the reaction was performed in toluene at 120C. However, the resulting compound has only two OH groups replaced by the alcohol. The third group could not be replaced, and this might be due to steric hindrance. After four hours, the reaction is finished, as it can be visualized from the water that is formed and collected at the Dean Stark. When the reaction was left longer (approximately 12 hours), it was verified the formation of side compounds, resulted from the reaction of the methylol groups that condense with each other forming methylene and ether linkages, as shown is Scheme 4.
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OH OH OH CH2OH CH2OH O B (1) O CH2OH + OH CH2OCH2
+

OH CH2 (2)

H3BO3

OH

not present in the acid, and the band at 1350 and 1300 cm-1 (BO) refers to the acid. The strong band at 1200 cm-1 and the remaining bands at 700 cm-1 refer to alcohol and acid (Smith, 1999).
(3)

+
H2O

Scheme 4: Synthesis of boron resin.

When the reaction is interrupted after four hours, the product is only the compound resulting from the condensation of boric acid with salicylic acid (Knop and Pilato, 1985), an amber and high-viscous compound. The non reacted salicylic acid precipitated as white solid. Analysis of the boron modified phenolic resin Figure 8 shows the FT-IR spectrum of the boron resin. The main bands are in agreement with the bands coming from boron and the alcohol. The region at 3400-3300 cm-1 shows characteristic bands for alcohol and acid. The band at 1592 cm-1 belongs to the alcohol. Boric acid has a strong and characteristic band at 1480 cm-1 and the alcohol has several bands between 1482 and 1417 cm-1. Therefore, the bands that were observed between 1493 and 1421 cm-1 belong to both acid and alcohol. The bands at 1395 and 1234 cm-1 belong only to alcohol, since these bands are

In general, the 1H-NMR and 13CNMR spectra of the BPFR resins are always complicated to analyze, which reflects the complexity of the boron containing system. The 1H-NMR spectrum is shown in Fig. 9. The wide resonance lines (multiplets) at the region of 6.89-7.19 ppm refer to the aromatic protons (Ar-H). The resonances at the region of 4.97-5.04 ppm and 3.60-3.90 ppm are assigned to the methylene groups (CH2OH) and ether linkages (CH2OR). The peaks at the region of 2.5 ppm are assigned to the OH groups that come from boric acid and salicylic alcohol. The elemental analysis of the resin showed 66.49% carbon, 5.36% hydrogen, 13.96% oxygen and 4.46% boron. The calculation of the percentage value of boron that can be present in a resin (pre-polymer), obtained from boric acid reaction, gave a value of about 4%. The calculation was carried out based on the compound resulted from the reaction of boric acid with two molecules of salicyl alcohol (Fig. 10a). The difference resulted from the measured elemental analysis was about 10%, which might be from the small amount of product containing methylol group condensation that started to form (Fig. 10b), which presents higher content of boron.

0.75 0.70 0.65 0.60 0.55 0.50 0.45 0.40 0.30 0.25 0.20 0.10 0.05 -0.00 0.35

Boron resin 6 Durascope NX08.548

Absorbance

1252 1272 1234 1201

1421 1395

1349

1493

1301

4000

3500

3400

3000

2500

2000

1592

0.15

1500

1000

Wavenumbers (cm-1)

Figure 8: Fourier transform spectroscopy (FT-IR) for boron resin.

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936 848

1108 1089 1039 1005

1456

735

751

0.80

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KAWA2713_BORON RESIN 6_1H-NMR.ESP

0.45 0.40

6.82

4.96

0.50

6.84

Normalized Intensity

0.35

6.93

0.30 0.25 0.20

7.12 7.00

6.69 6.68

5.04

3.87 3.81 3.78

2.51 4.81
0.23

0.15 0.10 0.05 0 8.0 7.5

6.67 6.67

6.65

0.65

4.55

0.09

3.70

0.03

7.0

6.5

6.0

5.5

5.0

4.5

4.0

3.5

3.0

2.5

2.49
2.0

Chemical Shift (ppm)

Figure 9:

H-NMR of boron resin.

CH2OH O

OH B O

CH2OH

CH2OH O

O B O

CH2

Figure 10a

Figure 10b

Figure 10: (a) Molecules of salicyl alcohol (b) product containing methylol group condensation.

Differential scanning calorimetry analysis With differential scanning calorimetry (DSC) measurement is possible to get a thermal profile of the investigated sample under the conditions of thermal dynamic or isothermal scanning. The results of the measurements produce the knowledge of the reaction behavior, the beginning, the end and at which point the reaction reach its maximum peak. It also gives the heat of reaction and the glass transition temperature when operated under dynamic scanning. Figure 11 shows the DSC curve of the boron phenolic resin. The reaction starts at around 205C, with a peak in 224C, and ends at 260C. The heat of reaction is approximately 120 J/g.The Tg at DSC from cured samples is shown in Fig. 12. The value of Tg for the boron phenolic resin is approximately 266.4C, which is superior to the commercial phenolic resin that has a value of 130C.

Figure 11: DSC curve of the boron resin at 20C/min in N2, 20 mL/min, mass of 11 mg in a tightly closed aluminium sample holder.

Table 1 summarized the results obtained from the isothermal cure showed in Fig. 10. These curves give the possibility to calculate the partial heat of reaction, which subsequently could be used for determining the rate of conversion of the ongoing curing reaction. Thermogravimetric analysis The thermogravimetric (TG) analysis is an important thermal analysis that shows the thermal stability of the
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around 25%, which results in a significant yield of 75%. As a comparison, condensation cure phenolic resins show a carbon yield of 45% tested under similar conditions. In synthetic air, the material showed a similar behavior, but with a weight loss of 10% up to 500C, and 27% up to 800C, shows an yield of 72%.

Figure 12: DSC analysis for determining glass transition temperature of boron resin after DSC curing. The red line is the specific heat curve.

materials. Also, the profile of decomposition process and yield of the material associated with the thermal treatment can be obtained. The TG curve of a uncured boron-modified phenolic resin is shown in Fig. 13. It shows two stages of weight loss. The first stage started around room temperature and continued until 250C, with 12.5 0.3% of weight loss, which is related to the curing reaction. In the second stage, 250790C, the weight loss was 25.7 0.2%, which was due to the decomposition of the polymer, leaving a carbonaceous residue equal to 61.9 0.4% of the initial mass.

Figure 14: TG of the cured boron-modified phenolic resin in nitrogen (20 mL/min). Heating rate = 10C/min; sample weight = 12 mg.

100
[ ] Weight (%)

4.0
(12,5 0,3)% 250.00C (25,7 0,2)%

3.5 3.0 2.5


[ ] Deriv. Weight (%/min)

80 60 40 20 0

792.00C Residue (61,9 0,4)%

2.0 1.5 1.0 0.5 0.0

Figure 15: TG of cured boron-modified phenolic resin in synthetic air (20 mL/min). Heating rate = 10C/min; sample weight = 11.6 mg.

200

400 Temperature (C)

600

800

-0.5

Universal V4.1D TA Instruments

Figure 13: TG and DTG curves of uncured boron resin (nitrogen, 10C/min).

Figures 14 and 15 show the TG analysis for a cured boron-modified phenolic resin in nitrogen atmosphere and synthetic air atmosphere, respectively. In nitrogen, the material showed a maximum weight loss of 5% up to 500C, when an inflexion begins until, approximately, 600C. Up to 800C, the material showed a weight loss
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The controlled degradation mechanism under pyrolysis of phenol formaldehyde type resins has been described elsewhere in many works during the last four decades (Costa et al., 1997; Serio et al., 1991). The structural changes are mainly monitored by thermogravimetry coupled with mass spectroscopy and FT-IR. In inert atmosphere and temperatures above 350C, there is mainly evolution of water and unreacted oligomers (Costa et al., 1997). Up to 500C, the polymer network remains essentially unaffected, whereas above 500C dramatic changes can be noticed, leading to the collapse of the network and formation of polyaromatic domains (Costa et al., 1997; Clayton, Fabish and Lagedrost, 1969).

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According to Costa (Costa et al., 1997), air oxidation takes place in lower temperatures (~300C) than when the resin was heated in an inert atmosphere. This was confirmed in the present work for the boron-modified phenolic resin (Figs. 14 and 15). Although similar morphology rearrangements can take place, in the presence of an oxidizing atmosphere, oxidative degradation is not an important pyrolysis pathway, as mentioned by Costa et al. (1997). In the case of the boron-modified phenolic resin, an hyperbranched structure can take place after curing, which increases the carbon yield (~80%/mass in nitrogen at 800C) in the air in relation to the conventional phenol formaldehyde resin (~45%/mass in nitrogen at 800C) (Costa et al., 1997). On the other hand, Liu et al. (2007) studied the pyrolysis and the structure of hyperbranched polyborate modified phenolic resin using thermogravimetry. The resin was prepared by mixing resole with boric acid in acetone. The yield in weight loss obtained by thermogravimetry was found to be ~75%/mass in nitrogen up to 800C, which is similar to the result found in the present work (Fig. 14). The thermogravimetric studies performed on the boronmodified phenolic resin show the outstanding performance of this material in oxidizing environment (Fig. 16) in relation to the commercial phenolic resin (Fig. 17). Boron has been used as an oxidation resistant material for carbon materials, as a surface coating or as a mixture in the formulation of the carbon material (Castro, 1991; McKee, 1991). So, it is possible that the B-C linkages formed in the resin during charring can enhance oxidation resistance during temperature excursion. Figures 16 and 17 show curing process for boron phenolic resin comparatively to CR2830 phenol-formaldehyde resin at different heating rate in synthetic air. The results can prove the superior thermal properties of the boron-modified phenolic resin when compared with the commercial phenolic resin that are in current use at the institute in the thermal protection of the Rocket program. Additionally, the high yield (~70%/mass at 700C) of the resulting carbon from boron-modified resin, compared to the commercial phenolic resin, is a significant result for decreasing the processing time for Carbon/Carbon composite, which consequently reduces the number of cycles required for the pyrolysis/impregnation processes. Results of thermal diffusivity Figure 18 shows the curve of thermal diffusivity for boron phenolic resin. The majority of the polymers have thermal
Figure 16: TG/DTA curves for the cured boron-modified phenolic resin. (A) Rate of heating of 2.5C/min, in synthetic air, weight of the sample = 2.184 mg; (B) Rate of heating of 10C/min, in synthetic air, weight of the sample = 2.2669 mg.

diffusivity in the range of 1.0 x 10-7 and 1.5 x 10-7 m2/s at room temperature (Santos, Mummery and Wallwork, 2005). Thermal diffusivity of unfilled phenolic resin is hardly found in literature. Besides, thermal properties of unfilled polymer materials are given by their thermal conductivity. Anyway, the thermal conductivity of an unfilled phenolic resin at 25C is 0.21 W/m.K and increases to 0.28 W/m.K at 316C (US Army Armament Research, Development, and Engineering Center, 1991). The specific heat of a typical phenolic resin is ~1.2 kJ/ kg.K and the density is ~1250 kg/m3 this results in a thermal diffusivity of ~0.14 mm2/s at 25C, which agrees reasonably with the result found for the boron-modified phenolic resin (Fig. 18). At temperatures higher than 200C, phenolic resin undergoes morphological changes and the thermal conductivity at 316C can only be taken as a reference. Rheological characterization Figure 19 shows results of the storage shear modulus (G), loss modulus (G), Tan d and viscosity () as a function of shear stress (t).

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104 104

tan() ( []

103

G" ( [Pa]

103

102

) G' ( [Pa]

Eta* ( ) [Pa-s]

101

102 10-1

100

[Pa]

101

102

100 103

Figure 19: Elastic modulus (G), loss modulus (G), tan d and viscosity () versus shear stress for boron phenolic resin at room temperature (25C).

Figure 17: TG/DTA curves for a cured CR2830 phenolformaldehyde resin. (A) Rate of heating of 2.5C/ min, in synthetic air, weight of the sample = 2.432 mg; (B) Rate of heating of 10C/min, in synthetic air, weight of the sample = 2.206 mg.

Figure 20 shows the plot of viscosity () as a function of temperature for the boron-modified phenolic resin. It can be seen that the minimum viscosity of the resin reach a value lower than 20 Pa at 60C, keeping it constant up to approximately 200C. This indicates that, in this range of temperature, the cure reaction is latent. This consequently results in benefits for processing as, for instance, a longer pot life for the resin. In this range of temperature (60200C), is not temperature dependent, which characterizes a polymer that contains mainly olygomers.

1800 1600 1400 Viscosity ( *) - Pa.s 1200 1000 800 600 400 200 0 0 25 50 75 100 125 150 175 200 225 Time (s) 250

Figure 18: Thermal diffusivity as a function of temperature for the cured boron-modified phenolic resin.

Figure 20: Dynamic scanning at the rate of 5C/min for shear elastic modulus (G), shear loss modulus (G), tan d and viscosity () at frequency of 1 rad/s and shear stress of 6 Pa.

The shear stress defines the conditions for testing the neat resin, which corresponds to the near newtonian behavior related to the storage shear modulus. For the phenolic boron resin, the chosen value for shear stress was 6 Pa, which corresponds to the region of maximum G. This value was kept constant for all the other tests.

Figure 21 shows graphics of viscosity as a function of time for the boron-modified phenolic resin at isotherm temperatures of 160, 180 and 200C. In this case, it can be seen that cure reactions start at 20 minutes, 13 minutes and 5 minutes, respectively.

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2000 1800 1600 Viscosity / * (Pa.s) 1400 1200 1000 800 600 400 200 0 0 200 400 600 800 1000 1200 1400 1600 Time (s)
o 200 C o 180 C o 160 C

Figure 21: Viscosity as a function of time at temperature isotherms of 160C, 180C and 200C for the boronmodified phenol resin.

For composite processing, results of viscosity as a function of time and temperature are important, since they can define the schedule of the curing cycle. Figure 22 shows the curing cycle that has been proposed for curing composites made with the boron-modified phenolic resin matrix. The curing process started at a heating rate of 3C/min up to 160C. After 60C, the material exhibits adequate flow, which allows the wetting of the reinforcing fibers. After ~30 minutes at 160C, pressure of 0,7 MPa and vacuum are applied to the molding system, for compaction of the layers. After 1 hour at 160C, the curing proceeds up to 220C.

Figure 23: ILSS as a function of deflection for boron-modified phenolic resin composite/silicon fiber.

Figure 22: Curing cycle proposed for the boron-modified phenolic resin for composite preparation.

Figure 24: Comparative results of a ILSS as a function of deflection for composites made from commercial phenolic resin (CR 2830) and silica.

Results of interlaminar shear strength Figure 23 shows the interlaminar shear stress (ILSS) as a function of deflection for boron-modified phenolic resin composite and silica fiber, and Fig. 24 shows comparative results of composites made from commercial phenolic resin and silica fibers.

The results showed that there is no evidence of significant differences in the average values of ILSS for both materials, although there is a gently failure mode of the composite made with commercial phenolic resin in relation to the composite made with boronmodified phenolic resin. This is not a surprise, since interlaminar shear properties are a matrix dominated property.
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Results of Iosipescu shear test The value of the Iosipescu shear strength is around 25 MPa, corresponding to a deformation closer to 1.5%. The shear modulus (G12), calculated at the limit of 20 MPa, was approximately 3.5 GPa, which is a value close to many other polymer composite systems. Figure 25 shows the Iosipescu shear strengh as a function of shear strain for the boron-modified/phenolic resin. Figure 26 shows a representative Iosipescu composite specimen after the test. It can be observed that the failure region is located between the V-notches, which is a representative and valid failure mode for Iosipescu shear.

Figure 26: View of the failure in the central V-notch region of the Iosipescu specimen of boron-modified phenolic resin/silica fiber. Figure 25: Iosipescu shear stress as a function of shear strain for a boron-modified phenolic resin/slica fiber composite.

From DSC analysis it is also possible to see the superiority of the boron resin, comparing to the commercial phenolic resin. ILSS and shear resistance Iosipescu tests have been done in silica fiber and boron phenolic resin composite. ILSS was ~16 MPa for silica fiber/phenolic resin and silica fiber/boron-modified phenolic. The in-plane V-notch Iosipescu shear for silica fiber reinforced with boronmodified phenolic resin was 25 MPa. ACKNOWLEGMENT The authors thanks to Unesp-FEG, Dr. M. L. Costa, for the DSC and rheometer measurements, Wenka Schweiker from ICT (Germany) for some FT-IR measurements and for Dr. D. Camarano, from CDTN/CNEN, for the thermal diffusivity measurement.

CONCLUSIONS A boron-modified phenolic resin was prepared from the reaction of salicyl alcohol and boric acid using the ratio alcohol:acid of 2:1. The resulting compound has been fully characterized by NMR, IR, DSC, TG and elemental analysis, and it showed properties that indicate promising processing applications. It has been cured as composite with silica, and the results were compared with cured commercial phenolic resin. The results of TG of boron phenolic resin showed clearly a superior thermal performance when compared with the commercial ones, that are in use at the Brazilian space program.

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REFERENCES Abdalla, M.O., Ludwick, A., Mitchell, T., 2003, Boron-modified phenolic resin for high performance applications, Polymer, Vol. 44, pp. 7353-7359. America Patash Chem Corp., 1964, British patent 957611.. Ancelotti Jr., A.C., 2006, Efeitos da porosidade na resistncia ao cisalhamento e nas propriedades dinmicas de compsitos de fibra de carbono/resina epxi, Master of Science dissertation, Intituto Tecnolgico de Aeronutica, So Jos dos Campos, SP, Brazil. Bonner, J.G., Hope, P.S., 1993, Compatibilities and reactive blending. In: Folkes, M.J., Hope, P.S., Polymer blends and alloys, Blackie Academic and Professional, London, pp.46-74. Casiraghi, G., et al., 1980, Selective Reactions between Phenols and Formaldehyde. A Superior Synthesis of Salicyl Alcohols, Synthesis, Vol. 2, pp. 124-125. Castro, L.D., 1991, Inhibition of Oxidation of Carbon Materials. PhD Thesis, University of Bath, UK. Clayton, W.A., Fabish, T.J., Lagedrost, J.F., 1969, Thermal Conductivity of Phenolic Chars. Technical Report AFMLTR-69-313, Air Force Materials Laboratory, Wright Air Force Base, Ohio-USA. Costa, L., et al., 1997, Structure-charring relationship in phenol-formaldehyde type resins. Polymer Degradation and Stability, Vol. 56, No 1, pp. 23-35. doi: 10.1016/ S0141-3910(96)00171-1. Fahrenholtz, S.R., Kwei, T.K., 1981, Compatibility of polymer mixtures containing novolac resins, Macromolecules, Vol. 14, pp. 1076-1079. Gao, J.G., Liu, Y.F., Yang, L.T., 1999, Thermal stability of boron-containing phenolformaldehyde resinPolymer Degradation and Stability, Vol. 63, pp. 19-22. Gao, J.G., Liu, Y.F., Yang, F.L., 2001, Structure and properties of boron-containing bisphenol-A formaldehyde resin, European Polymer Journal, Vol. 37, pp. 207-210. Grenier-Loustalot, M.F., et al., 1996, Phenolic resins .2. Influence of catalyst type on reaction mechanisms and kinetics, Polymer, Vol. 37, No 8, pp. 1363-1369. Hirohata, T., Misaki, T., Yoshii, T.M., 1987, Improvement of flame retardance and heat resistance of

bromine, chlorine and boron modified phenolic resins, J Soc Mater Sci Jpn (Engl Transl), Vol. 36, No 401, pp. 184-188. Knop, A., Sheib, W., 1979, Chemistry and application of phenolic resins, Springer-Verlag, Berlin. Knop, A., Pilato, L.A., 1985, Phenolic resins, SpringerVerlag, Berlin. Lemon, P.H.R.B., 1985, Phenol formaldehyde polymers for the bonding of refractories, Brit. Ceram. Trans. J., Vol. 84, N. 2, pp. 53-56. Lenghaus, K., Qiao, G.G., Solomon, D.H., 2000, Model studies of the curing of resole phenol-formaldehyde resins. Part I.The behaviour of ortho quinone methide in a curing resin, Polymer, Vol. 41, No.6, pp. 1973-1979. McKee, D.W., 1991, Oxidation protection of carbon materials, In: Thrower, P.A., editor, Chemistry and physics of carbon, Vol. 23, pp. 173-232. Liu, C.L., et al., 2007, Evolution of microstructure and properties of phenolic fibers during carbonization, Materials Science and Engineering A, Vol. 459, No 1-2, pp. 347-354. Okoroafor, E.U., Villemaire, J.P., Agassant, J.F.,1992, The viscosity of immiscible polymer blends:influences of the interphase and deformability, Polymer, Vol. 33, No 24, pp. 5264-5271. Park, B.D., et al., Polymer, 1999, Vol. 40, No 7, pp. 1689-1699 Santos, W.N., Mummery, P., Wallwork, A., 2005, Thermal diffusivity of polymers by the laser flash technique, Polymer testing, Vol. 24, No 5, pp. 628-634. Schmidt, D.L., Graig, R.D., 1982, Advanced Carbon Fabric-Phenolic for Thermal Protection Application, AFWAL US, AFWAL-TR-81-4136, USA. Segal, C.L., 1967, High Temperature Polymers, Marcel Dekker, New York. Serio, M.A., et al., 1991, Pyrolysis of phenolformaldehyde resin: experiments and modeling. ACS Div. Fuel Chem. Prepr., Vol. 36, No 2, p. 664. Smith, A.L, 1999, Infrared Spectroscopy, John Wiley & Sons, Hoboken, NJ, USA.

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US Army Armament Research, Development, and Engineering Center, SMCAR-BAC-S, 1991, Military Handbook 754 (AR) Plastic Matrix Composites with Continuous Fiber Reinforcement, Picatinny Arsenal, Dover, NJ, USA.

United States Patent and Trademark Office 4 045 398, 1977 . Whitehouse, A.A.K., Pritchett, E.G.K., Barnett, G., 1968, Phenolic Resins, Iliffe Books Ltd., London; American Elsevier, New York.

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doi: 10.5028/jatm.2010.02026510

Institute of Aeronautics and Space So Jos dos Campos Brazil pardini@iae.cta.br

Luiz Claudio Pardini*

Institute of Aeronautics and Space So Jos dos Campos Brazil mloug@yahoo.com.br *author for correspondence

Maria Luisa Gregori

Modeling elastic and thermal properties of 2.5D carbon fiber and carbon/SiC hybrid matrix composites by homogenization method
Abstract: Advanced carbon fiber hybrid carbon-ceramic matrix composites are realizing their potential in many thermostructural components for aerospace vehicles. This work presents ab-initio predictions of elastic constants and thermal properties for 2.5D carbon fiber reinforced carbon-silicon carbide hybrid matrix composites, by using the homogenization technique. The homogenization technique takes properties of individual components of the composites (fiber and matrix) and characteristics of the geometrical architecture of the preform to perform calculations. Ab-initio modeling of mechanical and thermal properties is very attractive, especially during the material development stage, when larger samples may be prohibitively expensive or impossible to fabricate. Modeling is also useful when bigger samples would be prohibitively expensive or impractical. Thermostructural composites made of 2.5D preforms are easy to manufacture in relation to 3D preforms. Besides, 2.5D preforms are also resistant to thermo cycling and have high resistance to crack propagation in relation to ply stacked composites such as unidirectional (1D) and bidirectional (2D) structures. The calculations were performed by setting an overall carbon fiber volume fraction at 40, 45 and 50 for a 2D stacked composite, and volume fraction in Z-direction of 2, 4 and 6. Keywords: Mechanical properties, Carbon-SiC composites, Elastic properties, Thermal properties.

INTRODUCTION Advanced fiber-reinforced composite materials have been widely used in various load bearing structures, from sporting goods to aerospace vehicles. The ever-increasing popularity of fiber-reinforced composites is largely due to their lightweight, high strength, and superior structural durability. The microstructure of composites plays a dominant role in forming all the composite properties, including failure mechanisms. In principle, property characterization of fibrous composites should be based on their precise microstructures. In practice, however, the true microstructures of the composites are often simplified in the characterization models, both geometrically and from the point of view of materials. The degree of simplification depends on the desired engineering accuracy. The theory of homogenization (Yan, 2003) is almost universally applied to characterize fibrous composite properties. Composite homogenization is a mechanics-based modeling scheme that transforms a body of a heterogeneous material into a constitutively equivalent body of a homogeneous continuum. A set of effective properties is obtained for the equivalent homogeneous continuum. Homogenization
Received: 07/04/10 Accepted: 11/05/10

is an essential first step towards the design and analysis of larger scale and load-bearing structures in fibrous composites. The analysis of a multidirectional composite made of a single unidirectional fiber-reinforced lamina is a classical example. In this case, the unidirectional single lamina is first homogenized, each one with a set of effective properties. The laminate is then treated as a layered plate structure, capable of carrying globally applied thermomechanical loads. Composites can be divided according to their temperature use. At high temperatures (T>500C), only composites made with carbon or ceramic matrices and carbon fiber or any other ceramic fibers, as reinforcement, can be used in structural applications. Their outstanding thermomechanical properties overcome the shortcomings of ceramic or metal components. These materials have been largely developed on an empirical basis. Examples of thermostructural composites can be seen in Fig. 1. Carbon fiber reinforced carbon/silicon carbide hybrid matrix composites (CRFC-SiC) are considered to be one of the most potential thermostructural materials for aerospace components (e.g. thermal protection systems of reentry vehicles or rocket engine components) (Naislan, 2005; Bouquet, et al., 2003; Christin, 2002). For example, carbon materials are suitable for high temperature structural
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Pardini, L.C., Gregori, M.L.

(A)

(B)

(C)

(D)

Figure 1: Applications of thermostructural composites. (A) Aircraft brake, (B) preform for a rocket nozzle, (C) vectorable vanes, (D) thermal protection system from Orion capsule.

materials because of their stable mechanical properties such as hardness and wear resistance in inert atmosphere. They are also light and not corrosive, but they exhibit a brittle like fracture. The traditional 2D preforms have high performance in-plane but they are susceptible to delamination. The multidirectional (3D, 4D, 5D, etc.) preforms exhibit an improved isotropy, good delamination resistance and thick part manufacturing capability (Hinders and Dickinson, 1997). By matching the good in plane properties of 2D composites and the high delamination resistance of multidirectional composites, it is possible to obtain a 2.5D reinforced composite. The 2.5D composites can be needled punched, Z-pinned or stitched, as depicted in Fig. 2. Commercially, thermostructural CRFC-SiC composites can be obtained by the routes as shown schematically in Fig. 3. In this case, the starting point is usually a porous carbon fiber reinforced carbon composite. The SiC matrix can be incorporated by the gas phase route (chemical vapor infiltration) from an
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organosilicon gas precursor, by infiltration of silicon in a porous carbon fiber reinforced carbon composite preform or by polymer impregnation and pyrolysis (PIP), using siliconbased polymers as precursors (Heindenreich, 2007; Guiomar, 1996; Interrante et al., 2002). Considering investment, the PIP route is the simplest technique. The modeling of properties in this work considers the use of PIP method. Typically, CFRC-SiC composites have been made of bidirectional woven fabrics which are stacked together or wound to the desired thickness. Composites having 2.5D reinforcement differ from conventional 3D preforms by their fiber volume fraction. For 2.5D fiber reinforced composites fiber volume fraction in the Z-direction can be up to 10%. For a balanced orthogonal 3D composite, the fiber volume fraction can be up to 25% in each fiber axis direction. The insertion of Z direction reinforcement in bidirectional composites makes these composites in-plane crack resistant and allows them to endure many heat treatment cycles.

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(A)

(B)
Figure 2: (A) Z-pinned preform, (B) needled punched preform, (C) stitched preform.

(C)

THE AVERAGE STIFFNESS COMPUTATIONAL METHOD The properties of composites are designed by the selection of the fibers, their volume fraction, orientation, and architecture in the part. The problem is that the properties of the fibers are frequently altered by processing, and the properties of the matrix are even more sensitive to composite architecture and processing. The prediction and modeling of elastic constants for anisotropic materials and particularly for composites use analytical methods such as the Classical Lamination Theory or Finite Element Analysis (Hyer, 1998). Another way to predict elastic properties of composites take into account their microscopic nature, i.e. their intrinsic microstructure. The appropriate combination of the intrinsic properties of reinforcing fibers and matrix is then assumed. This approach is known as micromechanics, which is a study of the mechanical or thermal properties of composites, in terms of those of constituent materials. General assumptions in micromechanics of composites are: composite are macroscopically homogeneous and orthotropic, linearly elastic, initially stress free, and free of voids. Besides, it is assumed that there is complete bonding at the interface of the constituents and there is no transitional region between them. The displacements are continuous across the fiber matrix interphase (there is no interfacial slip). Fibers are homogeneous, linearly elastic, isotropic or orthotropic/transversely isotropic, regularly spaced, perfectly aligned, circular in cross-section and infinitely

Figure 3: Commercial process routes used to obtain Carbon fiber reinforced carbon-silicon carbide composites.

long in the longitudinal direction. Matrix is homogeneous, linearly elastic and isotropic. If any temperature effects are considered, the constituent material properties have to be known at a given temperature. The process of smoothing out quantities which vary on a microstructural lengthscale (lying between the atomic and macroscopic scales) is used in order to obtain some effective macroscopic properties. A set of effective properties is obtained for the equivalent homogeneous
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continuum. Of course, all matter is inhomogeneous at some scale, but frequently it is convenient to treat it as homogeneous. A good example is the continuum concept used in continuum mechanics. The Fig. 4A shows a representation of a unidirectional composite cross-section. An increase in the representative volume element (RVE), as showned by dotted lines, leads to a higher degree of homogeneity. Fig. 4B, on the other hand, shows schematically the effect of smoothing a generic asymptotic function that converges to a medium average value as the window length of the RVE is increased. This process of replacing an equation with a highly oscillatory coefficient for a homogeneous (uniform) coefficient is known as homogenization, which is linked to the subject of micromechanics. As a result, homogenization can be viewed as an extension of the continuum concept to materials which possess microstructure. The RVE is the analogue of the differential element in the continuum concept, which contains enough atom, or molecular structure to be representative of that material in homogenization and micromechanics. This RVE contains enough statistical information about the inhomogeneous medium in order to be representative of the material. Therefore, averaging over this element gives an effective property to fibrous composites, and so the homogenization is an essential first step towards the design and analysis of larger scale and load-bearing structures. The analysis of multidirectional composites made of unidirectional single lamina is a classical example. In this case, the unidirectional single lamina is first homogenized, each one with a set of effective properties. The laminate is then treated as a layered plate structure capable of

carrying globally applied thermomechanical loads. For the reader, it is useful to review some points related to micromechanics for a better understanding of the average stiffness method, which is the basis of the elastic and thermal properties calculations. The micromechanics approach is therefore used for elastic and thermal properties calculations. In the Classical Lamination Theory, for instance, the development of a procedure to evaluate stress and strain relations of composite laminates is fundamentally dependent on the fact that their thickness is much smaller than its plane dimensions. Typical thicknesses for individual composite layers can range from 0.10 to 0.25 mm. Consequently, composites having from 5 to 50 layers are considered thin plates and can be analyzed bearing in mind the simplifications of the thin plate theory. In the case of perfectly aligned fibers in a composite, as shown in Fig. 5, assuming linear elastic behavior and perfect adhesion, the Rule of Mixtures is applied, Eq. (1) (Matthews and Rawling, 1994). The equation is a representation of the composite longitudinal elastic modulus (E11). The subscripts refer to the main reinforcement direction and the direction of applied stress, respectively. The transverse modulus (E22) of the composite is defined by Eq. 2.
E11 = E fiber V fiber + Ematrix Vmatrix

(1) (2)

E22 =

(V fiber Ematrix ) + (Vmatrix E fiber )

E fiber Ematrix

(A)

(B)

Source: Thomas et al., 2008. Figure 4: (A) Representative model of a unidirectional composite showing an increase in size of the representative volume element (RVE) and (B) asymptotic function model showing conversion to a medium value.
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properties of the homogenized fiber (Fig. 6B) are obtained. The second level refers to fictitious multidirectional composite, having tows of fibers (rods) homogenized (Fig. 6C). The regularly spaced fibers in the composites allow to determine the representative volume element (Fig. 6D), and to evaluate the homogenized material (Fig. 6E) in terms of macroscopic quantities (global) (Pastore and Gowayed, 1994; Gramoll, Freed and Walker, 2001).

Figure 5: Schematic representation of a unidirectional (1D) composite and main axis. (A)

Where Efiber is the modulus of reinforcement, Ematrix is the matrix modulus, Vfiber is the volume fraction of fibers, Vmatrix is the volume fraction of matrix. The in-plane shear modulus (G12) of a unidirectional composite is given by Eq. (3). Both the transverse and shear modulus are strongly influenced by the matrix modulus (Gmatrix).

(B)

(D) (C) (E)

G12 =

(V fiber Gmatrix ) + (Vmatrix G fiber )

G fiber Gmatrix

(3)

Where Gfiber is the shear modulus of the fiber, Gmatrix is the matrix shear modulus, Vfiber is the fiber volume fraction, Vmatrix is the matrix volume fraction. For transversely isotropic materials, properties of the material in directions 2 and 3, from Fig. 5, are almost the same and are transversely isotropic to the direction 1. So, the following identities are valid: E22 = E33, n12 = n13, G12 = G13, and:

Figure 6: The hierarchical constitutive model: (A) unit cell, (B) composite rod, (C) representative unit of the fiber as unidirectional reinforcement, (D) preform representation and unit cell of the composite, (E) homogenized composite.

G23 =

E22 2 (1 + v23 )

(4)

Where n12, n13 and n23 are Poisson ratios, where the first subscript refers to the direction of stress and the second subscript refers to the direction of contraction. The numerical procedure for the analysis of composites assumes the following hypotheses: (i) regular distribution of fibers in the tow and, (ii) regular assembly of fibers in the unidirectional composite rod. These hypotheses allow figuring out the problem of property estimation in the scope of micromechanics theory of periodic microstructure heterogeneous materials, corresponding to two levels of homogenization (Yan, 2003: Pastore and Gowayed, 1994; Gramoll, Freed and Walker, 2001). The first level refers to the fibers, which are analyzed independently by the rule of mixture model. Each unidirectional fiber forms the composite (Fig. 6A) having the fiber volume fraction similar to the packing density. So, the mechanical

This model is described as Fabric Geometry Model - FGM (Pastore and Gowayed, 1994), which is based on the idea that the elastic properties of the composite can be calculated as a function of the relative proportion of the properties of the fibers, at specific directions, and the matrix. In summary, the composite is analytically divided in volume elements (unit cell) composed of composite rods. Each unidirectional reinforced rod has its own fiber volume fraction and from their vetorially oriented contributions forms the properties of the homogenized composite. The properties of each direction, represented by the composite rod in the unit cell, are calculated and the results for elastic constants refer to the local axis system (1-2-3), as shown in Fig. 7.
Z

3 1 c 2 b Y a X

Figure 7: Local axis system (1, 2, 3) and global axis system (x, y, z) of coordinates, and 1, 2 and 3 are orthogonal.
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The axis transformation from the stiffness matrix (C) and compliance (S) can be obtained by means of stress/ strain transformation axis (Pastore and Gowayed, 1994; Gramoll, Freed and Walker, 2001). The resulting equation from axis transport for the stiffness matrix can be obtained as shown in Eq. (5).
[Cglobal ]=[K][T][Clocal ][K]

(8)

(5)

Where [Cglobal] is the matrix stiffness in the global axis system (x,y,z), [K] is the stress/strain transportion matrix, [Clocal] is the stiffness matrix in the local axis system (1-23), and T is the transformation matrix. The transformation of constants from the local system to the global system is done by a transformation matrix composed of entities related to direction cosines (angles q and a, respectively related to elevation and azimuth) from orientation of the rods. So, due to orthogonality only the Te matrix is needed, which is represented in Eq. 6. The li, mi and ni are direction cosines components of the unit basis vectors associated with the principal axes of the fibrous reinforcement.

Where Ccomp is the composite stiffness matrix, Vfiber is the total fiber volume fraction, Vfiber-i is the relative fiber volume fraction from the i-esime unidirectional composite rod, Ci is the stiffness of the i-esime unidirectional composite rod and n is the number of unidirectional composite rods. The thermal properties (thermal conductivity and coefficient of thermal expansion) were also calculated on the basis of average properties from the individual constituents of the composite by using the Fabric Geometry Model FGM. During transient heat flow, transverse heat flow between the fiber and the matrix is expected to occur. This is the case for materials with significantly different thermal conductivities. If their interfaces are negligible in thickness, the longitudinal thermal conductivity of the composite will only be affected by the fibers and the matrix thermal conductivities, and will be unaffected by the fibers/ matrix interface according to Eq. 9. (9) Where kc(//) is the thermal conductivity parallel to the fiber direction, kfiber and kmatrix are the thermal conductivity of the fibers and matrix, respectively and Vfiber and Vmatrix are the volume fraction of the fibers and matrix, respectively. The thermal conductivity in the perpendicular direction of the composite is calculated by means of Eq. 10.

(6)

In Fig. 7 the axis 1 is related to vector r1, which is the unit vector associated with fiber axis (l1, l2, l3), the axis 2 is related to vector r2, which is the unit vector associated with #2 direction of the fiber (m1, m2, m3), and axis 3 is related to vector r3, which is the unit vector associated with #3 direction of the fiber (n1, n2, n3). The vector r1 can be known by solving the geometrical relationship represented by Eq. (7). The other two vectors can be known by solving through geometric relationships. Because they are mutually orthogonal, it can be proved that r1.r2 = 0, r2.r3 = 0 e r1.r3 = 0. As they are direction cosines vectors, ||r1|| = ||r2|| = ||r3|| = 1, and a, b and c are the edges of the unit cell.

(10)

(7)

Where (diagonal)2= a2 + b2 + c2. The contribution from each rod in the direction of the global axis system is done by the superposition of the stiffness matrix or flexibility matrix transposed for the global system, as shown by Eq. 8 (Pastore and Gowayed, 1994).
188

Where kc (^) is the thermal conductivity perpendicular to the fiber direction, kfiber (//) is the thermal conductivity parallel to the fiber, .kmatrix(//) is the thermal conductivity parallel to the matrix, and Vfiber and Vmatrix are the volume fraction of the fibers and matrix, respectively. For modeling the coefficient of thermal expansion, each phase is assumed homogeneous and isotropic and linearly elastic over a small range of volumetric strains. In the absence of the phase interaction, one may expect

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Modeling elastic and thermal properties of 2.5D carbon fiber and carbon/SiC hybrid matrix composites by homogenization method

the coefficient of thermal expansion of a composite, with a reasonable approximation, to follow the simple rule of mixtures. However, because of the differences in the thermal expansivities of the phases (fiber and matrix), a state of micro-stress often exists between them, influencing the thermal expansion behavior of the body and giving rise to discrepancies. Thus, its thermal expansion coefficient does not follow the rule of mixtures (Thomas et al., 2008; Mukerji, 1993). Karadeniz and Kumlutas (2007) investigated the existing theories for prediction of coefficient of thermal expansion based on micromechanics and finite element analysis, considering the fiber volume fraction ranging from 10 to 90% for the studied composites (Mukerji, 1993). The theories agreed quite reasonably for calculation of the thermal expansion coefficient in the main fiber axis direction (a1), at least for ordinary unidirectional polymer matrix composites, even compared with sophisticated modeling techniques, such as finite element calculations, for a range of fiber volume fractions (Mukerji, 1993). Nevertheless, for the transverse direction (a2), the rule of mixtures seems to have a better agreement with finite element calculations than other micromechanical theories. The coefficient of thermal expansion for composite materials is a function of stress and strain in the matrix and fiber, according to Eq. (11). (11)

(12)

If there is free expansion in the direction of the fiber, e1 = a1.T, where a1, it is according to Eq. (13) as follows:

(13)

For the transverse direction to the fiber axis, the coefficient of thermal expansion (a2) is obtained as shown in Eq. (14), as follows:

(14)

RESULTS FOR AVERAGE STIFFNESS 2.5D CARBON FIBER REINFORCED C/SIC HYBRID MATRIX COMPOSITES For the prediction of the mechanical properties of 2.5D CFRC-SiC composites through the micromechanics method, it is necessary initially to establish representative properties of the carbon fiber, the carbon matrix and the silicon carbide matrix. Mechanical properties of carbon fibers are well documented in the literature (Peebles, 1994; Inagaki, 2001; Asakuma et al., 2003). Table 1 shows the properties of carbon fiber, SiC matrix and carbon matrix found in literature. The best value for the properties of a carbon matrix can rely on synthetic graphite mechanical and thermal properties (Inagaki, 2001). Synthetic graphites are obtained by a controlled pyrolysis process, up to 2500oC, from a mixture of pitch and coke. In relation

Considering ecomp = ematrix = efiber, in the fiber direction, the Eq. (12) is obtained.
Table 1:

Properties of carbon fiber, SiC matrix and carbon matrix reported in the literature and from manufactures data

Temperature (C)

Elastic modulus (GPa) Longitudinal 230 230 230 Transversal 20 20 20 Shear modulus (GPa) 12 12 12 0.18 Poisson Ratio n Density (g/cm3) 1.78 k (W/m.K) Longitudinal 8.40 Transversal 0.84 a (10-6/C) Longitudinal 18 Transversal 1.2 *calculated based on Nicalon CG fiber. Source: Peebles (1994), Inagaki (2001), Asakuma (2003).

RT

Carbon fiber 1000 1200

RT 225 225 75

SiC matrix* 1000 1200 225 225 75 0.14 2.55 1.768 1.377 0.164 225 225 75

RT 10 10 4.2

Carbon matrix 1000 1200 10 10 4.2 0.18 1.80 60 10 10 4.2

120

55

-0.6

1.5

2.0

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to other carbon matrix materials obtained from gas phase deposition or thermoset resin pyrolysis, the mechanical properties of synthetic graphite are lower. A reasonable estimation of the elastic properties of a carbon matrix based on pitch coke, which is nearly the same of other graphitic materials, was reported by Asakuma (Asakuma et al., 2003). Silicon carbide can be obtained by a number of techniques, and the most common are hot pressing and chemical vapor deposition. In this manner, their properties can vary greatly depending on the method of preparation and the final microstructure obtained. But only few works have mentioned properties of silicon carbide obtained by any of the silicon polymer pyrolysis methods, possibly because of the difficulties of getting representative samples for traditional mechanical tests, such as tensile strength. On the other hand, mechanical properties for hot pressed silicon carbide only rely on flexural strength or compressive strength, and respective modulus, mainly because covalent ceramics are not suitable for use under tensile loads. Reported values for flexural strength of hot pressed SiC can be up 450 MPa (Mukerji, 1993). Somiya and Inomata (1992) found for a CVD-SiC material, tested under three-point bending values in the range of 200690 MPa, and in this work a tensile strength of 590 MPa was also reported. The best combination of properties was obtained for CVD-SiC having a 1.5-m grain size (Munro, 1997). The Youngs modulus of typical hot-pressed SiC materials is reported in the range of 275-465 GPa. The characterization of tensile strength of SiC, as any other covalent ceramic, is hardly difficult because they are prone to surface defects due to machining and by other inadequate specimen preparation procedures which leads to misleading measurements. Besides, tensile strength of SiC has a low value compared to their flexural and compressive strength. This is the reason why the uses and the mechanical characterization of SiC are practically done under flexure or compressive loading. In fact, the tensile tests lead to conservative results in relation to the other types of tests, such as flexure tests, and, as a consequence, the tensile strength can be much lower than flexural strength. Munro (1997), for instance, found a tensile strength of ~250 MPa for a hot pressed a-SiC, from 25oC to 1400oC. The best known SiC material obtained from silicon polymer pyrolysis is the Nicalon fiber (Yajima et al., 1979). Although the Nicalon SiC fiber varies in composition, it represents the properties of a typical polymer ceramic silicon carbide matrix. The chemical composition of Nicalon ceramic grade fiber has typically ~65% SiC, ~15% carbon and ~20% SiO2. At room temperature, its Youngs
190

modulus is ~200 GPa and the tensile strength is 3.0 GPa. If considered isotropic, the shear modulus of Nicalon ceramic grade fiber is ~87 GPa, considering the relation E=2G(1+n), but experimental results show values near 75 GPa for fibers processed at 1200oC. Increasing the test temperature up to 1200oC causes no noticeable changes on Youngs modulus and in the shear modulus (Villeneuve and Naslain, 1993). Studies conduced by Sorar, Dallapiccola and Dndrea (1996) on SiCxOy glasses synthesized by the sol-gel method found a Youngs modulus of 115 MPa for these materials. For SiCxOy glasses, the properties beyond 1200oC fall rapidly. The prediction of elastic and thermal properties for carbon fiber reinforced carbon-SiC hybrid matrix was done by taking the properties of Table 1, for carbon fiber, SiC matrix and carbon matrix. In this case, the properties of the SiC matrix were considered as similar to the SiC fiber which is the best approximation for a typical amorphous polymer ceramic Si-C-0 matrix. For composites made with ceramic matrices, processed by the polymer impregnation method, porosity in the range of 5 to 20% is usually attained (Rice, 1999). In this work, for comparison purposes and for good of prediction, it is considered a composite having ~5% volume porosity, and carbon fiber volume fraction of 40, 45 and 50%. The carbon matrix volume fraction will vary from 35, 30, and 25%, respectively to carbon fiber volume fraction, as shown in Table 2. The volume of SiC polymer ceramic matrix is kept, also for comparison purposes, at 20% volume fraction. In the calculations, the out-of-plane Z fiber addition is considered to be uniformly distributed throughout the composite. So, properties of the CFRC-SiC composite can be varied by taking the relative proportions of carbon and silicon carbide, according to the rule of mixture, as shown in Table 2. It is important to point out that mechanical properties are approximately constant from room temperature to 1200oC for these composites. From input parameters from Table 1 and Table 2, the output parameters processed by the FGM model such as local resilient matrix and stiffness matrix, and global stiffness matrix, are obtained, as shown in Table 3, related to the direction cosines of a unidirectional composite. Results from Table 3 leads to elastic and thermal properties showed in Table 4. The elastic modulus for bidirectional Carbon Fiber Reinforced C/SiC Hybrid Matrix was also calculated, for comparison purposes. It is hardly difficult to find properties of C-SiC composites mainly because differences in the processing routes, type of carbon fiber used, level of porosity in the composite and C/SiC matrix ratio. Besides, fiber volume fraction can vary from one material to another and mechanical properties are mostly found as manufactures data sheet rather than a rigorous scientific research. Moreover, for the

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Table 2:

Properties of hybrid matrices of carbon/silicon carbide related to volume fractions of carbon and silicon carbide used for modeling the properties of CFRC/SiC-modified composites

Total carbon fiber volume fraction (%) Carbon matrix volume fraction (%) SiC matrix volume fraction (%) Void volume fraction (%) C/SiC matrix ratio Density (g/cm3) Tensile strength (MPa) Elastic Modulus (GPa) Shear modulus* (GPa) Poisson ratio k (W/m.K) a (10-6/oC) *calculated by E=2G(1+n).

40 35 20 5 65/35 2.06 145 82 28 0.17 79 1.00

45 30 20 5 60/40 2.10 165 96 32 0.16 72 1.04

50 25 20 5 55/45 2.14 180 105 35 0.15 66 1.17

Table 3:

Direction cosines, transformation matrix, local resilient matrix, local stiffness matrix and composite stiffness matrix for a CFRC-SiC unidirectional composite model 1 0 1 0 0 0 0 0 0 0 1 0 0 0 0 0 0 0 0 1 0 0 1 0 0 0 0 0 1 0 0 0 0 0 0 0 0 1 1

Direction cosines Transformation matrix

1 0 0 0 0 0

Local resilient matrix -0.00110448 0.00597015 -0.00110448 0.0297619 -0.00110448 -0.00748348 0 0 0 0 0 0 Local stiffness matrix

-0.00110448
-0.00748348 0.0297619

0 0 0
8.4592 9.4381 36.2871

0 0 0 0.047619 0 0 0 0
0 21.0000

0 0 0 0 0.0744908 0 0 0 0 0
13.4245

0 0 0 0 0 0.047619 0 0 0 0 0
21.0000

170.6299 8.4592 8.4592

8.4592 36.2871 9.4381

0 0 0 0 0 0 Composite stiffness matrix

0 0 0
8.4592 9.4381 36.2871

0 0 0 0
0 21.0000

0 0 0 0 0
13.4245

170.6299 8.4592 8.4592

8.4592 36.2871 9.4381

0 0 0

0 0 0

0 0 0

0 0

0 0 0 0 0
21.0000

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Table 4:

Properties of unidirectional (1D) carbon fiber reinforced C/SiC hybrid matrix

Table 5:

Properties of bidirectional (2D) carbon fiber reinforced C/SiC hybrid matrix

Total carbon fiber volume fraction (%) C/SiC matrix ratio E11 E22 E33 G12 G23 G13 12 13 23 k11 k (W/mK) k22 k33 a11 a22 a (10-6/C) a33

40 65/35 141 36 36 20 14 20 0.18 0.18 0.25 57 35 35 0.12 0.68 0.68

45 60/40 156 35 35 21 14 21 0.18 0.18 0.25 50 30 30 0.70 0.34 0.34

50 55/45 167 33 33 21 13 21 0.18 0.18 0.25 45 25 25 1.05 0.63 0.63

Total carbon fiber volume fraction (%) C/SiC matrix ratio E11 E22 E33 G12 G23 G13 12 13 23 k11 k (W/mK) k22 k33 a11 a(10-6/C) a22 a33

40 65/35 89 89 37 20 17 17 0.07 0.23 0.23 46 46 35 0.56 0.56 0.04

45 60/40 96 96 36 21 17 17 0.06 0.22 0.22 40 40 30 0.92 0.92 0.54

50 55/45 98 98 37 21 18 18 0.06 0.21 0.21 38 38 28 0.97 0.97 0.60

majority of applications, the Z reinforcement has the main purpose of holding together the bidirectional stacks of fiber reinforcement fabrics, improving interlaminar shear and through-the-thickness fracture toughness than truly improve through-the-thickness elastic or thermal properties. So, with a reasonably approximation, the calculated properties using the Fabric Geometry Model can be compared with 2D CRFC-SiC composites. For instance, Wang et al. (2008) found for a 2D CFRC-SiC composite processed by CVI technique, having 40%/volume of fibers and 13% porosity, a Youngs modulus of 959 GPa. Arendts and Maile (1998) reported a Youngs modulus of 70-80 GPa for a 2D CRFCSiC composite obtained by polymer pyrolysis having 8%/ volume porosity, and a Youngs modulus of 50-70 GPa for a 2D CRFC-SiC composite processed by liquid silicon infiltration, having 5%/volume porosity and 40% fiber volume fraction. Nie et al. (2008) found a Youngs modulus of 81 GPa for a 2D CFRC-SiC matrix, obtained by the CVI technique, having 40% volume fraction of carbon fibers and 11%/volume porosity. In the same work, stitched carbon fiber fabrics processed in the same way exhibited a Youngs modulus of 62-64 GPa. Nie et al. (2009) also found a Youngs modulus of 754 GPa for a needled carbon fiber densified with a SiC matrix, obtained by the CVI technique. These properties can be compared with those shown in Table 5 and Table 6. It is well known that Youngs modulus of composites is mainly dependent on fibers properties and on their volume fraction. In the present work, the calculated elastic modulus for unidirectional CFRC-SiC composites, in the fiber direction, ranges from 140 to 170 GPa, and from 36 to 33 GPa,
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perpendicularly to fiber direction, considering a fiber volume fraction from 40 to 50%, respectively. For the 2D CFRCSiC composite, elastic modulus range from 90 to 100 GPa, considering a fiber volume fraction from 40 to 50%. For the 2D CFRC-SiC composites having Z-reinforcement ranging from 2 to 6%, elastic modulus range from 80 to 95 GPa in the plane of reinforcement, and from 43 to 57 GPa in the out-ofplane direction, considering a total fiber volume fraction from 40 to 50% in the composite. Heidenreich (1997) resumed data on properties of C-SiC composites obtained from many companies. For instance, C-SiC composites obtained by CVI technique, having 45% fiber volume fraction, had the elastic modulus reported as 90-100 GPa. In the same work, C-SiC composites obtained by liquid polymer infiltration and by liquid silicon infiltration had the elastic modulus reported as 65 GPa (Heidenreich, 2007). Although these data are from various material types, it is possible to infer that the calculated values from this work, as shown in Tables 5 and 6, are reasonably in the range of those found in the literature. The thermal properties depend on the axis of measurement and are mainly influenced by the carbon fiber. Calculation for thermal conductivity of CRFC-SiC composites (Table 6) are in the range from 32 to 46 W/m.K. The survey of properties of C-SiC composites, obtained by Heidenreich (1997), shows more conservative results for thermal conductivity, which are in the range of 5 to 20 W/m.K, although values up to 40 W/m.K can be found. These differences can be attributed to the differences on the manufacturing method and the presence of pores and microcracks which are not exactly accounted in Fabric Geometry Model. Thermal expansion coefficients calculated by the Fabric Geometry Model for

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Table 6:

Properties of 2.5D carbon fiber reinforced C/SiC hybrid matrix, having 5% volume porosity, from RT to 1200C

Total fiber volume fraction (%) C/SiC matrix relation Fiber volume Z direction (%) E11 E22 E33 G12 G23 G13 n12 n13 n23 k11 k (W/mK) k22 k33 a11 a (10-6/oC) a22 a33

2 86 86 43 21 17 17 0.09 0.19 0.19 46 46 37 0.50 0.50 0.15

40 65/35 4 83 83 48 22 17 17 0.11 0.17 0.17 45 45 37 0.50 0.50 0.22

6 79 79 53 22 17 17 0.13 0.14 0.14 45 45 39 0.50 0.50 0.30

2 91 91 44 22 18 18 0.09 0.18 0.18 42 42 34 0.90 0.90 0.66

45 60/40 4 87 87 50 23 23 18 0.11 0.16 0.16 42 42 35 0.90 0.90 0.72

6 84 84 56 24 18 18 0.12 0.12 0.14 42 42 36 0.88 0.88 0.77

2 94 94 45 23 23 19 0.08 0.18 0.18 40 40 32 0.96 0.96 0.74

50 55/45 4 90 90 51 24 24 19 0.10 0.15 0.15 39 39 33 0.94 0.94 0.80

6 86 86 57 24 24 19 0.12 0.12 0.13 39 39 34 0.94 0.94 0.84

the CFRC-SiC composites are in the range of 0.15x10-6/C to 1x10-6/C, which are in the range (-1x10-6/C to 6x10-6/C) showed in the survey of properties of C/SiC materials of the work of Heindenreich (2007). CONCLUSION This work described a simple method for estimation of the elastic and thermal properties of 2.5D carbon fiber reinforced carbon-SiC hybrid matrix composites. These materials are the state-ofthe-art composites for use in thermal protection systems. The Z-direction reinforcement allows higher delamination resistance and endurance on thermal stresses generated by heat treatment processing, and also the interlaminar fracture toughness is improved. Mechanical and thermal properties of 2.5D CRFC-SiC composites were calculated based on composite average stiffness micromechanics. The modeling of properties by this simple method allows avoiding costly testing and reducing time consuming specimen preparation. Mechanical properties of composites are fiber dominated. Calculations were done by considering the total carbon fiber volume fraction in the range of 40 to 50%, which are commonly found in carbon and ceramic composites reinforced with carbon fibers. The addition of only 2% of fibers out of the main plane of reinforcement increases the elastic modulus in the out-of-plane direction by about 20%. An increase in the carbon fiber volume fraction from 40 to 50%, results in higher elastic properties, but nevertheless decreases the thermal conductivity. The calculated inplane Youngs modulus is in the range of 84 to 94 GPa,

and the out-of-plane Youngs modulus is in the range of 43 to 57 GPa. The calculated shear modulus is in the range of 17 to 24 GPa, regardless of the plane of shear stress. The calculated thermal conductivity of 2.5D carbon fiber reinforced carbon-SiC hybrid matrix composites was found to be in the range of 32 to 46 W/m.K, and the calculated coefficient of thermal expansion was in between 0.15.10-6/C to 0.94.10-6/C. These results agreed in some extent to values found in the literature for similar materials. The knowledge of the envelope of elastic and thermal properties of carbon and ceramic composites made with carbon fibers allows ab initio modeling thermoelastic properties of composites. These properties can be easily calculated by taking individual properties of each component (fiber and matrix) and the relative proportions of these components in the composite which is the essence of the homogenization theory. REFERENCES Arendts, F.J., Maile, K., 1998, Thermomechanicshes Verhalten Von C/C-SiC. Arebeits-und Ergebnisbericht SFB 259. Asakuma, Y., et al., 2003, A New estimation method of coke strength by numerical, Multiscale Analysis ISIJ International, Vol. 43, No 8, pp. 1151-1158. Bouquet, C., et al., 2003, Composite technologies development status for scramjet applications, In: 12th AIAA international space planes and hypersonic systems
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and technologies, Norfolk, Virginia, December 15-16, AIAA-2003-6917. Christin, F., 2002, Design, fabrication, and application of thermostructural composites (TSC) like C/C, C/SiC, and SiC/SiC composites, Adv Eng Mater, Vol. 4, No 12, pp. 903-912. Gramoll, K.C., Freed, A. L., Walker, K. P., 2001, An overview: of self-consistent methods for fiber reinforced composites, NASA-TM 103713. Guiomar, N., 1996, Caractrisation physico-chimique et microstructurale de ceramiques sic issues de polymeres precurseurs application a llaboration de composites a matrices ceramiques, Tese de Doutorado, Universit Paris 6, 212 p. Heidenreich, B., 2007, Carbon fibre reinforced sic materials based on melt infiltration, 6th International Conference on High Temperature Ceramic Matrix Composites, New Delhi , India, 6 p, Sep 4-7. Hinders, M.; Dickinson, L., 1997, Trans-laminar (TLR) reinforced composites, NASA CR-204196. Hyer, M.W., 1998, Stress Analysis of Fiber-Reinforced Composite Materials, McGraw Hill Intl. Edition, USA. Inagaki M., 2001, Applications of polycrystalline graphite, In: Graphite and Precursors, P. Delhaes, Gordon and Breach Science Pub., UK. Interrante L.V., et al., 2002, Silicon-based ceramics from polymer precursors, Pure Appl. Chem., Vol. 74, No 11, pp. 2111-2117, 2002. Karadeniz Z.H., Kumlutas, M., 2007, A numerical study on the coefficients of thermal expansion of fiber reinforced composite materials., Composite Structures, Vol. 78, No 1, pp. 1-10. Matthews F.L., Rawling R. D., 1994, Composite materials: engineering and science, Cambridge - UK, Chapman & Hall. Mukerji, J., 1993, Ceramic Matrix Composites, Defence Science Journal, Vol. 43, No 4, pp. 385-395. Munro, R.G., 1997, Material Properties of a Sintered a-SiC. Journal of Physical and Chemical Reference Data, Vol. 26, No 5, p. 1195-1203. Naislan, R., 2005, SiC-matrix composites: nonbrittle ceramics for thermo-structural application, Int J Appl Ceram Techn, Vol. 2, No 2, pp. 75-84.

Nie, J. et al., 2008, Effect of stitch spacing on mechanical properties of carbon/silicon carbide composites, Composites Science and Technology, Vol. 68, pp. 2425-2432. Nie, J. et al., 2009, Microstructure and tensile behavior of multiply needled C/SiC composite fabricated by chemical vapor infiltration, Journal of Materials Processing Technology, Vol. 209, pp. 572-576. Pastore, C.M., Gowayed, Y. A., 1994, A self-consistent fabric geometry model: modification and application of a fabric geometry model to predict the elastic properties of textile composites. Journal of Composites Technology and Research, Vol. 16, No 1, p. 32-36C. Peebles, L.H., 1994, Carbon fibers: formation, structure, and properties, CRC Press, Boca Raton. Rice, R.W., 1999, Effects of amount, location, and character of porosity on stiffness and strength of ceramic fiber composites via different processing, Journal of Materials Science, Vol. 34, pp. 2769-2772. Somiya, S., Inomata, Y., 1992, Silicon Carbide Ceramics-2, Gas Phase Reactions, Fibers and Whisker Joining, Elsevier Applied Science, London. Sorar, G. D., Dallapiccola, E., Dndrea, G., 1996, Mechanical characterization of sol-gel-derived silicon oxycarbide glasses. Journal of the American Ceramic Society, Vol. 79, No 8, pp. 2074-2080. Thomas, M. et al., 2008, Estimation of effective thermal conductivity tensor from composite microstructure images, 6th International Conference on Inverse Problems in Engineering: Theory and Practice, Journal of Physics, Conference Series 135, 012097. Villeneuve, J.F., Naslain, R., 1993, Shear moduli of carbon, Si-C-O, Si-C-Ti-O and Alumina Single Ceramic Fibers as Assessed by Torsion Pendulum Tests, Composites Science and Technology, Vol. 49, pp. 191-203. Wang, Y., et al., 2008, Characterization of tensile behavior of a two-dimensional woven carbon/silicon carbide composite fabricated by chemical vapor infiltration, Materials Science and Engineering, A 497, pp. 295-300. Yajima, S., et al., 1979, Development of a SiC fiber with high tensile strength, Nature, Vol. 261, pp. 683-685. Yan, C., 2003, On homogenization and de-homogenization of composite materials, Philadelphia, PhD Thesis, Drexel University, USA.

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doi: 10.5028/jatm.2010.02026910

Daniel Soares de Almeida*

Institute of Aeronautics and Space So Jos dos Campos Brazil dsalmeida@iae.cta.br

Carlos Alberto Alves Cairo

Institute of Aeronautics and Space So Jos dos Campos Brazil ccairo@iae.cta.br

Thermal barrier coating by electron beam-physical vapor deposition of zirconia co-doped with yttria and niobia
Abstract: The most usual ceramic material for coating turbine blades is yttria doped zirconia. Addition of niobia, as a co-dopant in the Y2O3-ZrO2 system, can reduce the thermal conductivity and improve mechanical properties of the coating. The purpose of this work was to evaluate the influence of the addition of niobia on the microstructure and thermal properties of the ceramic coatings. SEM on coatings fractured cross-section shows a columnar structure and the results of XRD show only zirconia tetragonal phase in the ceramic coating for the chemical composition range studied. As the difference NbO2,5-YO1,5 mol percent increases, the tetragonality increases. A significant reduction of the thermal conductivity, measured by laser flash technique in the zirconia coating co-doped with yttria and niobia when compared with zirconia-yttria coating was observed. Keywords: TBC, EB-PVD, Zirconia, Niobia, Thermal conductivity.

Cosme Roberto M. Silva

University of Braslia Braslia Brazil cosmeroberto@gmail.com

National Institute for Space Research So Jos dos Campos Brazil maria@las.inpe.br *author for correspondence

Maria do Carmo A.Nono

INTRODUCTION The great advantage of coatings is that it is possible to modify its response to the environment by changing only the superficial part of the component, thus providing completely different properties. Some of the obtained benefits are: reduction of maintenance costs, increase of the working temperature, reduction of thermal loads, resistance increase to erosion and corrosion and reduction of the high temperature oxidation (Funatani, 2000). The electron beam-physical vapor deposition (EB-PVD) process enables to attain coatings with unique properties. The process parameters are adjusted so that the deposit has a columnar grain structure perpendicular to the interface. This morphology maximizes the resistance to strains that arise from differences in thermal expansion coefficients. Other advantages are: aerodynamically favorable smooth surface, better interaction with the substrate, greater thermal cycle tolerance and, hence, greater lifetime comparativeness with the plasma spray process (Xu, Goug and Deng, 1998; Schulz et al., 2000; Evans et al., 2001; Zhu et al., 2000; Goward, 1998; Nicholls, Deakin, Rickerby, 1999; Czek et al., 1999; Hass, 2001; Almeida et al., 2007 and 2006; Nicholls et al. 2002; Guo and Wang, 1998). There are four primary constituents in a thermal protection system. They comprise: (1) the thermal barrier coating (TBC) itself based usually on ~8 wt.
Received:19/05/10 Accepted:14/06/10

% (8.7 mol % YO1.5) yttria stabilized zirconia; (2) the metallic component, treated here as the substrate; (3) an aluminium containing bond coat (BC) located between the substrate and the TBC; and (4) a thermally grown oxide (TGO), predominantly a-alumina, that forms between the TBC and the bond coat. The TBC is the thermal insulator, the bond coat provides oxidation protection, since the zirconia is essentially transparent for the oxygen at high temperatures, and the metallic component, usually a nickel base super-alloy, sustains the structural loads. The TGO is an oxidation reaction product of the bond layer, and plays a role in the metal/ oxide adhesion. Each of these elements is dynamic and all interact to control the performance and durability (Mumm and Evans, 2001; Stver and Funke, 1999). When ZrO2 is utilized for technical applications, the hightemperature polymorphs cubic (c) and tetragonal (t) phases should be stabilized at room temperature by the formation of solid solutions, which prevent deleterious tetragonalto-monoclinic (m) phase transformation. The alloying oxides, which lead to the stabilization, are alkaline-earth, rare-earth, and actinide oxides. It has been suggested that the factors that may influence the stabilization are size, valency, and concentration of solute cations and crystal structure of the solute oxides, where the valency and concentration determine the number of oxygen vacancies created by the formation of substitutional solid solutions (Kim, 1990; Lehmann et al. 2003). Dense zirconia-based materials already exhibit low thermal conductivity. The introduction of a stabilizer,
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required to avoid the detrimental effect of tetragonal to monoclinic phase transformation, is accompanied by the incorporation of a substantial amount of vacancies providing an efficient source of phonons scattering (Schulz et al. 2000). When a trivalent oxide, e.g., Y2O3, is added to ZrO2 as a stabilizer, a certain amount of lattice defects, e.g., oxygen vacancies and negatively charged solutes, are produced in the ZrO2 lattice (Kim, Tien, 1991). The addition of Ta2O5, Nb2O5 and HfO2 to bulk Y2O3 stabilized tetragonal ZrO2 increases transformation, as for example the tetragonal (t) to monoclinic (m) transformation temperature, of the resulting zirconia ceramics. The enhanced transformability is related to the alloying effect on the tetragonality (c/a cell parameters ratio) of stabilized tetragonal ZrO2 (Fig.1), subsequently, by adding these oxides the tetragonal distortion of the cubic lattice is increased. The increase in the tetragonality, due to alloying, is consistent with the increase in the fracture hardness and the increase in the t to m transformation temperature (Guo and Wang, 1998; Raghavan et al., 2001; Guo et al., 2001; Raghavan et al., 1998; Kim, 1990). Evidently, t-ZrO2 become unstable as their tetragonality increases toward 1.020, which corresponds to the c/b axial ratio of m-ZrO2 at room temperature. On the other hand, they become stable as the tetragonality decreases toward unity, which corresponds to c-ZrO2. This relationship allows the classification of oxides into either a stabilizer (decreasing tetragonality) or a destabilizer (increasing tetragonality) for the t-ZrO2 phase (Kim, 1990; Kim and Tien, 1991; Lee et al., 1998).

oxides, pentavalent oxides are positively charged when dissolved in the ZrO2 lattice, the addition of these oxides in the partially stabilized zirconia (PSZ) will definitely affect the original defect structure, as well as its properties (Guo and Wang, 1998). The effect of doping with pentavalent oxides such as tantala and niobia (cationic radii in the +5 oxidation state ~0.68 for both) indicate that both ions reside as substitution defects in the zirconium lattice (ionic radius of the Zr4+ ion is 0.79 ), annihilating oxygen vacancies generated by yttria doping. Thus, the defects generated by the two dopants are also identical and would be expected to scatter phonons, i.e. can reduce the thermal conductivity, due to the difference in ionic radius and atomic bonding (Raghavan et al., 2001). Thermal conductivity is one of the physical key properties of the TBCs and increasing its insulation capability emerges as a technical and economical challenge for engine manufacturers. Lowering TBCs thermal conductivity would increase the engine performance by improving the combustion efficiency (higher turbine entry temperature), reduce the specific fuel consumption, allow the reduction of internal cooling, reduce the metallic component temperature and extend their lifetime (Hass, 2001; Kim, 1990; Kim and Tien, 1991; Raghavan et al., 1998; Lee et al., 1998). The thermal conductivity, k, of ceramic coatings can be measured using either a direct (steady state) or a transient approach. In the latter, the thermal diffusivity, a, of a material is measured and subsequently related to thermal conductivity using the relationship, as shown in Eq. (1): k = acp (1)

Where cp is the heat capacity at constant pressure and is the specific mass of the material. There are several classical techniques to measure the thermal properties of a material. Such classical methods, which involved the fitting of steady state and nonsteady state experimental temperature data to theoretical models, were usually time expendable. Furthermore, the large sized samples imposed intolerable limitations, usually tied to heat losses and contact resistance between the specimen and its associated heat source, heat sinks and measurement devices. The flash method, used in the present work, eliminated the problem of contact resistance and minimized heat losses by establishing the measuring time to be sufficiently brief so that very little cooling could take place (Couto et al., 2003; Degiovaninni and Lament, 1986).

Figure 1: Influence of the alloying oxide in the c/a axial ratio of bulk zirconia-based ceramics.

The thermal conductivity of partially stabilized ZrO2 (PSZ) is determined by its defect structure and the association between defects. Contrary to trivalent

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The study of the considered ceramic coating is motivated by the potential of the niobia to overcome the deficiencies presented in conventional yttria stabilized zirconia coatings, i.e. high thermal conductivity when compared with plasma spray coatings and relatively low mechanical properties. EXPERIMENTAL SAE 304 stainless steel plates were used as metallic substrates. Both bond layer and ceramic top coating were EB-PVD deposited using one source 30kW electron beam equipment. This consists of an electron gun with accelerating voltage of 25 kV and beam current variation from 0 to 1.2 A. The vacuum system has an ultimate pressure of 10-6 torr (~10-4 Pa). A substrate holder assembly is situated above the vapor source at a vertical distance of 150 mm. A tungsten filament is used to heat the substrate by Joule effect to the desired temperature (~500oC) during bond coating deposition and ~900oC during ceramic layer deposition), which is measured and maintained by a thermocouple and programmable temperature controller. A water-cooled copper crucible is used for evaporation of sintered targets. The ceramic targets (cylinders of 20 mm diameter and mass of 20 g) were prepared from cold compacted powder mixtures of zirconia, yttria and niobia sintered at 1700oC under vacuum (10-4 Pa). The MCrAlY targets were prepared from a Ni31Cr11Al0.65Y (wt %) powder alloy sintered at 1340oC under vacuum (10-4 Pa). The bond layer has a 25 m thickness. The crystalline phases of ceramic coatings, with an average thickness of 50 m, are identified by X-ray diffraction using a XPert Philips PW 1380/80 diffractometer and a XPert MRD Philips diffractometer with a PW 3050 goniometer. The ceramic coating microstructure and grain morphology were observed by SEM and the chemical composition was estimated by EDS using a LEO 435 VPI scanning electron microscope. The specific mass (), disregarding pores and other defects, was calculated from the cell parameters (from XRD data) and molar concentrations of zirconia, yttria and niobia (from EDS analysis), using the Eq. (2): (2) Where: n: cations in unit cell (n=4 for fcc); AYO1.5: yttria atomic mass (112.905); ANbO2.5: niobia atomic mass (132.905); AZrO2: zirconia atomic mass (123.22); x and y: molar

fraction of yttria and niobia, respectively; a and c: cell parameters of t-ZrO2 calculated from XRD data. For thermal properties determinations of coatings, the Thermal Flash 2000/Holometrix equipment was used. This method, laser technique, consists of heating the front surface of a thermally insulated specimen with a high-intensity short-duration radioactive heat pulse and measuring the temperature evolution on the back surface by means of an infrared detector. The nonintrusive backside measurement method eliminates the concern and issues with sensor attachment to the sample, and removes all uncertainties associated with contact resistance and sensor measurement accuracy (Couto et al., 2003). After stabilizing the sample at a desired uniform temperature (T0), a nearly instantaneous pulse of energy (usually laser, Xenon lamp or other discharge source) is imposed on its front surface, as well as on the temperature increase on the rear surface of the sample and is then recorded as a function of time. The thermal diffusivity is then determined by comparing this thermogram with theoretical models that describe this transient heat conduction phenomenon. Several theoretical models are available for the flash method, which includes adiabatic boundary conditions, heat losses, surface coating effects, among many other aspects. The values of thermal diffusivity (average of three measurements, for each sample at each temperature) were calculated in accordance with the Degiovaninni model (Degiovaninni and Lament, 1986). Considering that the energy of the laser is used only for heating the sample, disregarding the interfaces (contact resistance) and using Eq. (3) it is possible to calculate the coating thermal conductivity from Holometrix equipment measurements. (3) Where c is the heat capacity (J/kgK), r is the specific mass (g/cm3), a is the thermal diffusivity (cm2/s), k is the thermal conductivity (W/mK), e is the thickness (m) and the index a, m and c is relative to the sample, metallic substrate and ceramic layer, respectively. RESULTS AND DISCUSSION Typical microstructure of EBPVD coating, as seen by scanning electron microscopy on fractured cross-section, is shown in Fig. 2. It is possible to see the ceramic layers where the columnar structure is evident. Measurements on ceramic coatings fractured cross-section show almost the same size of columns diameter for samples 1 and 6,

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without significant differences in the columns morphology. However, for the sample 11, where the amount of niobia is higher, the columns diameter was increased.

in the coating primary growth direction (Bernier et al., 2003). However, the X-ray diffraction technique allows determining, with sufficient precision, the position of the peaks. The position of the peaks is correlated with crystalline cell lattice parameters and they vary strongly with the chemical composition of the films. The chemical composition, the cell parameters deduced from diffraction patterns and the values of specific mass of the coatings are reproduced in Table 1.
Table 1: Chemical composition and lattice parameters of the samples

Cell parameters mol%* mol%* YO1.5 NbO2.5 a c c/a 1 8.00 0 5.1070 5.1650 1.0114 6.04 2 8.13 0 5.1040 5.1620 1.0114 6.05 3 6.84 0 5.0950 5.1490 1.0106 6.09 4 4.78 0 5.1170 5.1970 1.0156 6.00 5 5.13 5.10 6 6.12 7.52 5.1000 5.2320 1.0259 6.02 7 10.67 8.79 5.0840 5.2150 1.0258 6.06 8 10.37 10.85 5.1240 5.2030 1.0154 6.00 9 13.79 12.87 5.0960 5.1780 1.0161 6.10 10 8.53 20.02 5.1050 5.3190 1.0419 5.99 11 10.40 14.50 5.1240 5.2770 1.0299 5.93 12 8.7 0 5.096 5.165 1.0135 6.06 13 8.7 5.6 5.100 5.212 1.0220 6.02 *From EDS analysis on ceramic coating cross-section. Sample Figure 3 shows the influence of the difference (NbO2.5 YO1.5) mol% on the zirconia tetragonality. The tetragonality was calculated from the (111) and the (400) peaks position of the XRD diffractograms on the surface

C
Figure 2: SEM of EBPVD ceramic coatings fractured crosssection. (A) Sample 1 (column diameter=1.15 m), (B) Sample 6 (column diameter=1.29 m), (C) Sample 11 (column diameter=2.53 m).

X-ray diffractions with high angular resolution (0,0001o for 2q) performed on the ceramic coating samples surface with different niobia contents show only the zirconia tetragonal phase. XRD techniques do not allow the identification of special textures related to XRD peak intensity because the PVD coatings show a strong crystallographic texture and the diffraction patterns are taken normal to the substrate surface, not
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Figure 3: Relation between difference (NbO2.5 -YO1.5) mol% and tetragonality (c/a).

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of the zirconia-based coatings. Chemical composition was determined by EDS analysis on the ceramic coating cross-section. As the difference (NbO2.5YO1.5) mol% increases, the ratio c/a (tetragonality) increases. Despite the compositional gradients in the coatings and inaccuracy of oxide semiquantitative analyses by EDS techniques, the linear regression shows a high linear coefficient (R=0.920). Research with sintered tablets (bulk material) of stabilized tetragonal ZrO2 shows that they become unstable as their tetragonality increases toward 1.020, at room temperature (Hass, 2001; Kim and Tien, 1991). This research agrees with the present works experimental results, in which niobiayttriazirconia coatings with NbO2.5 contenting higher than 7 mol% (c/a >1.020) had a tendency to spall after the deposition cycle. It is possible to evaluate the maximum content of niobia that can be added to the yttria-doped zirconia coating without losses in its mechanical properties. Thus, through the graph of Fig. 3, a coating with 8.7 mol% YO1.5 (8 wt.% yttria) can be co-doped with up to 10 mol% NbO2.5 (10.8 wt.% niobia). Figure 4 shows the typical microstructure of EBPVD ceramic coating, as seen by SEM on polished crosssection. The ceramic layer shows that color bands associated with chemical composition changes due to the differences in saturation vapor pressure of the individual components as function of the temperature and complex chemical interactions between them. For these reasons, the evaporation of alloys is a selective process, resulting in depletion and enrichment in the melt pool and, consequently, in the coating.

Figure 5: EDS semi-quantitative analysis of ceramic layer (sample 11).

remarkably for the niobia concentration, due to the difference in melting point and vapor pressure between niobia, zirconia and yttria. It is clear that compositional gradients can reduce the thermal stability due to differences in layers thermal expansion coefficients. Nevertheless, because of the high melting point of the ceramic, the liquid pool during evaporation is shallow in comparison with target volume, there is not sufficient liquid volume for high level of segregation and as the process is predominantly random, the influence on the thermal stability and in the X-ray data is not high. Another factor that reduces the influence of the multilayer nature of the coatings with differences in composition between the layers in the XRD data is the X-ray penetration (attenuation length) (Henke et al., 1993). ZrO2 has an attenuation length of 17 mm (phonon energy of 8050 eV and incident angle of 90o), thus the XRD data is based on integration or average of a significant thickness of the coatings. Two ceramic formulation coating samples (sample 12 and 13, Table 1) were used for determination of the coatings thermal conductivity. The measurements of thermal diffusivity samples are carried out on coatings with their substrates and bond coats attached to them. All samples were coated with colloidal graphite to optimize the laser energy absorption (black body) and to make the infrared sensor data acquisition uniform in the sample backside during thermal diffusivity measurements. On account of its high thermal conductivity value in comparison with zirconia (kgraphite = 24 W/m K, kzirconia = 1 W/m K, at 25 oC), the graphite layer (thickness of ~30mm) was not considered in the calculations. Figure 6 presents the coatings thermal conductivity variation with the temperature as calculate by using

Figure 4: SEM (BS mode) of an EB-PVD ceramic coating polished cross-section (sample 3).

The results of EDS analysis performed on the ceramic coating cross-section are summarized in Fig. 5. The composition of the ceramic layer differs point-to-point,

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with pentavalent metallic ions, showing that significant decrease in thermal conductivity (up to 40%) can be achieved, when compared to the standard 8 wt.% yttria partially stabilized zirconia. The reduction of almost 50% in the thermal conductivity coating promoted by niobia addition can be attributed to several factors: the increase in the level of porosity of the yttria niobia co-doped zirconia coating; the phonons scattering promoted by the ionic radii differences and chemical bonds between matrix (zirconia) and dopants (niobia and yttria) and, in lower degree, to the small reduction of the specific mass coating promoted by the niobia addition.
Figure 6: Variations of coatings thermal conductivity with temperature.

CONCLUSIONS The niobia addition, up to 6 wt.%, as co-dopant in the yttria partially stabilized zirconia coatings is insufficient to change its microstructure. The laser flash technique in conjunction with Degiovaninni model demonstrates efficiency to determine thermal conductivity of the TBC attached to the substrates. The single-phase tetragonal niobia and yttria co-doped zirconia coatings show a lower thermal conductivity than conventional 6-8 mol% yttria stabilized zirconia coating, the material conventionally used for thermal barrier coating. ACKNOWLEDGMENT The authors express their gratitude to FAPESP (process number: 02/06514-1) and CNPq (process number: 490845/2006-1) for the financial support. REFERENCES Almeida, D. S. et al., 2006, EB-PVD TBCs of Zirconia Co-doped with Yttria and Niobia, a Microstructural Investigation, Surface and Coatings Technology, Vol. 200, pp. 2827-2833. Almeida, D. S. et al., 2007, Thermal conductivity investigation of zirconia co-doped with yttria and niobia EBPVD TBCs, Materials Science and Engineering: A, Vol. 443, pp. 60-65. Bernier, J. S., et al., 2003, Crystallographic texture of EB-PVD TBCs deposited on stationary flat surfaces in a

Eq. (3). The zirconia heat capacity values were taken from literature (Raghavan et al., 1998), an approach which is possible due to the little influence of the oxides dopants in these physical properties of zirconia. Thermal conductivity of standard 68 wt.% yttria partially stabilized zirconia EB-PVD coatings is typically 1.51.9 W/m K. The thermal conductivity of a ceramic layer depends on the intrinsic thermal conductivity of the bulk ceramic, which is linked to its composition and structure, and to the framework of the porous structure, i.e. pore volume fraction, geometry and distribution (Schulz et al., 2000; Schulz et al., 2003). The present work shows an yttria-doped zirconia coating, with mean thermal conductivity value of 1.17 W/m K significantly lower than those indicated by literature for EB-PVD coatings (1.51.9 W/m K). This reduction can be explained by the coating thickness. The thermal conductivity of EB-PVD PYSZ coatings strongly depends on the coating thickness with lower values for thin TBCs, this effect is caused by the different microstructure across the coating roughly characterized by a fine grained inner zone and a coarse grained outer zone (Rtzer-Scheibe et al., 2006). A 50% reduction in the yttria niobia co-doped zirconia coating thermal conductivity (average value: 0.54 W/m K) was observed when compared with yttria-doped zirconia coating. Schulz et al. developed a model based on solid state physics considerations regarding heat conduction mechanisms in disordered oxide ceramics for the calculation of the thermal conductivity of zirconia based materials doped with trivalent ions and co-doped

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Thermal barrier coating by electron beam-physical vapor deposition of zirconia co-doped with yttria and niobia

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Xu, H.; Goug, S., Deng, L., 1998, Preparation of thermal barrier coating for gas turbine blades by EB-PVD, Thin Solid Films, Vol. 334, pp. 98-102. Zhu, D. et al., 2000, Thermal conductivity of EB-PVD thermal barrier coatings evaluated by a steadystate laser heat flux technique, Ohio: NASA, 18 p. (NASA/TM2000-210238).

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doi:10.5028/jatm.2010.02026610

Jos A. Orlowski de Garcia*


Instituto de Aeronutica e Espao So Jos dos Campos Brazil orlowski@iae.cta.br

Nilton Souza Dias (in memoriam)


Instituto Nacional de Pesquisas Espaciais So Jos dos Campos Brazil

Advances of orbital gas tungsten arc welding for Brazilian space applications experimental setup
Abstract: The present work describes details of the several steps of the technology involved for the orbital Gas Tungsten Arc Welding (GTAW) process of pure commercially titanium tubes. These pieces will be used to connect the several components of the propulsion system of the ChinaBrazilian Satellite CBERS, and is part of the Brazilian aerospace industry development. The implantation involved the steps of environment control; cut and facing of the base metal; cleaning procedures; piece alignment; choice of the type, geometry and installation of the tungsten electrode; system for the pressure of the purge gas; manual tack welding; choice of the welding parameters; and, finally, the qualification of welding procedures. Three distinct welding programs were studied, using pulsed current with increasing speed, continuous current and pulsed current with decreasing amperage levels. The results showed that the high quality criteria required to the aerospace segment is such that usual welding operations must be carefully designed and executed. The three welding developed programs generated welds free of defects and with adequate morphology, allowing to select the condition that better fits the Brazilian aerospace segment, and to be implanted in the welding of the CBERS Satellite Propulsion System. Keywords: Orbital GTA welding, Titanium, Satellite.

Instituto Nacional de Pesquisas Espaciais So Jos dos Campos Brazil gerson.lima@lit.inpe.br

Grson Luiz de Lima

Wilson D. Bocallo Pereira

Instituto de Aeronutica e Espao So Jos dos Campos Brazil pistolinha@iae.cta.br

Instituto Nacional de Pesquisas Espaciais So Jos dos Campos Brazil nivio@tge.inpe.br * author for correspondence

Nvio Fernandes Nogueira

INTRODUCTION During the 1980s, the National Institute of Space Research (INPE, acronym in Portuguese) began developing priority programs such as CBERS (ChinaBrazil Earth Resources Satellite), which is a cooperative effort between the Brazilian and the Chinese governments. One of the features of CBERS is its stabilization on three axes. This occurs because of a positioning control know as the propulsion system. This is constituted of four fuel storage tanks (hydrazine), sixteen 1 N micro thrusters and two of 20 N, valves and filters, amongst others, as well as distribution lines made out of commercially pure titanium grade 2 to interconnect the various components. Maintaining the positioning of the satellite during orbit depends basically on this system. An eventual fuel leakage from its welds would compromise the entire mission. For this reason, the quality criteria regarding the welding of its components are extremely rigorous and follow the Chinese manufacturing standards for the aerospace sector. With the objective of integrating and testing CBERS, INPE/LIT invested approximately US$ 220,000 to implant a welding laboratory furnished with equipment for controlling environmental conditions, cleaning and welding of components to be used in the aforementioned satellite by means of the Orbital GTAW process.
Received: 06/05/10 Accepted: 07/06/10

For illustration purposes, Fig. 1 to 4 are representative of the integration of the CBERS Satellite, carried out in the facilities of INPE/LIT by the authors of this study. It is important to point out that these operations were carried out immediately after the stages of experimental setup, qualification and characterization of the welded joints. The success of the project (a rejection indices of only 0,7%) is attributed to the manufacturing procedures developed for handling, cutting, facing, pickling, tacking, welding, internal purging and the use of standardized electrodes and samples during welding operation. Simultaneously, the use of gases with special characteristics associated with filters, rigorous environment control and leak tests were decisive in increasing the quality of the final product. Considerations regarding titanium and its alloys Titanium is used in its commercially pure grades or in combination with other elements known as alloys. It possesses unique characteristics, which are responsible for stimulating the extensive interest of a wide range of industrial segments, in particular, the aerospace industry that first used titanium components in airplanes and afterwards in spacecraft. Commercially pure titanium is used in situations of elevated resistance to corrosion associated with forming. Although the 300 series stainless steel has similar characteristics and is significantly cheaper,
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Figure 1: Measuring the internal pressure.

Figure 3: GTAW operation.

Figure 2: Manual tack welding operation.


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Figure 4: GTAW operation.


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its use in the aerospace industry is limited because of its greater density. Boyer (1996) shows there is around a 50% reduction in structural weight when titanium and its alloys are used as opposed to conventional alloys. Another interesting metallurgic characteristic of titanium and its alloys is the corrosion resistance levels of the base metal on the welded joints. The oxide responsible for the high index of this parameter forms equally on welds as it does on the base metal and results in analogous performance independently of the environment to which they are exposed (Smith, Threadgill and Gittos, 2009). The commercially pure titanium (CPTi) is 99 to 99.5%Ti, and also contains iron and some interstitial elements classified as impurities, such as hydrogen, nitrogen, carbon, and the most important of all, oxygen, with which it has great chemical affinity. The CPTi is available in several grades depending on their chemical composition. Though present in small quantities, these elements exert a strong influence on the mechanical properties of titanium; oxygen and nitrogen exert a great extent, while iron and carbon have a lesser impact (AWS, 1984; Boyer, Welsh and Collings, 1998; Lathabai, Jarvis and Barton, 2001). The CPTi alloys (grades 1 to 4) display good weldability as they have low coefficients of thermal conductivity and linear thermal expansion, which facilitate the welding operation. They are used in applications in which mechanical resistance is not the highest requirement, unlike resistance to corrosion associated with high ductility (AWS, 1984; Boyer, Welsh and Collings, 1998). In the CBERS Satellite specifically, the use of titanium is restricted to the propulsion system, in other words, the ultra high purity lines of the hydrazine circuit. Basically, the setup consists of several components interconnected by small diameter tubes. Its joints are connected using the Orbital GTAW process due to the extreme demands regarding the quality of the final product. Considerations regarding Orbital GTA welding Orbital welding systems are made up of a programmable power supply, an orbital weld head, electric cables, gas hoses and optional accessories. The power supply is a portable, fully programmable piece of equipment whose welding sequence is controlled by means of a microprocessor. This allows one to adjust different levels for the welding variations according to the diameter, thickness and material to be welded. Precision in relation to the welding parameters is in the order of 1%. The welding machine allows one to program the parameters such as the welding speed and the amperage, either continuous or pulsed (Morgan and

Henon, 1999; Henon, n.d.). Power supplies up to 150 A only use continuous current. Such situations are designed for autogenous welding where filler metal is not used. In general, it is applied when joining small outside diameter tubes (3.2 mm a 177.8 mm) and limited to a maximum thickness of 3.9 mm. The welding is carried out in one step on square butt joints, whose typical configuration can be seen in Fig. 5 (Morgan and Henon, 1999; Brond and Henon, 1996).

Figure 5: Joint configuration.

MATERIALS AND METHODS The initial phase of the work consisted of creating a welding laboratory capable of meeting the manufacturing requirements of the very high purity propulsion system of the CBERS Satellite. In this type of setup, the use of a clean room with precise humidity, temperature and particulate control is absolutely necessary. The specified values for the above mentioned parameters are achieved by installing appropriate filters and curtains to purify the air in the working environment. Next, there was the purchasing of equipment to provide continuity for the manufacturing stages. Firstly, the equipment for the final cleaning of the components, the particulate counter, equipment for facing the tubes and finally the Orbital GTAW power supply for joining the propulsion system components. The base metal used was imported commercially pure titanium grade 2 in the form of seamless tubes, fittings (union cross, tees and spherical connections) and components (filters, valves, transducers etc.) with a diameter and wall thickness equal to 6.0 0.1 mm and 1.0 0.05 mm, respectively. The consumables used were an EWCe-2 electrode (2% cerium tungsten) with a diameter of 1.6 mm and a tip geometry with an angle of 30 and high purity argon gas (99.999%) for shielding and purging.
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The success of the orbital technology applied to the aerospace sector is as much a function of the programming of the primary welding parameters, as it is of a series of defining conditions, which together add consistency and quality to the results (Serafin, n.d.; Orlowski, n.d.). In this manner, because of the great number of variables involved in the preparation stages of the base metal and the welding itself, the following sequence of events, described below and presented in the results and discussion sections, was established: environment control; base metal preparation (selecting, cutting and facing); cleaning procedure; alignment; tungsten electrode type, geometry, dimensions and installation; purging gas pressure control; manual tacking; surveying of the welding parameters; and welding qualification procedure. Three welding programs using constant and clockwise rotation were separately developed to join the commercially pure titanium tubes, as follows: pulsed current with increasing speed (#A), continuous current (#B) and pulsed current with decreasing amperage levels (#C). Additional data referring to the operational process and to the used material were obtained by consulting specific standards (AWS, 2000; AMS, 1991). After the welding cycles, the welds were visually inspected (outside and inside) to see if the weld adhered to the criteria established by the Chinese Standards (CAST, n.d.). Three weld beads were selected, each one of which corresponded to one of the programs, in other words, constant (#B), pulsed current with increasing speed (#A) and, finally, pulsed current with decreasing amperage levels (#C). Once the welding parameters were determined, nine test specimens were welded for each one of the welding programs being studied, and were submitted to visual inspection, radiography and leak tests. The welded joints were cut and the width of the face and root of the weld beads were measured. The evaluation of the welded joints regarding mechanical tests and metallurgic characteristics will be the subject of a future publication. RESULTS AND DISCUSSION This part of the work presents the deployment of titanium welding technology in the Brazilian aerospace industry, including the preparatory steps involved in setting up the laboratories, preparing the welding, determining the procedures for welding and inspection of the welded joints. Control of environmental conditions The manufacturing cycle of ultra-high-purity systems of which welding is a fundamental part, requires precise control, not only of its stages, but also of the environment in which
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it is manufactured. In this sense, the Welding Laboratory at INPE/LIT is specifically equipped for this purpose, capable of maintaining humidity between the ranges of 40 to 50%, temperature between 18 and 22C and particulate control of 10,000, as required by the Chinese Specifications. Preparation of base metal (selecting, cutting and facing) Due to the rigorous standards applied to weld bead quality, the presence of gap between components to be welded is a reason for rejection in accordance with aerospace procedures. Equally, deformities, out-of-roundness and variations of thickness along the joints are responsible for causing inconsistencies (Mannion and Heinzman, 1999a; Mannion and Heinzman, 1999c;). Based on such information, strict control is necessary, related to material specification such as dimensional tolerances, as well as the preparation of the joints and the obligatory facing of appropriate equipment. The tubes were cut into appropriate lengths, which was followed by the facing of both extremities with respect to perpendicularity requirements (< 0.02 mm), section roundness (< 0.05 mm), absences of deburring and beveling of the edges. Argon gas was then injected into the tubes to remove residues left over from the above operations. When facing was completed, the edges were deburred and configured for welding. Cleaning procedures Firstly, chemical pickling is carried out to remove the oxide layer. Initial tests establish the average time for immersing the test specimens in successive acid solutions baths (70% nitric acid, 50% hydrofluoric acid and water with distinct fractions of 15, 3 and 82 parts per volume, respectively). Next, the test specimens were transferred to an oven for drying, where they remained for 2 hours at a temperature of 50 to 60C. Following this, the parts were placed in plastic bags filled with argon (99.999%) so as to eliminate any possible form of contamination. Final cleaning (or internal cleaning) consists of circulating isopropyl alcohol through the insides of the tubes while connected to a machine of 99.995% pure gaseous nitrogen and at a pressure of 1.50.5 bar. The machine contains vacuum filters at several points of the cleaning system, which allows samples of liquid to be collected on membrane filters throughout the process and analyzed under an optical microscope using particle counting techniques. The purpose of this operation is to verify the degree of cleanliness. Once the pre-established criteria have been achieved, regarding the dimension of particles, the cycle is interrupted and the drying of the components at a temperature of 605C begins. After this stage, the tubes are placed in plastic bags filled with argon

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(99.999% pure) and duly identified. Figure 6 outlines the equipment used.

recommendations (Arc Machines, Inc., 1991). The values are calculated in function of the tube to be welded and the model of the orbital weld head. Control of purging gas pressure The technique for pressurization consists of establishing a positive pressure inside the parts by supplying purging gas under a constant pressure. Its value depends on the tube diameter, the position of the joint, pressure losses and an airtight purge plug with a small diameter exit orifice to restrict the escape of gas (Henon and White, n.d.). This practice allows one to control the geometry of the weld bead and avoids the occurrence of discontinuities. The equipment used in this process consists of a Magnehelic (Dwyer Instruments, Inc., USA) pressure gauge and a small T device, both shown in Fig. 8. The determination of the correct working pressure involves the insertion of the small T device into the joint to be welded. Two of its extremities are connected to the network, while the third is fixed to the Magnehelic gauge.

Figure 6: Final cleaning equipment. (1) cleaning and drying compartment; (2) samples collecting circuit for analysis; (3) equipment controls; (4) cleaning circuit.

Alignment For orbital systems, the precision of alignment between the parts to be welded is of considerable importance, regarding the quality of the weld beads. Should there be any internal projections as a result of improper settings; these can interfere in the flow of fluids (hydrazine) or, in extreme cases, require reworking (Mannion and Heinzman, 1999b; Mannion and Heinzman, 1999c). For this purpose, a stainless steel alignment gauge was developed to overcome this short-coming. The model consists of two parts, each of which has a groove on its inner part so as to line up the tubes, as seen in Fig. 7. The four external screws help in securing the tubes while the central ones guarantee the correct positioning. The side openings of 180 facilitate the welders view of the joint and consequently the manual tacking operation.

Figure 7: Alignment gauge.

Figure 8: Magnehelic gauge.

Tungsten electrode - type, geometry, dimensions and installation The choice of material, its geometry and the electrode dimensions should follow the manufacturers

After reading the pressure, the device is removed from the system and substituted by the orbital weld head, and the welding is accomplished. The pressure is the result of the internal tube diameter (ID) purge gas flow rate and the size of the restriction orifice purge plug used at the end. The
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difference in pressure is adjusted by increasing or decreasing the flow rate. The working pressure should be sufficient so as to produce weld beads with the same profile as the tube walls. Manual tacking This is necessary for maintaining the parts in position. This operation is executed manually using a GTAW torch without filler metal. The dimension of the tacks must be minimum, however sufficiently resistant to keep the joint aligned. The use of purging gas is recommended when tacking, because as well as preventing oxidation of the inner tube, it helps in cooling. The welding parameters are set out in Table 1.
Table 1: Manual tack welding operation

Table 2:

Welding parameters for three programs

Survey of welding parameters The welding parameters for the three programs (#A), (#B) and (#C) are presented in Table 2. It can be observed that, for each of the programs, the nine test specimens produced flat, smooth welds which are of homogeneous width around their perimeters and are devoid of oxidation or other defects on the outside and inside diameters. Figure 9 shows the welding of the test specimens together with the respective equipment, power supply, orbital head and pressure gauge. Programs #A and #C displayed similar characteristics, considering the employment of pulsating current associated with the reduction in the heat input due to an increase in welding speed (#A) and the reduction in amperage (#C) throughout the respective welding cycles. Both procedures are widely used in joining small diameter tubes, so as to minimize the accumulative effects of the energy from welding, particularly in the final phase of the welding cycle (Kou and Le, 1984). In this manner, the presence of concave welds or even perforations defects generally associated with excesses of energy can be restricted or avoided. Despite the fact that specialized literature (Kou and Le, 1984; Henon, n.d.) recommends the use of the above mentioned techniques for welding of small diameter tubes, program
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Figure 9: Orbital GTAW operation of the test specimen.

#B used the same heat input for welding the test specimens. The success of the results, like the other programs, can be attributed to the use of the technique of internal pressurization with purging gas. This is responsible for controlling the morphology of the fusion zone, for protecting the molten area and the other heated regions of the tube as well as cooling the part/set (Henon, n.d.). Table 3 shows the heat input values employed for each of the programs being studied. This parameter can be defined as being the quantity of energy supplied by the arc to the joint. It was calculated by the expression HI = f (E.I/v), where HI = heat input, E = volts, I = amperes, v = millimeters per second and f is the efficiency of the heat transfer equal to 0.9 for the GTAW process. The voltage readings were obtained by the use of a multimeter whose positive and negative terminals were connected to the tube and orbital weld head rotor, respectively. The average value corresponding to a total of five readings carried out during each of the welding programs was 8.37 V. In such a way, it was

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Advances of orbital gas tungsten arc welding for Brazilian space applications experimental setup

Table 3:

Heat Input for three welding programs

Table 4:

Dimensions of the fusion zones

possible to obtain the welding energy values for each level (quadrants) of the programs under test. Increasing values can be observed in the sequence #B, #C and #A. Although programs #A and #C employed pulsating current in their respective cycles, the higher welding energy values can be justified by the low speeds (#A) and high amperages (#C). Visual and X-ray inspection Figure 10 shows the typical weld bead from the programs being studied, where it is possible to see the aspect of the face and root. Its principal characteristics are uniformity in width, alignment, total penetration, smooth finishing and no oxidation in the heated regions. All nine weld sets for each of the welding programs are aligned without mismatching. The examination of the internal diameter of the welded joints using a boroscope indicated conformity with the Chinese Quality Standards (CAST, n.d.). X-ray inspection revealed no defects on the welded samples, which were then considered approved.

following order: program #B, #C and #A, respectively. The increased width of the face and root can be attributed to higher welding energy contribution, as can be seen in Table 3. The maximum width should be inferior to 6.0 mm (CAST, n.d.), which was obtained for all welding programs. Leak test According to project data, the minimum prescribed levels for welded joints are 1.0 x 10-7 Pa m3/s. All welded joints achieved this value without presenting signs of leakage and as such were considered approved. CONCLUSIONS The following conclusions could be obtained from this study, whose objective was to develop titanium welding techniques using the Orbital GTAW process to join components of the CBERS Satellite Propulsion System: - it could be concluded that the above welding operations involving control of environmental conditions, cutting and facing of the base metal, cleaning procedures, alignment and type, geometry, dimensions and installation of the tungsten electrode were shown to be effective, as well as being necessary for the success of the welding; - the technique developed using internal pressurization with purging gas proved to be effective, given the results of the internal morphology of the weld bead and the absence of any defects; - the device used for manual tacking was effective and guaranteed the strict alignment standards required for welded joints; - the three welding programs developed produced satisfactory results regarding the non-destructive tests carried out, as did the geometrical characteristics of the weld
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Figure 10: Weld test coupons.

Table 4 displays the dimensions of the fusion zones of the welding programs under test, a total of five readings per welding program. Increasing average values were recorded for the width of the face and root of the weld beads in the

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bead. One of these will be chosen for welding components of CBERS Satellite Propulsion System after a mechanical and metallurgic examination of the welded joints. REFERENCES Aerospace Material Specification (AMS), 1991, AMS 2689A, Fusion welding titanium and titanium alloys. American Welding Society (AWS), 2000, AWS D10.6/ D10.6M: 2000. Recommended practices for gas tungsten arc welding of titanium piping and tubing, Miami, FL, American Welding Society. American Welding Society (AWS), 1984, Metals and their weldability, 7. ed., Vol. 4, Miami: W.H. Kearns. Arc Machines, Inc., 1991, Model 207A power supply operator training guidelines, 2nd. ed, Pacoima.. Boyer, R.R., 1996, An overview on the use of titanium in the aerospace industry, Materials Science and Engineering A, Vol. 213, No 1-2, pp. 103-114. doi:10.1016/0921-5093(96)10233-1. Boyer R., Welsh G., Collings, E.W., 1998, Materials properties handbook: titanium alloys. 2nd. ed., ASM International, Ohio, USA. Brond, A., Henon, B.K., 1996, Orbital pipe welding technology for the power generation and offshore industries, Proceeding of 22th National Meeting on Welding Technology, 10th Latin American Welding Congress, Blumenau, Brazil. Chinese Academy of Space Technology (CAST), n.d., Chinese Standard CBERS propulsion subsystem pipe integrating and welding requirement (specification). Chinese Academy of Space Technology (CAST), n.d., Chinese Standard CBERS propulsion subsystem pipe leakage check requirement (specification). Henon, B.K., n.d., High technology orbital tube and pipe welding equipment used on pharmaceutical high purity piping installation, Available at: <http://209.35.63.149/ appPages/bmw02.html>. Access on Oct 24, 2001. Henon, B.K., n.d., Orbital welding of small diameter tubing, Available at: <http://www.arcmachines.com/ appPages/smalldia02.html>. Access on Oct 24, 2001. Henon, B.K., n.d., Practical application of orbital tube and pipe welding, Available at: <http://www.arcmachines. com/appPages/pract02.html>. Access on Nov 17, 2001.
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Henon, B.K., White, J., n.d., Use of ID pressurization to control weld profile in semiconductor ultra-highpurity process gas lines, Available at: <http://www. arcmachines.com/appPages/dsi02.html>. Access on Oct 24, 2001. Kou, S., Le, Y., 1984, Heat flow during the autogenous GTA welding of pipes. Metallurgical Transactions A, Vol. 15, No 6, pp. 1165-1171. doi: 10.1007/BF02644711. Lathabai, S., Jarvis, B.L., Barton, K.J., 2001, Comparison of keyhole and conventional gas tungsten arc welds in commercially pure titanium, Materials Science and Engineering A, Vol. 299, No 1-2, pp. 81-93. doi: 10.1016/ S0921-5093(00)01408-8. Mannion, B., Heinzman, J., 1999a, Determining parameters for GTAW: starting points for success, Available at: <http://www.pro-fusiononline.com/feedback/ pwt-aug99.htm>. Access on Sept 21, 2001. Mannion, B., Heinzman, J., 1999b Orbital tube welding, Available at: <http://www.pro-fusiononline. com/feedback/articles.htm>. Access on Nov 21, 2001. Mannion, B., Heinzman, J., 1999c, Setting up and determining parameters for orbital tube welding, Available at: <http://www.pro-fusiononline.com/ feedback/fab-may99.htm>. Access on Sept 24, 2001. Morgan, J., Henon, B. K., 1999, Discovering applications for orbital fusion welding, Available at: <http://www. arcmachines.com/appPages/tpj02.html>. Access on Oct 24, 2001. Orlowski, J.A.G., n.d., The orbital welding of the CBERS (China-Brazil Earth Resources Satellite) Propulsion System, Available at: <http://www.arcmachines.com/ appPages/cbers02html>. Access on Jul 30, 2004. Purnell, S., n.d., Assessing developments in orbital weldingpart 1: taking the monotony out of tube welding, Available at: < http://www2.thefabricator.com/Articles/Tube_and_ Pipe_Article.cfm?ID=59>. Access on Mar 31, 2004. Serafin, M., n.d., Orbital welding for space program applications, Available at: <http://www.2thefabricator. com/Articles/Tube_and_Pipe_Article.cfm?ID=443>. Access on Mar 31, 2004. Smith, L.S., Threadgill, P., Gittos, M., 2009, Weldability of materials: titanium and titanium alloys, Available at: <http://www.twi.co.uk/j32k/protected/band_3/jk24. html>. Access on Jul 23, 2010.

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doi: 10.5028/jatm.2010.02026710

Jos A. Orlowski de Garcia*


Instituto de Aeronutica e Espao So Jos dos Campos Brazil orlowski@iae.cta.br

Instituto Nacional de Pesquisas Espaciais So Jos dos Campos Brazil gerson.lima@lit.inpe.br

Grson Luiz de Lima

Characterization of titanium welded joints by the orbital gas tungsten arc welding process for aerospace application
Abstract: In this work, three welding programs for orbital gas tungsten arc welding (GTAW), previously developed, were used, using pulsed current and increasing speed (#A), constant current (#B) and pulsed current and decreasing current (#C). One of these should be used for the propulsion system of the Satellite CBERS (China Brazil Earth Resources Satellite). Welded joints using tubes of commercially pure titanium were obtained with these procedures, which were characterized by means of mechanical and metallographic tests. The obtained results showed that the three welding procedures produce welded joints free of defects and with adequate shape. Although small differences on mechanical properties and on microstructure have been observed, the three welding programs attained compatible results with international standards used in the aerospace segment. The welding program #B, due to the reduced heat input used, was considered to obtain slightly advantage over the others. Keywords: Orbital GTAW, Titanium, Satellite.

Wilson D. Bocallo Pereira

Instituto de Aeronutica e Espao So Jos dos Campos Brazil pistolinha@iae.cta.br

Valdir Alves Guimares


Univers. Estadual Paulista Guaratinguet Brasil valdir@feg.unesp.br

Instituto Tecnolgico de Aeronutica So Jos dos Campos Brazil mneto@ita.br

Carlos de Moura Neto

Universidade Estadual do Norte Fluminense Rio de Janeiro Brazil paranhos@uenf.br * author for correspondence

Ronaldo Pinheiro R. Paranhos

INTRODUCTION Orbital welding was developed at the beginning of the 1960s to provide the aerospace industry with the basic conditions to manufacture highly reliable components. The existence of failures of joints in hydraulic systems joined by fittings that had been exposed to vibrations and mechanical stresses during flights at speeds close to that of the speed of sound brought about the need for a more reliable joining technology. In this way, the orbital system was developed from the already existing gas tungsten arc welding (GTAW) process (Henon, 1998; Henon, n.d.; Orbimatic, n.d.). The orbital GTAW system is used in the industrial welding of tubes and ducts of diverse sized diameters and thicknesses in situations where quality and productivity go hand in hand. The minimal heat input permits distortion control and the retaining of dimensional accuracy (Orbimatic, n.d.; Mannion, 1999; Henon, n.d.; Morgan and Henon, 1999; Brond and Henon, 2000; Littlewood and Henon, 2000).
Received: 06/05/10 Accepted: 09/06/10

The welding of small diameter tubes with reduced thickness involves square butt joint and single pass. The tubes are maintained in a fixed position, while the electrode moves along the joint, forming a homogeneous weld bead whose properties are close to those of the base metal. The operation is carried out in an inert gas environment which is responsible for shielding the extremities of the electrode, the fusion zone and the heated regions of the component against atmospheric contamination (Mannion, 1999; Morgan and Henon, 1999; Arc Machines, Inc., 2001). Figure 1 shows the principles of orbital GTAW. The success of orbital GTAW technology applied in the aerospace sector depends not only on the programming of the primary welding parameters, but also on a series of boundary/ outlying conditions (chemical composition of the material, setup requirements, type and purity of the gases, type and geometry of the electrode, amongst others) which, together, provide the consistency and quality of the welded components. This study is part of an important national effort which allows the Brazilian aerospace industry to develop part of the technology to build satellites. In the first part of the study (Orlowski et al., 2007), the development of three

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The shielding gas used was high purity argon (99.999%), with a flow of 5.2 L/min. The pressure of the purging gas which produced the best results in terms of weld bead geometry was 3.2 L/min of argon. The metallographic preparation was carried out using usual techniques. An alumina solution (200 mL), water (20 mL), potassium hydroxide (2 g) and oxalic acid (30 g) were used in the mechanical polishing. Krolls reagent containing 100 mL of distilled water, 2 mL of hydrofluoric acid and 5 mL of nitric acid was used to reveal the microstructural features. The employed technique was to immerse the samples in the solution for approximately 10 seconds. A metallographic evaluation of the welded joints was performed using an optical microscope (OM) and a scanning electron microscope (SEM). Images were captured using a data acquisition program called DT Acquire, version 2.0. The grain size of the base metal and the heat affected zone (HAZ) were measured using a computer program known as Image Tool for Windows, version 2.0, by taking the captured images during the optical microscope analysis. Vickers microhardness profiles were carried out on the base metal, the HAZ and the fusion zone with a 100 g load and penetration time of 7 seconds using a digital machine FM model (Future Tech Corporation). Three measurements were taken for each region. The indentations were made midway between the surface and the base of the transversal sections of each of the samples corresponding to the three welding programs. The hardness traverse passed through the base metal, HAZ and unaffected weld metal. Mechanical tensile tests were used to evaluate the properties of the base metal and the welded joints from the three welding programs. Nine test specimens were prepared for each type of welding and three for the base metal. The tests were developed in accordance to the AWS B4.0M:2000 Standard (AWS, 2000a). The analysis of the fractured surface of the test specimen from the uniaxial tensile test was performed by SEM. RESULTS AND DISCUSSION Three different welding programs (Orlowski et al., 2007), utilizing continuous and clockwise rotation, were developed to weld the commercially pure titanium tubes. Their characteristics were, as follows: pulsed current with increasing speed (#A); continuous current (#B); pulsed current with decreasing amperage levels (#C). The welding procedures are presented in Table 2. Further details can be obtained in the first part of this study (Orlowski et al., 2007). Table 3 shows the heat input values used in each of the programs under test. This acts on the cooling rate of the joint, microstructure and mechanical properties, amongst others. It is calculated from the formula HI = f(E.I/v), where HI is the heat input, E is the voltage, I is the intensity of the current and v, the welding speed. The value of f (heat transfer efficiency) is taken as being 0.9, valid for the GTAW process.

Figure 1: Principles of Orbital GTAW process.

different programs was carried out using orbital GTAW technology, establishing adequate welding procedures for this task. In the second part of the study, the welded joints were evaluated and characterized. MATERIALS AND METHODS The employed base metal was commercially pure titanium (grade 2), obtained from China, in the form of seamless tubes of diameter of 6.0 0.1 mm and thickness of 1.0 0.05 mm. Chemical composition is shown in Table 1 and is in agreement with the standards established by literature (ASTM B338 03; AWS, 2000b).
Table 1: Chemical composition of the base metal (% weight)

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Table 2:

Welding parameters versus welding programs

Table 3:

Heat Input values for welding programs

Increasing heat input values were observed for the sequence #B, #C and #A. Though programs #A and #C used pulsed current in their respective welding cycles, the higher welding energy levels are attributed to the low welding speeds of program #A and the elevated currents of program #C (Table 2). Microstructural characterization Figure 2 shows the base metal microstructure which consists basically of equiaxed a phase grains with the presence of fine, disperse precipitations of phase. The presence of fine disperse precipitations can be seen in the boundary regions of the grains as well as inside them. Although the analysis of these precipitates is not within the scope of this study, the research carried out by Gould, Becker and Williams (1980) reveals that elements, such

Figure 2: Micro structure of CP titanium base metal. Optical metallography. Etchant: Krolls reagent. Magnification: 500x.

as iron, present in the form of impurities in commercially pure titanium, stabilizes phase elevating by up to 5% in quantitative terms its presence in the matrix. Specifically in the case of titanium, the fusion zone is characterized by temperatures above the solidus line of the material. In the HAZ, the temperature levels reach values above that of the allotropic transformation,
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transus, during the heating phase. During cooling, the product formed as a result of phase is because of the declining temperature rate in this area. Consequently, the effects resulting from the thermal cycles, in particular heat input, are principally responsible for the final properties of the welded joint because of the microstructural transformations. For example, titanium and its alloys can have different microstructural configurations, like equiaxial grains, peculiar of annealed structures, and more complex phases, such the metastables (martensite, bainite, Widmanstttens structure, amongst others) typical of elevated cooling rates (Lathabai, Jarvis and Barton, 2001; Danielson, Wilson and Alman, 2003). A second characteristic involving the welding of titanium and its alloys is the possibility of contamination due to the high reactivity level with gases from the atmosphere, in particular oxygen. For example, insufficient shielding gas flow or time, the presence of contaminants in the gas composition or leakages along the shielding gas feed line. In these cases, elements such as oxygen (Ra = 0.60 m; Ra = atomic radius) and nitrogen (Ra = 0.71 m), located on intersticial sites in the crystal lattice of titanium (Ra = 1.46 m), prevent the movement of dislocations. This phenomenon is responsible for the increase in hardness and strength of the welded joint and, equally, for its embrittlement (Danielson, Wilson and Alman, 2003). Figure 3 is a light optical micrograph of the orbital GTAW, showing the variation in the microstructure moving from the unaffected base metal through the HAZ

to the fusion zone. Because of the similarities between the microstructures, independently of the heat input applied, the welding program #B was chosen as being representative, so as to avoid unnecessary repetitions. The base metal (Fig. 3a) corresponds to the region that retains its original structure. It has not been significantly affected by the heat of the weld, and consists of small equiaxed a phase grains, as already shown in Fig. 2. The border area between the base metal and the HAZ, represented by the right and the left of Fig. 3b, clearly defines the area from where the welding thermal cycles operate incisively on the microstructural changes. In the area corresponding to the HAZ, large equiaxial grains sizes can be observed. A more detailed observation of the HAZ (Fig. 3c) shows a significant grain coarsening size, close to the fusion zone as a result of the thermal cycles with a greater peak temperature. The degree of grain coarsening increases as one moves toward the centre of the fusion zone. Similar results have been recorded by Lathabai, Jarvis and Barton (2001) and Danielson, Wilson and Alman (2003) in studies involving commercially pure titanium welds. Figure 3d shows the details of the weld metal microstructure. It consists of a larger grain size whose inside contains parallel a cells in different orientations surrounded by phase. This bore out the tendency expressed in literature (Danielson, Wilson and Alman, 2003) that the higher the energy input, the greater the spacing between these cells, as in welding program #A, which has slightly larger grains when compared with the other welding programs. Table 4 presents data related to the grain size of the base metal and the HAZ. It can be observed that the average grain size values increase in line with the gradual welding energy input increase, following the sequence #B (average grain size = 93 m), #C (average grain size = 122 m) and #A (average grain size = 193
Table 4: Measurements of the base metal and heat affected zone grain size

Figure 3: Optical micrographs of the regions of Orbital GTAW. #B welding program. Etchant: Krolls reagent. Magnification: 100x. (a) Base metal microstructure; (b) Base metal/HAZ transition micro structure; (c) HAZ micro structure; (d) Fusion zone micro structure.
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m), which confirms recent research data (Barreda et al., 2001; Yunlian et al., 2000; Sundaresan, Ram and Reddy, 1999). Contrary to the adjoining region between the base metal and the HAZ, whose outlines are well defined, the connecting or transition area located between the fusion zone and the heat affected zone cannot be precisely defined because of the similar microstructural characteristics of both regions. Similar difficulties were described by Lathabai, Jarvis and Barton (2001) and Danielson, Wilson and Alman (2003). The grains achieve their maximum size in the area where the metal fusion takes place. Figure 4 shows an SEM obtained image of the microstructures present in a weld. The sample is from the welding program #A, which corresponds to the highest energy supply. The data here corresponds with that supplied by OM analysis.

Table 5:

Results of tension tests

The greatest reduction corresponded to the program with the highest energy level (#A). In contrast, the values which were closer to those of the base metal are those attributed to the welding cycle with the lowest energy input (#B). The mechanical tensile test results, independently of the welding program used, are in agreement with the Chinese Standards (CAST, n.d.), in that they impose an acceptance criterion of 80% minimum strength for the welded joints in relation to the values obtained for the base metal. In this study, all the obtained values, without exception, were above the minimum specified level. There were recorded levels of 87.5, 90.5 and 91.5%. The microhardness profiles of the welded samples pertaining to the different welding programs are shown in Table 6. One characteristic that the three welding programs have in common is the vicinity of the results.
Table 6: Results of Vickers microhardness (HV100)

Figure 4: Scanning electron micrographs of the regions of Orbital GTAW. #A welding program. Etchant: Krolls reagent. Magnification: 500x. (a) Base metal micro structure; (b) Base metal/HAZ transition micro structure; (c) HAZ micro structure; (d) Fusion zone micro structure.

Mechanical properties With regard to the tensile properties (Table 5), there is a remarkable similarity in the tensile strength values. It is important to mention that in all test samples the failure location occurred away from the weld metal. Programs #A, #C and #B presented reductions of 12.5, 9.5 and 8.5%, respectively, of the ultimate tensile strength when compared to the base metal.

Independently of the welding program used, the lowest microhardness values are associated with the fusion zone region of the test specimens, while the highest values are located in the base metal.
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In an analogous manner to the ultimate tensile strength, the increasing microhardness values, displayed by the programs #A, #C and #B, are equivalent to the decreasing order of welding energy, as was expected. In order to facilitate the interpretation of the results, correlations of the mechanical properties of the welded joints are made with their equivalent microstructures. The higher welding heat inputs used in #A which are the reason for the significant coarse grain sizes in the HAZ and fusion zone, as well as for the greater spacing between the colonies of parallel plates of the a phase found inside the grains showed the lowest levels of ultimate tensile properties and microhardness when compared with the other two programs. The microhardness values, which are almost similar to the fusion zone and the HAZ, are justified by the proximity of the grain sizes in these areas. Traditionally, literature regarding material presents analogies in relation to its properties. One of these examples refers to the relationship between the grain size, hardness and strength, calculated by the following equations: H = H0 + k.h.d-1/2 s = s0 + k.d-1/2 (1) (2)

Figure 5: Analysis of the fracture surface. (a) Tension specimen with rupture; (b) detail of the fracture surface; (c), (d) and (e) SEM of the fracture surface of different magnifications (500, 1000 and 3000x, respectively).

Where H is the hardness; s the yield strength; d the diameter of the average grain size; kh and k are angular coefficient of the straight lines; H0 e s0 are the intersections of the straight lines with the ordinate axis. In accordance to the Eq. 1 and 2, the hardness and yield strength values are inversely proportional to the average grain size, thereby confirming the results obtained in this study (Tables 4, 5 and 6). In comparison, the smallest grain found in program #B, correspondent to the lowest heat input, provides the best results in terms of mechanical properties, as it presents the smallest grain size, the best hardness and ultimate tensile strength levels (Dieter, 1981). Analysis of the fracture surface As shown in Figs. 5a and 5b, the tension specimen presented a ductile fracture, as the rupture is preceded by a localized plastic deformation characterized by a reduction in diameter. Its surface is predominantly irregular and grey colored, like that of the extremities of the tension specimen (Fig. 5b). Observations of both faces of the tension specimen confirm that the fracture is predominantly caused by shearing. In this kind of fracture, the crack expands in shear planes at a 45 angle to the longitudinal axis (ASM , 1997; Wulpi, 1999).

Studies indicate that the fracture begins in the central section of the tension specimen, in a plane which is macroscopically normal in relation to the axis where the tensile stress is being applied. As the deformation progresses, the crack expands in the direction of the tension specimen surface. This phenomenon is related to the nucleation of small microcavities (dimples). In general, this is associated with inclusions, second phase particles, fine oxide particles and, finally, with grain boundary triple points for high purity metals. The coalescence of these cavities results in their growth when stress is applied and is responsible for the development of a ductile fracture (Dieter, 1981; Wulpi, 1999). The analysis of the fracture surface using SEM is shown by means of three photos of different magnifications (500, 1000 and 3.000x), which are shown in Figs. 5c, 5d and 5e. The area of rupture reveals the presence of dimples of varying sizes. The larger ones refer to points of spaced nucleation and are fewer in number, which permits the development of microcavities before these themselves coalesce. The smaller ones are formed from a large number of points close to one another. Therefore, the size of the dimples and the aspect of the fracture surface are related to the number and distribution of the nucleated microcavities from external stresses (ASM, 1997; Wulpi, 1999). The predominance of areas containing dimples with conical equiaxial morphology was noted. These are characteristics of fractures caused by uniaxial load conditions, such as tension tests. In some areas, there was a prevalence of shallow and elongated dimples, which were formed because of the shear fracture rupture mechanism. In this case, the dimples pointed in the direction of the shear fracture on both surfaces of the fracture, but with opposing directions, depending on the slip direction.

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On the contrary, where there were tear fractures, the dimples indicated a one-way fracture, determined by the coalescing mechanisms of the microcavities (Dieter, 1981; ASM, 1997; Wulpi, 1999). In short, the fracture is located in a part of the test specimen about 31 mm away from the center of the weld bead. The temperature levels reached here are not sufficient for eventual microstructure transformations. There was no evidence of cracks, pores or inclusions. CONCLUSIONS Programs #A, #B e #C, developed for Orbital GTAW of titanium tubes, proved to be adequate and displayed satisfactory mechanical results for the welded joint. Program #A (pulsed current and increasing speed) produced a weld bead with a lower hardness and ultimate tensile values, which was attributed to the greater grain size and spacing between the colonies of parallel plates of a phase. Both of these are characterized by a low cooling rate. Program #B (continuous current), correspondent to a lower heat input value, provided the best result between the hardness and mechanical properties due to the smaller grain size. REFERENCES American Society for Metals (ASM), Fractography, 9th ed, ASM, Ohio, USA. 1997,

American Phamaceutical Show, Centro Costa Salguero, Buenos Aires, Argentina, Available at: <http://www. arcmachines.com/appPages/atw02.html>. Access on Oct 24, 2001. Chinese Academy of Space Technology (CAST), n.d., Chinese Standard CBERS propulsion subsystem pipe integrating and welding requirement (specification). Chinese Academy of Space Technology (CAST), n.d., Chinese Standard CBERS propulsion subsystem pipe leakage check requirement (specification). Danielson, P., Wilson, R., Alman, D, 2003, Microstructure of titanium welds, Advanced Material & Processes, Vol. 161, No 2, pp. 39-42. Dieter, G.E., 1981, Metalurgia mecnica, 2nd ed, Ed. Guanabara Koogan, Rio de Janeiro, Brazil, 653p. Gould, J.E., Becker, D., Williams, J.C., 1980, Microstructural characterization of titanium weldments, In: Kossowski, R., Glicksman, M.E. (Eds.), Physical Metallurgy of Metal Joinning, The Metallurgical Society of AIME, Warrendale, PA, USA, pp. 199-221. Henon, B.K., n.d., Matsushita completes ultra high purity nitrogen system reducing contaminants to PPB levels. Available at: <http://www.arcmachines.com/appPages/ masca02.html>. Access on Oct 22, 2001. Henon, B.K., n.d., Practical application of orbital tube and pipe welding, Reprinted of Practical Welding Today. Available at: <http://www.arcmachines.com/appPages/ pract02.html>. Access on Nov 17, 2001. Henon, B.K., 1998, Orbital welding of small diameter tubing, Reprinted of Tube International, 03/1998, Available at: <http://www.arcmachines.com/appPages/ smalldia02.html>. Access on Oct 24, 2001. Lathabai, S., Jarvis, B.L., Barton, K.J., 2001, Comparison of keyhole and conventional gas tungsten arc welds in commercially pure titanium, Materials Science and Engineering A, Vol. 299, No 1-2, pp. 81-93. doi: 10.1016/ S0921-5093(00)01408-8. Littlewood, G., Henon, B.K., 2000, A case study of the installation of an orbitally welded higienic piping system. Reprinted of Pharmaceutical Technology Europe, 03/2000. Available at: <http://www.arcmachines.com/appPages/ pharmeo02.html>. Access on Oct 10, 2001. Mannion, B., 1999, The fundamentals of orbital welding, Welding Design and Fabrication, Feb., pp. 22-26.

American Welding Society (AWS), 2000a, AWS B4.0M:2000. Standard methods for mechanical testing of welds, AWS, Miami, FL, USA. American Welding Society (AWS), 2000b, AWS D10.6/ D10.6M:2000. Recommended practices for gas tungsten arc welding of titanium pipping and tubing, AWS, Miami, FL, USA. Arc Machines, Inc., 2001, Orbital welding delivers treatment plant on time. Welding Journal, Mar., pp. 51-52. Barreda, J.L., et al., 2001, Electron bean welded high thickness Ti6Al4V plates using filler metal of similar and different composition to the basic plate. Vacuum, Vol. 62, No 2-3, pp.143-150. doi: 10.1016/S0042207X(00)00454-1. Brond, A., Henon, B.K, 2000, Orbital welding technology for pharmaceutical piping systems. Latin

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Morgan, J., Henon, B.K., 1999, Discovering applications for orbital fusion welding. Reprinted of The Tube & Pipe Journal, 03/1999. Available at: <http://www.arcmachines. com/appPages/tpj02.html>. Access on Oct 24, 2001. Orbimatic, n.d., Origins and development of orbital welding, Available at: <http://www.subcontractingtalk. com/news/orb/orb131.html>, Access on Apr 11, 2003. Orlowski J.A.G, et al., 2007, Development of the Welding Technology of Titanium by the Orbital TIG Process for the Brazilian Airspace Segment. Part 1: Experimental Setup. Soldagem & Inspeo, Vol. 12, No 1, pp.46-54. Sundaresan, S., Ram, G.D.J., Reddy, G.M., 1999, Microstructural refinement of weld fusion zones in a titanium alloys using pulsed current welding. Materials

Science & Engineering A, Vol. 262, No 1-2, pp. 88-100. doi: 10.1016/S0921-5093(98)01010-7. Wulpi, D.J., 1999, Understanding how components fail. 2nd ed. ASM International, Ohio, USA, 262p. Yung, W.K.C, et al., 1997, An investigation into welding parameters affecting the tensile properties of titanium welds. Journal of Materials Processing Technology, Vol. 63, No 1-3, pp. 759-764. doi: 10.1016/S09240136(96)02719-7. Yunlian, Q., et al., 2000, Electron beam welding, laser beam welding and gas tungsten arc welding of titanium sheet. Materials Science & Engineering A, Vol. 280, No 1, pp. 177-181. doi: 10.1016/S09215093(99)00662-0.

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doi:10.5028/jatm.2010.02027210

Technological Institute of Aeronautics So Jos dos Campos Brazil mafraga@ita.br

Mariana Amorim Fraga*

Technological Institute of Aeronautics So Jos dos Campos Brazil rspessoa@ita.br

Rodrigo Svio Pessoa

Technology roadmap for development of SiC sensors at plasma processes laboratory


Abstract: Recognizing the need to consolidate the research and development (R&D) activities in microelectronics fields in a strategic manner, the Plasma Processes Laboratory of the Technological Institute of Aeronautics (LPP-ITA) has established a technology roadmap to serve as a guide for activities related to development of sensors based on silicon carbide (SiC) thin films. These sensors have also potential interest to the aerospace field due to their ability to operate in harsh environment such as high temperatures and intense radiation. In the present paper, this roadmap is described and presented in four main sections: i) introduction, ii) what we have already done in the past, iii) what we are doing in this moment, and iv) our targets up to 2015. The critical technological issues were evaluated for different categories: SiC deposition techniques, SiC processing techniques for sensors fabrication and sensors characterization. This roadmap also presents a shared vision of how R&D activities in microelectronics should develop over the next five years in our laboratory. Keywords: Silicon carbide, Sensors, Aerospace applications, Roadmap, Project planning.

Technological Institute of Aeronautics So Jos dos Campos Brazil homero@ita.br

Homero Santiago Maciel

Technological Institute of Aeronautics So Jos dos Campos Brazil massi@ita.br

Marcos Massi

Technological Institute of Aeronautics So Jos dos Campos Brazil ivo@ita.br *author for correspondence

Ivo de Castro Oliveira

INTRODUCTION Silicon carbide (SiC) has been widely studied as an electronic material since 1959, when Shockley, the inventor of the bipolar transistor, recognized this material as essential to enable the development of microelectronic devices that can withstand harsh environmental conditions where silicon cannot be used or have limited applications such as high temperatures and intense radiation (Shockley, 1959). The potential of SiC for these applications is due to its inherent properties as excellent thermal stability, high resistance to chemical attack, high hardness, high bandgap, high electric field breakdown and high saturation current of electrons (Rajab, 2005). Several techniques for obtaining thin films and bulks of SiC have been developed. Some companies that manufacture crystalline silicon wafers also offer SiC bulk wafers up to 3 inches in diameter. However, a SiC wafer has an average price fifteen times more than the Si wafer with the same dimensions (Muller et al., 2001). Besides the high cost, another problem of the use of SiC substrates is the difficult micromachining process and high density of defects (Wu et al., 2001). In this context, there is a crescent interest in deposition techniques of SiC films on Si or SOI (SiliconOn-Insulator) substrates. These films can be produced in crystalline and amorphous forms.
Received: 01/06/2010 Accepted: 30/06/2010

Crystalline SiC films are produced by techniques that use temperatures higher than 1000C such as Chemical Vapor Deposition (CVD), Molecular Beam Epitaxy (MBE) and Electron Cyclotron Resonance (ECR) (Sarro, 2000). The high temperatures involved in these techniques generally become impracticable for the processing of these films in conjunction with conventional microelectronics processes. Hence, the plasma-assisted techniques such as Plasma Enhanced Chemical Vapor Deposition (PECVD) and sputtering, that allow obtaining SiC films at temperatures below 400C, are very attractive (Prado, 1997). However, SiC films produced at low temperatures are amorphous and their properties are different from those observed in crystalline structures. In general, amorphous films have lower elasticity modulus and higher electrical resistivity. Since the 1970s, many studies have been performed on doping of amorphous SiC films in order to obtain properties near to crystalline for applications at different types of devices such as photovoltaic cells, optical sensors, diodes and thin film transistors (TFTs) (Spear and LeComber, 1975; Kanicki, 1991; Tawada et al., 1982). Nowadays, the processes most used to doping of SiC films are in situ doping (during film growth) and ion implantation. In the 1990s, due to emerging MEMS (Micro Electro Mechanical Systems) technology and the increasing demand for sensors operating at temperatures above 300C for different applications, SiC films and substrates
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started to be used as alternatives to silicon in the fabrication of sensors to operate in severe environments as combustion processes or gas turbine control, oil industry, nuclear power and industry process control (Cocuzza, 2004). Some sensors and electronic devices based on SiC that are currently commercially available are showed in Fig.1 (Nowak, 2005).

the laboratory by RF magnetron sputtering technique had appropriate characteristics for applications in electronics and MEMS (Micro Electro Mechanical Systems) devices (Rajab et al., 2006). In this context, in 2005 a PhD thesis on development of piezoresistive sensors based on SiC films was started with support from CNPq/Microelectronics National Program (PNM) (Fraga, 2009). In this thesis, besides the RF magnetron sputtering, the PECVD technique was used to produce the SiC films. This allowed comparing the properties of SiC films produced by both deposition processes. In addition, the influence of nitrogen doping on SiC film characteristics was also investigated (Fraga et al., 2008a; Fraga et al., 2008b). The reactive ion etching (RIE) of SiC films using SF6/ O2 gases mixtures was another process studied, because this step is very important in the fabrication of devices. The etching rate was investigated as a function of film composition and O2 concentration. The influence of thermal annealing on etching characteristics was also evaluated (Fraga et al., 2007a; Fraga et al., 2007b).

Figure 1: SiC-based devices commercially available.

As there is a great interest in the use of SiC in high temperature devices, especially for applications in aerospace and aeronautics fields, LPP-ITA has established a R&D line oriented to the development of SiC sensors as presented in the next sections. ANTECEDENTS OF R&D ACTIVITIES IN MICROELECTRONICS Since 1988, LPP-ITA has carried out research projects on plasma technology applications. One of the main research lines in this field is directed to synthesis and modification of semiconductor thin films through low temperature plasma processes such as radiofrequency (RF) magnetron sputtering, plasma enhanced chemical vapor deposition (PECVD), reactive ion etching (RIE) and inductively coupled plasma (ICP). The R&D activities in microelectronics were intensified in 2001, when a clean room environment was implemented through a financing of the So Paulo Research Foundation (FAPESP). The development of specific researches related to growth and characterization of SiC thin films were started in 2003 leading to a master thesis about the effect of thermal annealing on physical and electrical properties of SiC films (Rajab, 2005). This project was supported by a grant from CNPq/Microelectronics National Program (PNM). The results obtained during this thesis work showed that the SiC films produced in
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The evolution of R&D activities related to the development of SiC films at Plasma and Processes Laboratory is summarized in Fig. 2. In 2008, in order to make possible the development of devices based on SiC films, a collaboration project was established with the Microfabrication Laboratory of the Brazilian Synchrotron Light Laboratory (LNLS). The first devices developed through this project were strain gauges based on SiC films. The structure of these strain gauges consists of a SiC thin-film resistor with Ti/Au electrical contacts (Fraga et al., 2010a). Subsequently, a prototype of piezoresistive sensor based on SiC film was designed, fabricated and characterized (Fraga et al., 2010b). The development cycles of the SiC sensors are shown in Fig. 3. As it can be observed, two steps have not been performed in LPP-ITA yet: pattern transfer by photolithography and wire bonding process. CURRENT STAGE OF R&D ACTIVITIES The current stage of R&D activities at LPP-ITA aims to implement a technology roadmap for development of SiC sensors (Fig. 4). In this section, the roadmap development process is explained. The development process is divided into the following stages.

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Technology roadmap for development of SiC sensors at plasma processes laboratory

Figure 2: Evolution of R&D activities related to development of SiC films at Plasma Processes Laboratory.

Figure 3: Current development cycles of SiC sensors.


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Figure 4: Roadmap development process.

Needs identification This is the first stage of the process in which occurs the identification of the needs related to the SiC sensors technology development. These needs are grouped in three main categories: infrastructure, financing and human resources. Nowadays, the Plasma and Processes Laboratory counts on financing of the Brazilian Space Agency (AEB) to assemble a room for characterization of electronics and MEMS devices. Besides, the clean room facilities have been amplified with the recent acquisitions of an oxidation furnace, a KOH etching system and a hot plate through the financial support of the National Council for Scientific and Technological Development (CNPq). Additionally, a dual dc magnetron sputtering system for the growth of SiC films, from targets of silicon and carbon, is being implemented. The idea of this system is to control the stoichiometry and improves the quality/functionality of the films through use of pulsed dc power sources. The main needs associated with infrastructure are the clean room area enlargement and the acquisition of a mask aligner in order to perform all steps of sensors fabrication in the laboratory. In relation to human resources, since December 2009 the National Post-Doctoral Program (PNPD)/CAPES finances two grants on development of SiC sensors. Form working group to the development of roadmap Due to the interdisciplinary nature of SiC sensors technology, researchers from a wide variety of backgrounds
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are required to form roadmap working groups. The staff of Plasma Processes Laboratory consists of 42 members, and this interdisciplinary background has degrees in physics, material science, microelectronics and engineering. Five PhDs and one PhD student of these staff are working at the moment on researches related to SiC sensors. This working group discussed the framework roadmap and, subsequently, a methodology was adopted considering the itemization of issues and responses to each critical step and identification of the key technologies. The determination of a realistic timeline and of a cost range for the processes implementation was also required. In order to define an action plan roadmap, the working group divided the critical technologies into three categories: a) SiC deposition techniques;

b) SiC processing techniques for sensors fabrication; c) SiC sensors characterization.

For each category, the working group will define goals, the impact of the technology, the timeframe for development and the execution plan. Execution action plan A detailed project plan with indication of roles and responsibilities of each working group member is being finalized. A funding strategy will be developed to overcome critical infrastructure issues.

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Technology roadmap for development of SiC sensors at plasma processes laboratory

The progress of roadmap execution action plan will be evaluated by regular review of the project status and deliverables. The expectative is that the implementation of this roadmap raises the level of sharing and integration among staff, facilities and services of the laboratory. This allows that the researchers quickly define the key services and that they focus on the technical challenges. To help its staff keep pace with the changes in science and technology, the laboratory have formed masters and PhDs in plasma physics, materials science and microelectronics. PERSPECTIVES UP TO 2015 The development of the SiC sensors is based on progress in the following technologies: 1) improved electrical and mechanical properties of SiC films produced (optimization of SiC deposition process), 2) SiC film processing (optimization of etching process and metallization appropriate for high temperature applications), 3) microfabrication technology to fabricate miniaturized sensors and 4) sensors packaging for harsh environments. The R&D activities of the Technological Institute of Aeronautics have been focused on aerospace and aeronautical fields. In this manner, the goal of Plasma and Processes Laboratory is to develop SiC sensors with potential for use in a range of these applications. The sensor types of main interest are capable of measuring pressure, strain and acceleration under high temperatures and in the presence of corrosive media or intense radiation. Figure 5 shows the types of sensors that are being developed and the technological evolution that we intend to follow till 2015. The main technologies involved and some possible applications also are shown. In the next years, our goals will be concentrated in improving the performance of the SiC pressure sensors and strain gauges developed, besides making possible the development of accelerometers and SAW sensors based on the aluminum nitride (AlN) films deposited on SiC. CONCLUSIONS The vision expressed in this roadmap is to use the knowhow of Plasma and Processes Laboratory staff to develop SiC sensors. We believe that the way to do this is developing technologies, which enable science, engineering and manufacturing. Close cooperation between the laboratory and other research centers will always be necessary because this cross-disciplinary development will bring broad benefits through ideas, instruments and techniques that will result from developing and consolidating the required base technology.

Figure 5: Roadmap for development and application of SiC sensors.

ACKNOWLEDGMENTS The financial support of PNPD/CAPES is strongly acknowledged. The authors also thank the National Council for Scientific and Technological Development (CNPq), Brazilian Space Agency (AEB), Brazilian National Synchrotron Light Laboratory (LNLS/MCT), Associate Laboratory of Sensors and Materials (LAS/ INPE), the Center for Semiconductor Components (CCS/ UNICAMP) and the Department of Precision Mechanical of FATEC-SP. REFERENCES Cocuzza, M., 2004, Development of Silicon and Silicon Carbide-Based Micro-electromechanical Systems, PhD thesis in Electronics, University of Trento. Fraga, M. A., 2009, Desenvolvimento de sensores piezoresistivos de SiC visando aplicao em sistemas aeroespaciais, PhD thesis in Mechanical Engineering, Technological Institute of Aeronautics. Fraga, M. A. et al., 2010a, Effect of nitrogen doping on piezoresistive properties of a-Six Cy thin film strain gauges, Microsystem Technologies, Vol. 16, pp. 925-930. Fraga, M. A. et al., 2010b, Fabrication and characterization of piezoresistive strain sensors for high temperature applications, Proceedings of IEEE International Conference on Industrial Technology (IEEEICIT), pp. 513-516.
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Fraga, M. A. et al., 2008a, Nitrogen doping of SiC thin films deposited by RF magnetron sputtering, Journal of Materials Science: Materials in Electronics, Vol. 19, pp. 835-840. Fraga, M. A. et al., 2008b, Etching Characteristics and Surface Morphology of Nitrogen-Doped a-SiC Films Prepared by RF Magnetron Sputtering, Proceedings of Symposium on Microelectronics Technology and Devices, ECS Transactions, Vol. 14, pp. 375-384. Fraga, M. A. et al., 2007a, Etching Studies of PostAnnealed SiC Film Deposited by PECVD: Influence of the Oxigen Concentration, Proceedings of Symposium on Microelectronics Technology and Devices, ECS Transactions, Vol. 9, pp.227-234. Fraga, M. A. et al., 2007b, Synthesis and Etching of Amorphous Silicon Carbide Thin Films with High Carbon Content, Revista Brasileira de Aplicaes de Vcuo, Vol. 26, pp.193-197. Kanicki, J., 1991, Amorphous and microcrystalline semiconductors devices, Artech House, Norwood. Muller, St. G., 2001, Progress in the industrial production of SiC substrates for semiconductor devices, Materials Science and Engineering B, Vol. 80, pp. 327-321. Nowak, O., 2005, Press Release Wicht Technologie Consulting, Silicon Carbide Electronics Markets 20042009: New Horizons for Power Electronics, USA.

Prado, R. J., 1997, Propriedades qumicas e morfolgicas de filmes hidrogenados de carbeto de silcio amorfo, Dissertao de Mestrado apresentada ao Instituto de Fsica da USP. Rajab, S. M., 2005, Efeitos do recozimento trmico nas propriedades fsicas e eltricas do filme de carbeto de silcio, Master Dissertation in Mechanical Engineering, Technological Institute of Aeronautics. Rajab, S. M. et al., 2006, Effect of the thermal annealing on the electrical and physical properties of RF magnetron sputtering produced SiC thin films, Thin Solid Films, Vol. 515, pp. 170-175. Sarro, P. M., 2000, Silicon Carbide as a new MEMS technology, Sensors and Actuators A, pp. 210-218. Shockley, W., 1959, Method of growing silicon carbide crystals, Proceedings of the First International Conference on Silicon Carbide, Boston. Spear, W.E., LeComber, P. G., 1975, Substitutional doping of amorphous silicon, Solid State Communications, Vol. 17, pp. 1193-1196. Tawada, Y., et al., 1982, Properties and structure of a-SiC:H for high-efficiency a-Si solar cell, Journal of Applied Physics, Vol. 53, pp. 5273-5281. Wu, H. et al., 2001, Fabrication and Testing of Single Crystalline 3C-SiC piezoresistive Pressure Sensors, Eurosensors XV, International Conference on Solid-State Sensors and Actuators.

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doi: 10.5028/jatm.2010.02025410

Marcela Barbosa de Moraes*

Universidade de Taubat Taubat Brazil marcelabmoraes@gmail.com

Francisco Cristovo L. Melo

Instituto de Aeronutica e Espao So Jos dos Campos- Brazil frapi@iae.cta.br

Analysis of technological innovation strategy for small and medium companies of the aeronautical sector
Abstract: The inherent risk in high-tech activity requires the construction of technological strategies that serve global strategy of the company. The present study aimed to characterize the technological position of small and medium technology-based companies of the aeronautical sector located in the Vale do Paraba, and to examine whether these companies have a technological strategy formalized and disseminated. The adopted methodology was a descriptive exploratory research, carried out through in-depth individual interviews conducted with the small e medium companys owners of the cities of Caapava, So Jos dos Campos and Taubat, Brazil. The authors concluded that it is necessary that companies, especially small and medium-sized, adopt a technological innovation strategy integrated with the companys overall strategy. This will help keeping them competitive within their specificities, and not only in the domestic market, but also in international markets. Keywords: Strategy, Technological innovation, Technological strategy, Small and medium technology-based companies. of how to establish a competitive advantage and how to ensure the survival of the company (Moraes et al., 2009a). Decide what future you want for the company, which technological strategy you have to follow to ensure this future, how to create and develop a climate which is favorable to innovation, which level of resources to allocate and how to develop this activity inside the corporation and in the market; this is one of the most complex and critical set of decisions that small and big companies have to face. An appropriate answer to these questions can ensure competitiveness and sustainability to these companies. Thereby, with the perspective of deepening the comprehension of this synthesis strategy, innovation and technology and the question of its application in small and medium technology-based companies, the matter of this research was formulated as follows: How can a strategic program, aimed at technological innovation, leverage the segment of small and medium firms in the Paraba Paulista Valley? Within this context, the research proposal relates to the characterization of the technological position of small and medium technology-based companies of the Aeronautical sector located in the Paraba Paulista Valley, and to examine whether these companies have a technological strategy formalized and disseminated.
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Edson A. A. Querido Oliveira


Universidade de Taubat Taubat Brasil edson@unitau.br

Instituto Tecnolgico de Aeronutica So Jos dos Campos Brazil cabral@ita.br *author for correspondence

Arnoldo Souza Cabral

INTRODUCTION The increase in the speed of technological change and globalization have turned technological innovation into something that is vital to the business survival and growth. According to Moraes et al. (2009a), in an environment that is more dynamic, competitive and increasingly complex, the strategies, represented by business decisions and actions that guide the organization in the search for success and technological innovation, playing a fundamental role in the life of technology-based companies, have become much more important and, at the same time, much more difficult to set and implement. In this sense, Clark and Wheelwright (1993) observed that in most industries of Japan, Europe or the United States, executives recognized that the development area of new products and processes (innovation) offers the greatest opportunities and that companies need to develop their capabilities. In other words, innovation, especially technology, is recognized as a major source of competitive advantage. Another important point is technological strategy, which becomes a central ingredient in the concept of company, and technology now represents one of the basis of strategic planning, guiding the fundamental question
Received: 05/02/10 Accepted: 20/04/10

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THEORETICAL REFERENTIAL This section constitutes a literature review of existing ideas about small and medium technology-based companies, the Brazilian Aeronautical Industry, Technological Innovation and Technological Strategy. This approach aims to establish how the relationship is developed between the mentioned areas. Small and medium technology-based companies The technology-based companies play an important role in the economic and social development of the country, contributing to innovation in products of high market potential, besides creating qualified jobs, stimulating the process of science and technology and narrow the relations between various bodies and sectors of the economy. For a better understanding of what a technology-base company is, it is necessary to characterize the concept of technology-based. The Associao Catarinense de Empresas de Tecnologia (ACATE, 2008) divides the technology-based into two topics: process or product that results from scientific research and whose aggregate value comes from the areas of advanced technology such as computers, biotechnology, fine chemicals, new materials, mechanics of precision, among others; application of scientific knowledge on complex techniques and on the high technical qualification work.

The Associao Nacional de Entidades Promotoras de Empreendimentos Inovadores (ANPROTEC) defines a technology-based company as an enterprise that support the productive activity in the development of new products and processes, based on the systematic application of scientific and technological knowledge and on the use of advanced and pioneering techniques (ANPROTEC, 2002). Technological innovation is, therefore, one of the benefits that technology provide to the market. Beaver and Prince (2004) argue that the definition and classification of small and medium technology-based companies is very complex. In Brazil, there is not a specific concept for these companies, so they are defined in a general concept which is associated with their size and not with their established activity, based on quantitative and qualitative criteria. The quantitative criterion is divided into two sub criteria: by number of employees, criterion adopted by Sebrae (Servio de Apoio s Micro e Pequenas Empresas), accordingly to the Status of Micro and Small Enterprise; the gross operating revenue according to the Brazilian Development Bank (BNDES) and indicates the operational and accounting movement of the firms.

The concept of technology-based is founded on these two points, implementation of scientific research and applying this knowledge to develop new technologies (Bert, 2006). Valrio Netto (2006, p. 3-4) defines the technologybased companies as those that adopt new technologies in their production process, including both manufacturing companies as services companies with high content of knowledge.

Leone (1991) states that the first criterion is both economical and social, because it offers indications of social problems related to the absorption of labor, level of income and productivity. About the second criteria, the author emphasizes that though it reflects the size of the market of the companies, it is vulnerable, because it may vary according to the fluctuation of the currency or changes in accounting criteria. The Table 1 details the criteria for classification by number of employees and by annual gross operating revenue. The quantitative criterion is important, because companies, according to their size, can often enjoy the benefits and

Table 1: Criteria for classification of micro, small and medium companies in Brazil

Industry Micro Small Sebrae Until 19 20 to 99 employees employees BNDES Until R$ 1,2 More than R$ million 1,2 million and less than R$ 10,5 million Source: Sebrae (2007) and BNDES (2008).
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Institution

Criteria for classification Medium 100 to 499 employees More than R$ 10,5 million and less than R$ 60 million Micro Until 9 employees Until R$ 1,2 million

Trade and services Small Medium 10 to 49 50 to 99 employees employees More than R$ More than R$ 1,2 million and 10,5 million less than R$ and less than 10,5 million R$ 60 million

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incentives provided by the Brazilian Legislation based on public policies (Bert, 2006). These policies aim at: increasing exports, generating employment and income and reducing informality of small and medium businesses. The qualitative criterion refers to the internal structure of the company, as well as the organization and management style (Bert, 2006). In this manner, a more accurate vision of the company is provided, that is, it is related to the direction styles, the profiles and attitudes of leaders and their perception of the environment. Leone (1991) explains that while the quantitative criterion provides a static image to the company, the qualitative criterion appear to offer a vision of movement, more action from management, in other words, it describes the operation of the company, the movements of staff, material resources and operations with suppliers and customers. Finally, the importance of small and medium technologybased companies to regional development occurs through the economic and social benefits that they provide to their region, especially in terms of process of industrialization, search for competitiveness and technological development (Bert, 2006). The Brazilian aeronautical industry: a historical overview In Brazil, the effort to create the basis of aeronautical and aerospace sector reaches 1945, when the Ministry of Aeronautics, created on January 21st, 1942, by law n 2961, designed and implemented the Aerospace Technological Center (CTA). On January 16th, 1950, CTA was running his engineering school, the Aeronautical Technology Institute (ITA), as the first class of ITA began their studies in 1947 in So Jos dos Campos (Lima et al., 2005). According to Rodrigues (2008), the city of So Jos dos Campos was chosen as the appropriate location for the installation of CTA due to some factors such as: location on the banks of the old road Rio So Paulo (nowadays, called President Eurico Gaspar Dutra Road Via Dutra), topographical features and climatic conditions favorable to aviation, easiness of obtaining energy, proper distance from urban centers, proximity to the Port of So Sebastio and access to the medium and large-size industries installed in the surroundings of So Paulo city. Therefore, the creation of the Research and Development Institute in CTA, in 1954, reinforced the strategy of acquiring knowledge and self-sufficiency in key areas of the aeronautical industry, namely: aircraft design, electronics, materials, engines and flight tests (Lima et al., 2005).

Within this context, one can say that the center of this coordinated strategy has always been the target of this national capacity in the technological and industrial sectors. In October 1954, the Brazilian Aeronautics Industry started with the foundation of the Neiva Aeronautics Building Society, installed in the Manguinhos Airport, Rio de Janeiro. In 1960, the company opened an office in So Jos dos Campos, nearby CTA, aiming to increase research and development of aircraft (Rodrigues, 2008). Amato Neto and Santos (2005) argue that in spite of the effort for aviation, training bases have been founded in the 1940, being intensified in 1960, with the industry knowledge generated by the laboratories of CTA and added to other studies on engineering of other institutions. This fact allowed the suitability of products with world class standard in the sector. President Arthur da Costa e Silva, in August 19th 1969, under the leadership of Minister of Aeronautics, created the Embraer (Empresa Brasileira de Aeronutica S.A.), a private and public capital entity intended for serial manufacturing of aircraft (Rodrigues, 2008). According to Lima et al. (2005), Embraer is the main productive and technological core of the Brazilian industry, articulating a set of micro, small and medium supply companies around their economic activities. The aeronautical industry has had its development, especially with regard to Embraer, due to the incentives given by the government at the time of its creation (Silva, 2005). The author emphasized that the incentive was a concession by the militaries, from the donation of land in prime location to the required basic infrastructure, which was transferred from the Research and Development Institute directly to Embraer. Finally, the aerospace industry in Brazil is expected to reach the turnover of US$ 7.8 billion with the occupation of 27 thousand jobs in 2010 (Moraes et al., 2009b). To achieve these estimates, it is necessary to invest in the strengthening of small and medium companies of the aerospace sector (Bartels, 2003 apud Amato Neto and Santos, 2005). The city of So Jos dos Campos has become an aerospace pole due to its topographic conditions, climate and location. The city received federal investments and struggled for the implementation of this sector (Moraes et al., 2009b). Technological innovation In recent decades, the production systems have changed its organizational structures according to the market and

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environment in which they are inserted. In this process of changes, new technology of product and process are being introduced in the companies (Predrassoli, Silva and Ferreira, 2001), which has enabled the development of technological innovations. Technological innovation consists of an essential tool to increase the productivity and competitiveness of organizations, as well as to boost the regional development. For Tigre (2006), the development does not originate a simple growth of the existing economic activities, but rather reside fundamentally in a qualitative process of transformation of production structure to incorporate new products and processes and aggregate values to production through the intensification of the use of information and knowledge. The Frascati Manual (OCDE, 2002) defines innovation as the transformation of an idea into a new product, or into the improvement of a product that is introduced in the market, or new production systems and its diffusion, commercialization and utilization. According to Senz and Garca Capote (2002), the expression technology can be understood as a set of scientific and empirical knowledge, skills, experience and organization required to produce, distribute, commercialize and use goods and services. In this manner, it is possible to correlate technological innovation to the transformation of knowledge into products, processes and services that can be put on the market (Mattos and Guimares, 2005). It is important to emphasize that the origin of the concept of innovation can be credited to Joseph Schumpeter, when he made the conceptual distinction between invention and innovation. While the invention is related to the creation of a process, technique or new and inedited product, the innovation is associated with the process of creating a commercial product from an invention, in other words, involves both invention and commercialization (Schumpeter, 1982). In the vision of Schumpeter (1982), innovation is a set of new upgradeable functions that change the methods of production, creating new forms to organize work and to produce new products, also enabling the opening of new markets by creating new uses and consumption. The innovation that gives rise to the process and economic development or economic progress is the fundamental phenomenon of capitalist life, in other words, the capacity to generate innovation is the result of accumulation of technical and economic competences for survival and growth of companies in a certain country (Hiratuka, 1997).

Schumpeter (1982) explains that the economic development is the result of spontaneous and discontinuous changes, that is, the producer starts the economic change and the consumers are taught to want newness or things that differ in any aspect from those that they habitually use or buy. The author also emphasizes that the new combinations of productive resources or innovations in the development process include five alternatives (Schumpeter, 1982): Introduction of a new good a good that consumers are not familiar with yet; Introduction of a new method of production a method that has never been tested in the field of transformation industry, which in any way must be based on a original scientific discovery, and may also consist of a new way of commercially handling a commodity; Opening of a new market (market innovation) a market in which the particular branch of processing industry of the country concerned have not entered yet, whether this market existed before or not; Achievement of a new source of raw material supply of or intermediate input (input innovation) again, regardless of the fact that this source already exists or had to be created; and, Carrying out of a new industry organization (organizational innovation) creating a monopolist position or the fragmentation of monopolist position.

In summary, Schumpeter tries to explain how the circular flow is broken by the activation of the transformation capacity of the capitalist system, providing opportunities for economic expansion and for the economic cycle. Other important aspects for innovation are the technological changes. For Tigre (2006), these changes are differentiated by its degree of innovation and the extension of changes in relation to existing. The range of innovations observed in the economic activity is classified by Freeman and Soete (1997), as depicted in Table 2, according to its impacts. Finally, the innovation has been a main target for success not only to large-sized companies, as seen until 1997, but also for small and medium companies of various sectors (Tidd, Bessant and Pavitt, 2001).

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Table 2: Taxonomy of technological change

Daily improvement and changes. Radical Discontinuous jumps in products and process technology. New technological system Achieving changes that affect more than one sector and give rise to new economic activities. New technical and Changes that affect economical paradigm the whole economy involving technical and organizational changes by changing products and processes, creating new industries and establishing trajectories of innovations for decades. Source: Freeman and soete (1997). Technological strategy The technological strategy, as explains Coutinho (2004), becomes a central factor in the concept of company, and technology constitute a basis for strategic planning, guiding the fundamental question of how to establish a competitive advantage and how to ensure the survival of the firm. According to Morone (1989), the technology creates strategic opportunities; the innovative companies recognize these opportunities and build corporate strategy around them. Then, one can state that the strategy creates the technological needs. Coutinho (2004) argues that business and technology strategies are increasingly interdependent. However, the current dynamic of industry competition, the difficulty in identifying the potential impact of new technologies and the fact that the benefits of these technologies are not immediately quantifiable hinder this integration. Narayanan (2001) states that the concept of technological strategy has emerged in the period post World War II, when companies such as Westinghouse and General Electric sought to diversify through the efforts of R&D. From the recognition that technology was determining the competitiveness of technology-intensive industry, researchers and managers began to incorporate this dimension in business strategy (Coutinho, 2004). A paper presented by Prahalad, in 1974, identified the fundamental question that came to dominate further work in the area: Is the conception of a technological

Type of technological change Incremental

Character

strategy for the company realistic? (apud Kantrow, 1980). Rosenbloom (1978) answers this question with an emphatic yes. According to the authors, the concept of a technological strategy permits to build an integrated framework that is able to insert a technology of a company in the context of their business. Kantrow (1980) emphasizes that the studies carried out in the 1970s demonstrated the importance of technological decisions and its insertion in the context of strategic thoughts of companies. For Narayanan (2001), after this period, during the 1980s, the concept of technological strategy takes shape and begins to be idealized and developed. Therefore, the subject of technological strategy became important as companies wised up the probability of using technology as a competitive weapon (Burgelman, Maidique and Wheelwright, 1995). Friar and Horwitch (1985) argue that this awareness was due to the convergence of five historical forces: loss of faith in other basic strategies, apparent success of hightech small companies, the priority given to technology by Japanese companies, increasing awareness of the potential contribution of manufacturing strategy and process technology to competitiveness. According to Rieck and Dickson (1993), the term technological strategy is relatively new, as it was first mentioned in the literature on the beginning of the 1980s. Chiesa and Manzini (1998), the subject has attracted increasing attention, and models have been developed considering the technology as an input data in the process of strategy formulation, establishing a link between technological strategy and corporate and business strategies. For Maidique and Patch (1988), the technological strategy includes policies and decisions that impact on the technological processes of the company. It involves choices between new technological alternatives, the criteria by which they are incorporated by new products, processes and distribution of resources that will enable its successful implementation. Narayanan (2001) explains that the technological strategy is the pattern revealed in the technology choices of companies. The choices involve the commitment of resources to ownership, maintenance, exploitation and abandon of technological capabilities. These choices determine the character and extent of the main technical capabilities of the company and use the platform of processes and products available. Finally, Freeman and Soete (1997) identified six alternatives of technological strategy that should be taken as a spectrum of possibilities. These six alternatives are:
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Companies may select one or more strategies in different segments of their activities and change it over time; The choice of strategy is linked to the objectives of their executives and shareholders; The companies may decide to use their technical, managerial and financial capacities to seek alternatives that maximize return on investments at short term or thinking about building a technological basis for the future; They may turn to alliances with different partners or act independently; They may acquire technological packages or start developing their own solutions; and, Such decisions depend on financial and human available resources, on the characteristics of the markets, on the technological dynamics and on the explicit or implicit strategy that the company decides to follow.

or two attributes of the organization. The author also emphasizes that there is great predictive value, but focusing on one limited aspect or region of the companys behavior. Analyzing Table 3, one perceives that the authors are not based on a statistical analysis of data; they rather use their experience and knowledge about the industry. Nakano (1998), Narayanan (2001) and Loewe, Williamson and Wood (2001) explain that the strategies postulated in the proposed typologies are actually used by companies. In the typology presented by Ansoff and Stewart, in 1967, the strategies are based on the time when the product enters the market, in other words, they include strong marketing components (apud Nakano, 1998; Narayanan, 2001). The first company of the market will benefit from advantages of operating a temporary monopoly. It requires a strong commitment for Research and Development (R&D), the establishment of a technical leadership besides presenting a high rate of risk (Nakano, 1998; Narayanan, 2001). Following the leader or second on the market involves quick entry in growing markets based on the imitation of the pioneering innovations of direct competitors. The adoption of this strategy requires high development capacity (Nakano, 1998; Narayanan, 2001). The strategy of engineering application or market segmentation comprises the focus on specific market niches. It requires strong ability in engineering application such as good flexibility in the production area (Nakano, 1998; Narayanan, 2001). Adopting the strategy of Me Too or minimization of cost presupposes the capacity of obtaining relative advantages of cost through economies of scale, cost reductions from changes in process or product or by reducing overhead costs and controlling operating costs. It requires ability in product and process engineering (Nakano, 1998; Narayanan, 2001).

Technological positioning Numerous researchers have been trying to characterize and codify the technological strategies of the companies. However, the difficulty in understanding how the companies deal with aspects related to their technological strategy caused many of them to look for help in specific techniques and methodologies (Coutinho, 2004). There are several typologies for the strategic/technological positioning of the companies. These typologies are generally based on the time of entry of the product on the market (marketing), in innovation policy (technology), or the company strategy posture in relation to the environment (competition). For a better understanding, Nakano (1998) defines the typologies as special classifications that focus only one
Table 3: Typologies for technological posture of the company

Ansoff and Stuart (1967) Miles and Snow (1978) A. D. Little (1981) Freeman and Soete (1997) First on the market Defender Leader Offensive Follow the leader or Prospector Follower Defensive second on the market Analytical Niche Imitator Engineering Reactive Rational Dependent application and market Traditional segmentation Opportunist Me Too or Minimization of Cost Source: Adapted from Freeman and Soete (1997), Nakano (1998), Narayanan (2001) and Loewe, Williamson and Wood (2001). Tecnological strategy

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The typology of Miles and Snow, formulated in 1978, is based on strategy posture of the company in relation to its environment, that is, it incorporates elements of competition in innovation policy (Nakano, 1998). Companies with defensive strategy have a field of product and narrow market, seldom seeking new opportunities outside these limits. Profitability will come through the stability and efficiency (Nakano, 1998). The prospectors continuously seek new products and markets. They are constantly changing, often spending an idea of inefficiency, but always remain as a powerful force in the market (Nakano, 1998). The analytical companies combine aspects of defenders and prospectors. They put into action both stable form and changing. Reactive companies are slowly changing, unable or unwilling to change their fields of product and market. The change in their environment is noticed, but they can not accompany because there is not a consistent relationship between strategy and structure (Nakano, 1998). The typology of A. D. Little is based on two dimensions: scope and leadership. Decisions on the scope refer to the way firms answer the question: Which technologies should be explored? The decisions concerning technological leadership are related to the commitment of the company to pro-activity, which is expressed, in many cases, as pioneerism (Narayanan, 2001). The companies that are leaders in technology establish and maintain a competitive position through the development and exploitation of all technologies included in a certain market, providing a dominant position in this market (Narayanan, 2001). The technology is an important factor for creating and maintaining the competitive advantages in these companies. They seek competitive advantage through technological appropriateness. They can board a non-pioneer position in many cases. Therefore, they know that the market will be waiting for their input. Then, they avoid the initial phase of undefined of product, searching on their competences the knowledge to introduce a superior product for the pioneers, making it obsolete (Narayanan, 2001). The niche strategy is to focus on a limited number of critical technologies to seed the leadership. Technological Development is selective. Normally, it adopts the pioneering actions in order to take the market of the leader and build a pioneer reputation (Narayanan, 2001). Follower companies have expertise in a wide range of technologies. Their strategy is based on exploration,

avoiding the risks involved in basic research. For these companies, technology is not a primary instrument in the search for competitive advantage. They aim at acquiring skills that support their business corporate strategy (Narayanan, 2001). The Rational Companies comprehend those which possess knowledge in a selected group of technologies. For these companies, the technology deficit must be compensated by other competitive forces (Narayanan, 2001). The typology proposed by Freeman and Soete (1997) is based on how the company deals with technology in their innovation policy. The offensive innovation strategy has the characteristic of obtaining technological and marketing leadership by introducing new products. Normally, it is intensive in R&D and involves fundamental research. The defensive subject closely follows the leader and the technological change. The expense with R&D may be as high as those of the market leader, but a large portion of them seeks research application aiming to improve the products of competitors (Freman and Soete, 1997). The imitator company is interested in mimicking the innovations brought to the market. The expenses with R&D are reduced and there is an emphasis on the development and reduction of production costs (Freman and Soete, 1997). Companies with dependent strategy adopt reactive posture, promoting changes in products and processes only when requested by clients or headquarters. It is characterized by no expenses with R&D (Freman and Soete, 1997). The traditional strategy is used by companies that are under pressure to change their products. Market and competition do not require any adjustment in the product. Research and development are nonexistent and production processes are well developed (Freman and Soete, 1997). Finally, the opportunist company is constantly looking for opportunities in new markets while maintaining strict control over existing operations. The key to the success of this strategy is the control of costs and marketing innovations (Freman and Soete, 1997). METHODOLOGY This research adopted as methodology a formulation of exploratory descriptive research type, through individual in-depth interviews with owners of small and medium technology-based companies in the cities of Caapava, So Jos dos Campos and Taubat, Brazil.
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Data collected in the interviews were analyzed using qualitative approach, which allowed a clear and detailed description on knowledge of technological innovation and technological strategy of the owners in the small and medium technology-based companies of aeronautics sector of Paraba Paulista Valley. Population and sample Based on data collected from National Bank of Economic and Social Development (BNDES) (2007), currently, the cities Caapava, So Jos dos Campos and Taubat have an estimated population of 176 technology-based companies of small and medium size, in other words, these companies have annual gross operating revenue superior to R$ 1,2 million and inferior to R$ 60 million. Trivios (1987) defines population or universe as the set of people so that specific part of the environment in which the search will be conducted. The sample of this paper was probabilistic and finite, in other words, considering an estimated 5% error margin, 95% confidence interval and one-way variance, it had a sample of 36 small and medium technologybase companies. This number was obtained through the following equation (Spiegel, 1993):
Sample(n) = s2 Z 2 N s Z 2 + e 2 ( N 1)
2

According to technological strategic positioning of small and medium technology-based companies The present proposal of technological positioning assessment for small and medium technology-based companies takes as its starting point the analysis and proposals of Freeman and Soete (1997). For these authors, the technological strategy is based on the way that the company addresses the technology in its innovation policy. The privileged approach in this study has the innovation as purpose. The midpoint is to question the aptitudes that a company must initially hold so that the innovation occurs and be profitable. This conception is consistent with the proposal of Nelson and Winter (1982) which postulates the existence of routines to innovate on the basis of companies performance in dynamic competitive environments. To obtain this result, the study was initiated by analyzing a questionnaire on technological positioning which was applied to the owners of small and medium technologybased companies of aeronautics sector located in Caapava, So Jos dos Campos and Taubat. The Figure 1 shows the values in percentages obtained by the companies analyzed for each strategic/technological positioning. It was noted that 61% of small and medium technology-based companies of the aeronautical sector located in Caapava, So Jos dos Campos and Taubat are proactive followers, in other words, they adopt a defensive posture.

(1)

In which s2 is the variance; N is the population; Z is the confidence interval; is the margin of significance. Marconi and Lakatos (2000, p. 42) define sample as a portion and parcel, conveniently selected from the universe (population). In other words, is a subset of the studied population that shows certain characteristics in common. ANALYSIS OF THE RESULTS In Brazil, the domestic market is conservative and presents difficulty in introducing new features. It reduces the interest of companies in innovate, making them act only reactively, when there is the possibility of loss of market. Therefore, it is postulated in this section that there are business and technology strategies and postures that small and medium technology-based companies of the aeronautical sector in Caapava, So Jos dos Campos and Taubat can adopt in order to remain competitive within their specificities and not only in the domestic market but also internationally.
0 6 8

61

25

Buyer Reactive follower No opinion

Pro-active follower Imitator

Figure 1: Strategic positioning.

According to Freeman and Soete (1997), the defensive strategy shows that companies are closely following the leader and the technological changes. Expenses with R&D can be as high as those of the market leader, but a

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large portion of them seek research application aiming to improve the products of competitors. The interviewees reported, in general, that the firms differentiate their products from the knowledge of the clients business, that is, these companies have a product domain and a closed market, so they rarely look for new opportunities extrapolating these limits. We also checked that the reduction in the life cycle of products is leading to a decrease in the range of opportunities. The interviewees argue that the current age of discontinuity becomes difficult to survival of small and medium companies, which do not respond quickly to technological changes. From this perspective, one can say that the proactive followers companies have to be fast enough to ensure and increase the market share. Following, the reactive followers companies appear. Note that 25% of these companies promote changes in products and processes only when requested by customers or arrays, which means that they have a dependent strategy. It was also checked that these companies have reduced expenses with R&D and there is an emphasis on the development and reduction of production costs. The imitators posture is characterized by identifying the opportunities and copying the innovations brought to the market. It was noted that 8% of companies do not have expenditures with R&D. It was observed that 6% of the analyzed companies are characterized by being buyers of technology, in other words, Research and Development are nonexistent and the production processes are very developed. After the interviews, we found that imitators and buyer companies work with mature processes and products. They seek to minimize the operating cost (production, overheads and others), having scale and automation as main sources of competitive advantages. Finally, it was found that small and medium companies of the aeronautical sector of the cities of Caapava, So Jos dos Campos and Taubat do not have an offensive technological posture. One can say that the leadership companies are aimed to radical innovation, that is, bringing ideas, products and/or processes completely original to the market. According to business and technological strategies It is possible to say that there is no agreement on the definition and wide-ranging of what a technological strategy is, which makes it difficult to assess its contribution as a source of

competitive advantage. It is difficult to identify clear and measurable objectives for the technological strategy. According to Afuah and Utterback (1997), technological evolution requires different strategy for each phase of the life cycle of a product. The cumulative and differentiated nature of technological development in companies suggests that the dimensions used do not have to include and consider a variety of sources of technological opportunities and the different speeds and directions of their developments. These two aspects comprise the interfaces between technological, productive and organizational dimensions, making it difficult to identify which of them are representative and may account for performance gains in the company. The present proposal of assessment with small and medium technology-based companies of the aeronautical sector in Caapava, So Jos dos Campos and Taubat aims to identify how business and technological strategies are formalized and disseminated in the company. The Figure 2 shows the values in percentages obtained by the analyzed companies concerning the formalization and dissemination of business strategy. Analyzing the presented data, it was observed that 47% of the companies report having an informal business strategy, that is, they have an explicit business strategy, but it is restricted in some levels of management.

17 %

3% 0% 47 %

33 %

Forma l In process

Informal No opinion

An idea

Figure 2: Business strategy.

The interviewees reported that, when developing your business strategy, firstly it is necessary to analyze the changes on the environment, in other words, study the main environmental factors affecting the company and its likely development, as well as new factors that may exert influence in the future.

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And, posteriorly, it is necessary to analyze the resources and competences, that is, analyze the systematic efforts to expand the knowledge of the resources and the competence of the company in order to optimize the existing supplies by means of an effective and selective allocation. It was also noted that 33% of the companies reported having a formal, explicit and disseminated business strategy, which means that these companies strategically plan, organize, direct and coordinate the whole process. According to the answers, it was observed that the managers of small and medium companies establish a balance of the demands of internal and external environments, as well as the integration of all sectors of the organization. Intending, thereafter, optimize the allocation of resources and ensure the achievements of goals and objectives. The companies that stated that the business strategy comprises only one non-formalized idea which is shared by few individuals in key positions account for 17% of the sample, as shown in Figure 2. It was observed that these companies aim to simplify and process efficiency. Finally, it was verified that 3% of companies reported that their business strategies are in process of elaboration, that is, they are creating a focus on business decisions with emphasis on the importance of efficiency and effectiveness in their processes. The Figure 3 presents the results of technological strategy, that is, it is presented whether small and medium companies focused their efforts in the identification of the structural factors that affect the innovation performance. Analyzing Figure 3, it was noted that 52% of the studied companies reported that the technological strategy

comprise only one idea which not formalized and is share with few individuals in key positions. The interviewees argue that, in order to improve the technological strategy, it is necessary to create a technological intelligence, which would help in the process of identification and anticipation change, thus ensuring that the plans would not become quickly obsolete. It was also observed that there is no consensus on a precise definition of what constitutes a technological strategy or even on its extension. It was found that 39% of companies do not express an opinion about what technological strategy is. Due to the rapid technological change and the increasing concern about generating and managing these changes, aiming at generating competitive advantage, it was noted that 6% of the companies reported that their technological strategy is in process of elaboration. Finally, it was observed that 3% of companies reported having an informal technological strategy, that is, they have an explicit strategy, but it is restricted to some levels of management. It was perceived that the greatest difficulty in implementing the technological strategy is the doubt about the subject. Many entrepreneurs said that they do not possess knowledge about the topic. However, others interviewees raised the following issues, which form the basis of this strategy: how to choose the most appropriate technological alternative? What are the technological resources available? What will be the skills required in the future? With this analysis, we concluded that an integration between business strategy and technological strategy is necessary in order to establish a language which is common for both areas. FINAL CONSIDERATIONS

39 52

6 Forma l In process Informa l No opinion An idea

Industrialized countries have difficulty in maintaining its economic leadership in the process of permanent threat of global technological dynamism. It requires, by their companies, a continued investment in R&D aiming at innovations that allow maintaining competitiveness (Coutinho, 2004). The less industrialized countries experience a shortage of financial resources and macroeconomic instability that inhibits general investment, especially in technology.

Figure 3: Technological strategy.


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This study aimed to establish a concept of Technological Strategy, presented a proposal of assessment of the technological and strategic positioning of small and medium technology-based companies inserted in the aeronautical sector of Caapava, So Jos dos Campos and Taubat. In order to do that, a specific questionnaire on technological posture was employed, thus identifying the demands required to ensure the development of competitiveness of small and medium companies. The authors found that these companies do not have enterprise scale that allow incurring voluminous spending on R&D. Most of them position as proactive and reactive followers and work significantly in incremental and process R&D, thus acting not much with application R&D. The results indicate that small and medium technologybased companies of the aeronautical sector located in Caapava, So Jos dos Campos and Taubat did not have a formalized and disseminated technological strategy throughout their history. Therefore, it can be concluded that it is necessary that companies, especially small and medium-sized, adopt a technological innovation strategy integrated with the companys overall strategy, thus helping them keeping their competitiveness within their specificities not only in the national market but also internationally. REFERENCES Afuah, A. N.; Utterback, J. M., 1997, Responding to Structural Industry Changes: a technological evolution perspective, Industrial and Corporate Change, Vol. 6, No 1, p. 183-202. Amato Neto, J. Santos, I. C., 2005, Estratgias para Criao da Indstria Aeroespacial Brasileira, Revista Brasileira de Gesto e Desenvolvimento Regional, Vol. 1, No. 2, p. 16-40, mai./ago. Associao Catarinense de Empresas de Tecnologia (ACATE), 2008, Glossrio 2008, [cited Jun 29, 2008] Available at: < http://www.acate.com.br/index.asp?dep=39> Associao Nacional de Entidades Promotoras de Empreendimentos de Tecnologia Avanadas (ANPROTEC), 2002, Glossrio dinmico de termos na rea de Tecnpolis, Parques Tecnolgicos e Incubadoras de Empresas, Braslia, ANPROTEC. Banco Nacional de Desenvolvimento Econmico e Social (BNDES), 2007, Balano da PITCE em 2006, [cited 26 Nov, 2007] Available at: <http://www.desenvolvimento.gov. br/arquivo/ascom/imprensa/20070604balancopitce.pdf>

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o meio ambiente, In: VIII Simpsio de Engenharia de Produo (SIMPEP), Anais... Bauru, So Paulo, 12 a 14 de Novembro de 2001. Rieck, R. M.; Dickson, K. E., 1993, A Model of Technology Strategy, Technology Analysis & Strategic Management, Vol. 5, No 4, p. 397-412. Rodrigues, E., 2008, Planejamento Estratgico em Pequenas Empresas do Setor Aeroespacial de So Jos dos Campos SP, Taubat, Dissertao de Mestrado, Universidade de Taubat. Rosenbloom, R. S., Technological Innovation in Firms and Industries: assessment of the state of the art, In: Kelly, P.; Kranzberg, M., 1978, Technological Innovation: a critical review of current knowledge, San Francisco, San Francisco Press. Senz, T. W.; Garca Capote, E., 2002, Cincia, Inovao e Gesto Tecnolgica, Braslia, CNI/IEL/SENAI, ABIPTI. Servio Brasileiro de Apoio Micro e Pequenas Empreas (SEBRAE), Critrios de Classificao de Empresas Me EPP, [cited 10 Apr, 2008] Available at: <http://www.sebrae-sc.com.br/leis/defaulf. asp?vcdtexto=4154&%5E%5E> Schumpeter, J. A., 1982, Os Economistas: teoria do desenvolvimento econmico: uma investigao sobre lucros, capital, crdito, juro e o ciclo econmico, So Paulo, Abril Cultural. Silva, D. F., 2005, Crescimento e desequilbrio regional no Vale do Paraba: uma abordagem das disparidades econmicas e tecnolgicas, Taubat, Dissertao de Mestrado. Universidade de Taubat. Spiegel, M. R., 1993, Estatstica, 3. ed., So Paulo, Markron Books. Tidd, J.; Bessant, J.; Pavitt, K., 2001, Managing Innovation: integrating technological, market and organizational change, 2 ed., New York, Wiley. Tigre, P. B., 2006, Gesto da Inovao: a economia da tecnologia do Brasil, Rio de Janeiro, Elsevier, 2006. Trivios, A. N. S., 1987, Introduo pesquisa em cincias sociais: a pesquisa qualitativa em educao, So Paulo. Valerio Netto, A., 2006, Gesto de pequenas e mdias empresas de base tecnolgica, Barueri, SP, Minha Editora.

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doi:10.5028/jatm.2010.02027710

Depart. de Cincia e Tecnologia Aeroespacial So Jos dos Campos Brazil nestorbn@gmail.com

Nestor Brando Neto*

Depart. de Cincia e Tecnologia Aeroespacial So Jos dos Campos Brasil luheoliveira@gmail.com * autor para correspondncia

Lcia Helena de Oliveira

Proposta de um mtodo para uma atuao pr-ativa na gesto da inovao tecnolgica em uma instituio pblica de pesquisa aeroespacial
Resumo: O Departamento de Cincia e Tecnologia Aeroespacial (DCTA) tem funo relevante na satisfao das necessidades da Fora Area e no incremento da capacidade tecnolgica global do pas. Assumir um papel pr-ativo na gesto da inovao fundamental para o cumprimento dos objetivos estratgicos e deve ser encarado como uma condio necessria para a constituio de um ambiente propcio disseminao do conhecimento produzido s empresas do parque industrial brasileiro. Este trabalho fundamentou-se em duas abordagens: a de que a inovao tecnolgica um processo cumulativo o qual estabelecido por meio da interao entre o governo, empresas e instituies de P&D, alm do mercado e a abordagem technological foresight, no sentido de que a gesto estratgica da inovao tecnolgica implica negociar demandas e campos promissores de investigao e tambm em atuar nas condies do ambiente no qual esto inseridos os atores, promovendo uma macrocoordenao. Este artigo apresenta consideraes sobre a indstria aeroespacial brasileira e sobre o contexto da inovao tecnolgica no Ministrio da Defesa e no Comando da Aeronutica, especificamente no DCTA; o objetivo foi enfatizar a necessidade de uma atuao estratgica pr-ativa para a gerao de inovao tecnolgica e propor um mtodo de gesto dessa inovao para o DCTA. Palavras-chave: Gesto da inovao tecnolgica, Setor aeroespacial, Instituio Pblica de Pesquisa.

Proposal of a method to a pro-active action in the technological innovation management in an aerospace public research institution
Abstract: The Aerospace Science and Technology Department (DCTA, acronym in Portuguese) has a relevant role. of attending the air force necessities and of incrementing the Brazilians global technological capacity. Taking over to a proactive role in the innovation management is a fundamental step to achieve the strategic goals and it must be faced as a necessary condition for the formation of a favorable environment to disseminate knowledge to the Brazilian industrial sector. This work is based on two approaches: the technological innovation is a cumulative process which is established by means of the interaction among government, enterprises and R&D institutions, besides the market and the technological foresight approach, in which the strategic management of the technological innovation implies negotiating demands and promising investigation fields, besides influencing on conditions of the environment in which the actors are inserted, promoting a macro-coordination. This paper presents considerations about the Brazilian aerospace industry and about the technological innovation context at the Defense Ministry and at the Aeronautic Command, specifically at DCTA. The object was to emphasize the necessity of a pro-active strategic action in order to generate technological innovation, and to propose a method of management of this technology for DCTA Keywords: Technological innovation management, Aerospace cluster, Public research institution.
Received: 16/06/10 Accepted: 28/07/10
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INTRODUO Uma das premissas do desenvolvimento socioeconmico de uma nao refere-se consolidao de sistemas de inovao tecnolgica capazes de promover a interao entre o Estado, as universidades e centros de pesquisa e as indstrias. Essa uma mxima consagrada no mundo todo e diversas aes so tomadas no sentido de se criar e estruturar mecanismos de apoio ao desenvolvimento cientfico e tecnolgico. Outra mxima a de que, na sociedade do conhecimento, o diferencial competitivo balizado em funo da capacidade de aplicar os conhecimentos e gerar inovao. Em se tratando do Ministrio da Defesa e de seus comandos militares, a inovao tecnolgica tem adquirido relevncia. A orientao estratgica do Ministrio da Defesa, descrita em sua Poltica de Defesa Nacional, no sentido de que O fortalecimento da capacitao do Pas essencial e deve ser obtido com o envolvimento permanente dos setores governamental, industrial e acadmico, voltado produo cientfica e tecnolgica e para a inovao (Brasil, 2005, p. 16). A crena na importncia estratgica do desenvolvimento tecnolgico como fator de preservao da soberania nacional e de crescimento econmico e social tem levado a Aeronutica a adotar diretrizes que contribuam para o alcance da autonomia tecnolgica e para o desenvolvimento industrial brasileiro. O Departamento de Cincia e Tecnologia Aeroespacial (DCTA), rgo da Aeronutica responsvel pela Cincia, Tecnologia e Inovao (C,T&I), empenha-se em ampliar os conhecimentos cientficos e tecnolgicos do setor e em fomentar a capacidade produtiva da indstria aeroespacial brasileira interagindo com o ambiente produtivo. Mas como ampliar e promover essas interaes? Como criar um ambiente que favorea o comportamento empreendedor vinculando-o ao processo de inovao tecnolgica e crescimento organizacional? Como uma instituio pblica de pesquisa pode melhorar sua atuao em prol dessa interao? Essa temtica constante em estudos sobre gesto da inovao tecnolgica em academias, rgos representantes da classe empresarial e do governo, e deve ser considerada levando-se em conta as peculiaridades de cada setor econmico e foco de atuao institucional. Este artigo apresenta algumas consideraes sobre a indstria aeroespacial brasileira e o contexto da inovao tecnolgica no Ministrio da Defesa e Comando da Aeronutica, especificamente no DCTA. O objetivo foi enfatizar a necessidade de uma atuao estratgica prativa para a gerao de inovaes tecnolgicas e propor um mtodo de gesto dessa inovao para o DCTA.
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A INDSTRIA AEROESPACIAL BRASILEIRA A dependncia substantiva de conhecimentos e tecnologias direciona a indstria aeroespacial para a criao de um padro dinmico de atuao, no qual os esforos conjuntos do governo, dos rgos financiadores, das universidades e instituies pblicas de pesquisa e das empresas so essenciais para a base de sustentao do desenvolvimento social e da gerao de riquezas. Esse um aspecto crucial para a indstria aeroespacial, considerada aqui como um conjunto de sistemas complexos composto por trs segmentos inter-relacionados: o aeronutico, o de defesa e o espacial. um setor caracterizado pela exigncia de altos investimentos e por empregar mo de obra altamente qualificada. Requer longo ciclo de desenvolvimento e direcionamento governamental dos esforos de P&D. Nesses segmentos, a pesquisa e o desenvolvimento so fatores crticos e ocorrem principalmente no DCTA, que um importante fomentador brasileiro para essas atividades. No Brasil, a indstria aeroespacial atingiu a posio de destaque como a maior do hemisfrio sul, tendo como empresa lder a EMBRAER. Segundo dados da Associao das Indstrias Aeroespaciais do Brasil (AIAB, s/d), o desempenho econmico desse segmento industrial representou, nos anos de 2004 a 2007, cerca de 3% das exportaes da pauta brasileira. Outros indicadores sobre receitas, participao no PIB industrial, exportaes e empregos, alm da distribuio percentual por segmento so apresentados nas Tab. 1 e 2.
Tabela 1: Dados sobre o desempenho da indstria aeroespacial brasileira

Receitas (US$ bilhes) Participao no PIB industrial (%) Exportaes (US$ bilhes)

2004 2005 2006 2007 2008 4,2 4,3 4,3 6,2 7,55 1,9 3,5 1,5 3,7 1,5 3,9 1,9 5,6 2,02 6,74

Tabela 2: Distribuio percentual por segmento do desempenho da indstria aeroespacial brasileira

Distribuio percentual por segmento 2004 2005 2006 2007 Aeronutica 89,6 87,3 90,8 91,3 Defesa 9,23 9,29 5,78 6,6 Espacial 0,14 0,24 0,41 0,4 Exportao 82,72 90 90,5 90,8

2008 89,13 8,79 0,57 90,8

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Quando se observam os valores relativos exportao brasileira, verifica-se a importncia do setor aeroespacial para a balana comercial do pas. A EMBRAER a principal participante desse setor na balana comercial. Isso compreensvel pelo fato de a EMBRAER ser um dos principais fabricantes de aeronaves do mundo. De acordo com as pesquisas conduzidas pelo DIEESE/ CNM/CUT (2007), a EMBRAER articula um conjunto de micro, pequenas e mdias empresas (MPMEs) fornecedoras em torno de suas atividades econmicas, representando entre 70 e 80% das receitas dessas MPMEs. A INOVAO COMO FATOR COMPETITIVO Para uma nao manter-se em um nvel de competitividade que lhe proporcione um crescimento sustentvel, necessria uma infraestrutura econmica e social voltada acumulao de competncias tecnolgicas. O governo ator fundamental no Sistema Nacional de Inovao. Sua atuao estratgica, pois possui o papel de um rgo promotor do desenvolvimento socioeconmico do pas. Mas conforme descrito no Livro branco de cincia, tecnologia e inovao (Brasil, 2002b, p. 26): No basta, porm, promover o desenvolvimento cientfico. Deve-se reconhecer que limitada a capacidade, at agora demonstrada no pas, em transformar os avanos do conhecimento em inovaes traduzidas em efetivas conquistas econmicas e sociais (...) por intermdio de inovao que o conhecimento se socializa e se materializa em bens e servios para as pessoas. A inovao tecnolgica no pode ser relegada a um simples elemento de crescimento econmico do pas. Deve, ao contrrio, ser um instrumento primordial para a consolidao da funcionalidade do trinmio cincia, tecnologia e inovao. O modelo da Hlice Tripla III (Fig. 1), conceito definido por Etzkowitz e Leydesdorff (2000), que tem como

argumento bsico a articulao eficaz entre o governo, a indstria e as universidades (centros de pesquisa), aponta o caminho para a construo de uma interface slida entre os atores para que a inovao tecnolgica flua e produza benefcios sociedade por meio do aumento da competitividade das indstrias brasileiras. Nesse modelo, cabe ao governo a estruturao de mecanismos capazes de articular e estimular as parcerias por meio de polticas pblicas de desenvolvimento que promovam as atividades de cincia, tecnologia e inovao. s empresas cabe procurar criar valor econmico por meio da inovao. Essa deve ser parte integrante da cultura organizacional, sendo tratada como uma estratgia de negcio. Empresas que no inovam no sobrevivem no mercado atual. As empresas devem procurar oferecer inovao para diferenciar a sua marca de outras; do contrrio, o produto morre entre milhes de commodities. As universidades e instituies pblicas de pesquisa, como parte integrante desse sistema, devem utilizar-se da cincia para a pesquisa e desenvolvimento voltados gerao de produtos e servios que satisfaam aos anseios das empresas e da sociedade. A sobreposio das estruturas indica a necessidade da interao dinmica e atuao conjunta entre os atores, em que os processos inovativos so intensificados. Esses atores so elementos-chave para o gerenciamento da atividade inovativa e para a criao de ambientes favorveis inovao tecnolgica. Para Maciel (1997, p. 109), ambiente de inovao refere-se ao conjunto de fatores polticos, econmicos, sociais e culturais que estimulam ou dificultam a inovao. AS FORAS ARMADAS E A CINCIA, TECNOLOGIA E INOVAO A capacidade tecnolgica um fator fundamental na satisfao das necessidades reais das Foras Armadas para que tenham condies de cumprir da misso constitucional que lhes foi atribuda. O contedo tecnolgico dos produtos de defesa blicos, aeronaves, instrumentos de vigilncia, navios, carros de combate, entre outros tantos tem crescido de tal forma que se tornou praticamente impossvel a defesa do territrio nacional de forma autnoma e soberana sem essa capacidade tecnolgica. Tratando especificamente do setor aeroespacial, o Ministrio da Defesa, no documento Poltica da Aeronutica para o Desenvolvimento da Indstria Aeroespacial DCA - 14-3 (Brasil, 2002a, p. 8), cita que:
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Fonte: Adaptado de Etzkowitz e Leydesdorff (2000). Figura 1: Hlice tripla III.

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O conhecimento necessrio, mesmo o mnimo indispensvel para apenas manter as atuais aeronaves de combate e seus armamentos, j to elevado que, se o pas no possuir adequado suporte tecnolgico da sua prpria indstria, ele ser totalmente dependente dos pases fornecedores, e, assim, no ter capacidade autnoma sustentada de defesa. O desenvolvimento e a produo prpria de materiais para a defesa nacional o caminho para dominar esses conhecimentos. a busca, portanto, da auto-suficincia do parque industrial nacional. A DCA - 14-3 (Brasil, 2002a, p. 9) considera que o Parque Industrial Aeroespacial compreende: O conjunto das empresas, ou fraes de empresas nacionais, e de outras organizaes privadas ou governamentais civis ou militares que geram produtos ou servios....., especificamente destinados fabricao, ao emprego ou ao apoio direto de aeronaves ou de engenhos espaciais (...) So integrantes desse Parque Industrial Aeroespacial, os meios industriais e tecnolgicos da prpria Aeronutica...., das demais Foras Armadas e demais entidades, pblicas ou privadas, do Brasil. Dessa forma, a Defesa, especificamente a Aeronutica, considera imperativo diminuir a dependncia de fornecedores estrangeiros para suprir materiais aeronuticos, espaciais e blicos que contenham tecnologias sensveis suscetveis de embargos governamentais e de outras restries de cunho poltico-estratgico. Alm disso, o domnio do conhecimento cientfico e tecnolgico no desenvolvimento de produtos e servios para o setor aeroespacial possibilita ao Brasil inserir-se em um seleto mercado fornecedor de produtos e servios com alto valor agregado, gerando substanciais divisas para o governo e para as empresas nacionais na explorao aeroespacial. Para ilustrar a importncia destes aspectos, a FAB gastou na modernizao das aeronaves F5-E e F5-F, realizada pelas empresas EMBRAER e ELBIT (que israelense), o valor aproximado de US$ 400 milhes, conforme reportagem do jornalista Roberto Godoy (2010), publicado no jornal O Estado de S. Paulo, em 7 de junho de 2010. Essas aeronaves foram adquiridas na dcada de 1970 e, com essa modernizao, tem-se a expectativa de uso at 2021. A Pesquisa e o Desenvolvimento Aeroespacial esto, ento, incorporados em uma poltica estratgica nacional orientada tanto para a satisfao das reais necessidades da Fora Area Brasileira como para o incremento da capacidade tecnolgica global do pas.

A INOVAO TECNOLGICA NO DEPARTAMENTO DE CINCIA E TECNOLOGIA AEROESPACIAL O setor aeroespacial brasileiro tem demandado um sistema de inovao tecnolgica que atue como um pilar de sustentao para a ampliao de sua capacidade produtiva e competitiva. Nesse cenrio, o Departamento de Cincia e Tecnologia Aeroespacial (DCTA) tem um papel relevante por ser uma instituio-chave na pesquisa e desenvolvimento de solues cientfico-tecnolgicas, de inovaes para a satisfao das necessidades da Fora Area Brasileira e para incentivar o desenvolvimento econmico, promovendo e ampliando a capacitao da indstria nacional. Assumir um papel pr-ativo na gesto da poltica de inovao do DCTA fator fundamental para o cumprimento dos objetivos estratgicos e deve ser encarado como uma condio necessria para a constituio de um ambiente propcio disseminao do conhecimento. No se pode subestimar a complexidade desse papel. necessria a implantao de processos internos e externos ao setor responsvel no DCTA, com uma atuao gerencial estratgica para consolidar o preconizado nas polticas e diretrizes institucionais sobre gesto da inovao tecnolgica, assim como a coordenao entre o DCTA e suas organizaes militares subordinadas, alm da articulao com os atores governo e empresas. Como uma instituio privilegiada na gerao e difuso do conhecimento, o DCTA tem sob sua execuo um variado portflio de projetos e linhas de pesquisa com dualidade de aplicao civil-militar, caracterstica do setor aeroespacial. A possibilidade de surgimento de inovaes tecnolgicas a partir desse portflio de projetos e linhas de pesquisa considervel e deve ser fonte de anlise constante para apoiar a tomada de deciso quanto ao interesse do DCTA em dispor desse conhecimento, do modo considerado o mais conveniente para essa tecnologia, seja por meio de patenteamento, segredo industrial (know-how tcnico) ou at mesmo por meio da disponibilizao desse conhecimento para a sociedade. A condio da propriedade intelectual deve ser entendida nesse contexto no como o objetivo da instituio e sim como instrumento de valorao econmica da pesquisa para atrair o interesse do empresariado. Os institutos do DCTA, por meio de diversas aes, j realizam individualmente a aproximao com o ambiente empresarial e com as agncias de fomento com o interesse de transferir tecnologias e obter apoio no desenvolvimento dos

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projetos. Mas a coordenao institucional com o enfoque estratgico da gesto da inovao, interligando as aes com vistas ao fomento industrial fator primordial efetivao e consolidao da inovao tecnolgica nas indstrias. RECURSOS FINANCEIROS APLICADOS EM PROJETOS DE PESQUISA E DESENVOLVIMENTO NO DEPARTAMENTO DE CINCIA E TECNOLOGIA AEROESPACIAL Para que o DCTA desempenhe eficientemente a sua misso, necessrio um fluxo de recursos financeiros contnuos e elevados. A captao de recursos para projetos de P&D no DCTA provm do oramento pblico federal, por meio de rgos voltados ao fomento da cincia e tecnologia, de empresas conveniadas e de prestao de servios tcnicos especializados. Como alternativa escassez de recursos provenientes do oramento pblico federal, os pesquisadores do DCTA tm buscado recursos financeiros adicionais junto Financiadora de Estudos e Projetos (FINEP). Na execuo dos recursos financeiros, o DCTA utiliza o Grupamento de Infra-Estrutura e Apoio de So Jos dos Campos (GIA-SJ) e tambm a Fundao Casimiro Montenegro Filho (FCMF), Fundao de Cincia, Aplicaes e Tecnologias Espaciais (FUNCATE) e Fundao de Desenvolvimento da Pesquisa (FUNDEP), que fazem a execuo administrativo-financeira dos recursos provenientes da FINEP e das empresas. Essas fundaes procedem administrao dos recursos FINEP injetados no DCTA e financiam a pesquisa cientfica e tecnolgica realizada no Departamento. Os recursos oriundos das empresas pblicas e privadas conveniadas, na forma de capacitao e desenvolvimento tecnolgico, so executados pela FCMF. Esses recursos so investidos no DCTA a fim de buscar solues tecnolgicas para as dificuldades apresentadas pelas empresas, bem como realizar projetos de P&D tecnolgicos que se relacionam com a P&D de setores dessas empresas. Neste trabalho foi considerado o montante de recursos financeiros destinados s atividades de P&D no DCTA, oriundos do Governo Federal, originados do Comando da Aeronutica (COMAER), da Agncia Espacial Brasileira (AEB), da FINEP e do montante dos recursos injetados no Departamento sob forma de capacitao e desenvolvimento tecnolgico, por meio de empresas dos setores pblico e privado. O estudo abrange o perodo compreendido entre 2004 e 2009. Os valores do oramento pblico do COMAER e AEB foram extrados do sistema de gerenciamento financeiro interno do DCTA. Dados relativos FINEP foram obtidos

de relatrios fornecidos pela FCMF, FUNCATE e FUNDEP e so constantes da documentao do DCTA. Informaes das empresas, referentes capacitao e desenvolvimento tecnolgico so procedentes de relatrios da FCMF. A Fig. 2 mostra a relao do percentual entre os recursos oriundos do oramento pblico federal (COMAER e AEB), da FINEP e das empresas.

Fonte:

dados obtidos no Departamento de Cincia e Tecnologia Aeroespacial pelos autores com autorizao da instituio.

Figura 2: Relao do percentual entre os recursos oriundos do oramento pblico federal, da FINEP e empresas.

Verifica-se que, do total de recursos alocados na instituio em P&D, 71% foram originados do oramento pblico federal, 17% da FINEP e 12% foram oriundos de empresas. Considerando-se os recursos investidos pela FINEP e empresas em relao ao que o Governo Federal investiu na Instituio no perodo, observa-se isso implica em pouco mais de 1/3 do oramento pblico federal recebido um percentual de investimento expressivo. Importante ressaltar que dos valores investidos por meio dessas empresas, 84% pertencem ao setor privado e 16% ao setor pblico, e os recursos da FINEP abrangem todos os recursos financeiros entrantes no DCTA, executados pelas fundaes referenciadas, no perodo considerado. PROPOSTA DE UM MTODO PARA A GESTO DA INOVAO TECNOLGICA NO DEPARTAMENTO DE CINCIA E TECNOLOGIA AEROESPACIAL A dinmica da base conceitual proposta Considerando as diretrizes que norteiam a poltica de inovao do Ministrio da Defesa, do Comando da Aeronutica e do prprio DCTA, proposto um mtodo para uma atuao pr-ativa de gesto estratgica da
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inovao tecnolgica, contemplando os fatores internos e externos que condicionam a atuao do DCTA nessa importante atividade da Instituio. A dinmica da base conceitual proposta apresentada na Fig. 3. A base conceitual proposta compreende as condicionantes estruturais, as normativas, as do sistema produtivo e tambm as atividades consideradas de apoio inovao tecnolgica, que integram a efetiva gesto da mesma. As condicionantes estruturais referem-se s competncias de infraestrutura laboratorial, de pessoas e gerencial, alm do conjunto de projetos e linhas de pesquisa de interesse da Instituio. J as condicionantes normativas tratam da base legal sobre inovao tecnolgica, das polticas, diretrizes e planos do Ministrio da Defesa, do COMAER e do DCTA. As necessidades, interesses e capacidade da indstria aeroespacial brasileira so as condicionantes do sistema produtivo. Nessa base conceitual, a gesto da propriedade intelectual e o assessoramento ao processo de transferncia tecnolgica so consideradas atividades de apoio inovao tecnolgica.

Fundamenta-se na abordagem dada pela Organisation for Economic Co-operation and Development (OECD), denominada chain-linked (OECD, 1997) ou coupling model of innovation (Rothwell, 1994) (Fig. 4), visto que a inovao tecnolgica um processo cumulativo que se estabelece por meio da interao entre o governo, as empresas e as instituies de pesquisa e desenvolvimento, alm do mercado. Rothwell (1994) definiu esse modelo como sendo de terceira gerao. O de primeira gerao refere-se abordagem technology-push, baseada no modelo linear ofertista de inovao, no qual a oferta do processo de desenvolvimento tcnico-cientfico o mecanismo bsico que molda a direo do progresso tcnico. Nesse caso, a organizao empurra tecnologias no mercado sem identificar, primeiramente, o que o mercado necessita. O modelo de segunda gerao refere-se abordagem demand-pull (modelo linear reverso), na qual as necessidades do mercado direcionam as atividades de P&D que originaro resultados em vendas. No modelo chain-linked (OECD, 1997) ou coupling model of innovation (Rothwell, 1994), de terceira gerao, a pesquisa considerada como uma forma de solues de problemas e no apenas como fonte de ideias inventivas.

DCTA: Departamento de Cincia e Tecnologia Aeroespacial. Figura 3: Dinmica da base conceitual proposta.
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Proposta de um mtodo para uma atuao pr-ativa na gesto da inovao tecnolgica em uma instituio pblica de pesquisa aeroespacial

Fonte: Adaptado pelos autores de Rothwell (1994). Figura 4: Modelo coupling do processo de inovao.

um processo de articulao entre as necessidades da sociedade e do mercado com os avanos da cincia e tecnologia. Essa base fundamenta-se tambm na abordagem technological foresight, no sentido de que a gesto estratgica da inovao tecnolgica implica em negociar necessidades e reas propcias de pesquisa e tambm em atuar nas condies do ambiente no qual esto inseridos os atores, promovendo a articulao entre as partes. De acordo com Zackiewicz e Salles-Filho (2001, p. 144), a abordagem de technological foresight trata de buscar uma viso compartilhada de quais seriam as mais importantes demandas e campos promissores de pesquisa em um futuro prximo, de modo que se possa estabelecer prioridades. Em sntese: Foresight implica em negociar demandas e campos promissores de investigao, mas tambm em atuar nas condies do ambiente no qual esto inseridos os atores, promovendo uma macro coordenao. Conduzir um foresight , ao mesmo tempo, entender os processos competitivos e as trajetrias tecnolgicas subjacentes a eles e elaborar estratgias para concretizar inovaes e melhorar a capacitao dos atores para superar os desafios cientficos e tecnolgicos identificados. (Zackiewicz e Salles-Filho, 2001). O mtodo proposto para a gesto estratgica da inovao tecnolgica Perceber o contexto entendendo os processos competitivos do setor aeroespacial, os processos de gerenciamento de projetos da instituio e as diretrizes estratgicas para a inovao tecnolgica da Defesa, do COMAER e do DCTA fator primordial para a

implementao efetiva da gesto pr-ativa da inovao tecnolgica no Departamento. Sob a perspectiva do mtodo proposto, a ordenao de processos organizacionais tem condies de gerar roadmaps tecnolgicos alinhados s necessidades da instituio, possibilitando uma atuao organizada e com efeito impulsionador para o desenvolvimento e aplicao de tecnologias para o setor aeroespacial brasileiro. Um roadmapping de tecnologia um processo direcionado que auxilia na identificao e na seleo de tecnologias que satisfaam premissas definidas pela instituio (Garcia, 1997). uma ferramenta eficiente para a verificao de necessidades presentes e a previso das futuras, auxiliando a tomada de deciso no que diz respeito ao alinhamento das aes na instituio em busca da inovao tecnolgica. Consideraes relativas ao direcionamento de projetos de pesquisa, a utilizao futura de tecnologias ou a substituio das j existentes (bem como quando estas sero comercialmente relevantes), a capacidade industrial necessria para a produo em escala de determinada tecnologia e a necessidade de ampliar a capacitao em uma determinada rea do conhecimento a fim de atender s necessidades da Defesa e do COMAER so fundamentais conduo de aes para a aplicao das tecnologias no desenvolvimento do setor aeroespacial. No processo de roadmapping tecnolgico, algumas atividades so descritas considerando-se as condicionantes compreendidas na base conceitual proposta, tais como: condicionantes normativas ao DCTA: verificar as necessidades estratgicas da Defesa, do COMAER e do DCTA;

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verificar as diretrizes e a legislao sobre inovao tecnolgica brasileira; verificar as diretrizes e aes estratgicas do planejamento estratgico do DCTA, no que diz respeito inovao tecnolgica.

verificar a estratgia para a proteo intelectual das tecnologias em desenvolvimento; fazer estudo de viabilidade econmica do portflio de patentes do DCTA; verificar o interesse em negociar esse portflio (transferncia de tecnologia).

condicionantes do sistema produtivo brasileiro: realizar o mapeamento da capacidade instalada das indstrias do setor aeroespacial; verificar as demandas das empresas do setor aeroespacial brasileiro; verificar as demandas das empresas que desenvolvem projetos com o DCTA.

Essas atividades geraro informaes e conhecimentos a respeito do ambiente interno e externo, possibilitando ao setor responsvel o direcionamento de aes integradas aumentando a sinergia institucional e a sustentabilidade da gesto da inovao no DCTA. A complexidade inerente s atividades descritas evidente. Em funo disso, observa-se a necessidade de uma atuao em rede, bem como o delineamento do roadmapping tecnolgico com o enfoque estratgico necessrio. Um esquema genrico do processo de Roadmapping tecnolgico proposto apresentado pela Fig. 5. Nesse contexto, a proteo dos conhecimentos oriundos das pesquisas realizadas no DCTA, por meio de solicitao de propriedade intelectual, necessria e deve ser uma postura adotada por todos os pesquisadores e dirigentes

condicionantes estruturais internas ao DCTA: fazer prospeco tecnolgica para conhecer a trajetria das tecnologias do DCTA; realizar anlise dos objetivos e resultados dos projetos e das linhas de pesquisa do DCTA; fazer mapeamento das competncias infraestrutura e de pessoal do DCTA; de

DCTA: Departamento de Cincia e Tecnologia Aeroespacial. Figura 5: Esquema genrico do processo de roadmapping tecnolgico proposto.
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Proposta de um mtodo para uma atuao pr-ativa na gesto da inovao tecnolgica em uma instituio pblica de pesquisa aeroespacial

dessa instituio; porm, essa atividade isolada no tem efeito se no forem implantados processos capazes de transferir apropriadamente aos atores do sistema de inovao a utilizao das tecnologias desenvolvidas no mbito da Instituio. Desse modo, consideram-se a gesto da propriedade intelectual e o assessoramento ao processo de transferncia de tecnologias como atividades de apoio inovao tecnolgica. Trata-se de uma atividade-meio no gerenciamento dessa inovao. CONSIDERAES FINAIS Para fomentar e consolidar um setor exigente de conhecimentos e tecnologias como o aeroespacial caracterizado pela necessidade de altos investimentos por requerer um longo ciclo de desenvolvimento e direcionamento governamental dos esforos de P&D so necessrias aes polticas estruturantes e aes internas s instituies de modo a favorecer o comportamento empreendedor, associando-o ao processo de inovao tecnolgica e crescimento organizacional. Uma instituio pblica de pesquisa de excelncia como o DCTA requer atuao pr-ativa na gesto da inovao, de modo a ampliar os conhecimentos cientficos e tecnolgicos do setor e fomentar a capacidade produtiva da indstria aeroespacial brasileira. Tigre (2006, p. VII) cita que a gerao e apropriao de inovaes um processo complexo que depende no apenas das qualificaes e dos recursos tcnico-financeiros detidos pela firma, mas tambm do ambiente institucional no qual est inserida e do poder de negociao. A existncia de um ambiente com infraestrutura adequada e, principalmente, com orientao estratgica voltada inovao tecnolgica amplia a possibilidade de aplicao do conhecimento em tecnologias apropriadas utilizao pelo setor produtivo, com a consequente gerao de novos processos e disponibilizao de produtos e servios ao mercado. Utilizar-se de instrumentos gerenciais facilitadores ao entendimento do setor aeroespacial, buscando atuar nas condicionantes internas e externas que afetam o processo de inovao tecnolgica, possibilitar o estabelecimento de prioridades e alavancar a articulao dos envolvidos para superar os desafios tecnolgicos apresentados, alm de aumentar a aproximao das indstrias do setor aeroespacial ao DCTA. Auxiliar tambm o poder de negociao do DCTA em razo do maior entendimento das capacidades,

necessidades e interesses da indstria brasileira em relao P&D aeroespacial. Outro aspecto relevante que poder ser verificado o que se refere captao de recursos financeiros disponibilizados pelas agncias de fomento. O aporte de recursos que as agncias injetam na instituio expressivo, porm, observa-se que isso ocorre por iniciativa do pesquisador. Pela importncia que assumem esses recursos para a pesquisa e desenvolvimento no DCTA, a instituio identificando as competncias existentes, as demandas das empresas do setor aeroespacial e o portflio de projetos tecnolgicos ter acesso a fontes de informao para auxiliar a articulao junto s agncias na aprovao dos projetos, apoiando os pesquisadores, de modo que no caiba somente aos mesmos essa iniciativa. Esse fato, alm de colocar a instituio como corresponsvel por conseguir os recursos extras e necessrios aos projetos, faz tambm com que esses recursos sejam investidos em reas e linhas de pesquisa de interesse direto do COMAER. Alm desse aspecto, existe um fator estratgico que extrapola a execuo dos projetos. Trata-se da poltica das agncias de fomento quanto contrapartida da instituio para a gerao de produtos e servios inovativos que propiciem s indstrias brasileiras o aumento da inovao tecnolgica. A possibilidade de surgimento de inovaes tecnolgicas a partir do portflio de projetos e linhas de pesquisa do DCTA considervel e deve ser fonte de anlise constante para apoiar a tomada de deciso quanto ao interesse da instituio em dispor desse conhecimento do modo considerado o mais conveniente para essa tecnologia. Este trabalho apresentou uma proposta de um mtodo gerencial que ordene as atividades e possibilite a gerao de informaes e conhecimentos a respeito do ambiente interno e externo, o que permitir o direcionamento de aes integradas, aumentando a sinergia institucional e a sustentabilidade da gesto da inovao no DCTA. O mtodo proposto orienta o processo de gerenciamento da inovao tecnolgica, auxiliando o desenvolvimento de um ambiente favorvel ao comportamento empreendedor e a busca de solues para o desenvolvimento da capacidade produtiva. A abordagem technological foresight possibilita o entendimento dos processos competitivos envolvidos e as trajetrias tecnolgicas, com o objetivo de facilitar a elaborao de estratgias de inovao tecnolgica,
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Brando Neto, N.; Oliveira, L. H.

facilitar a negociao de demandas e campos promissores de investigao e tambm de atuar nas condies do ambiente no qual esto inseridos os atores, promovendo uma macrocoordenao. No houve a inteno de apresentar um roadmapping completo e tampouco indicar que a forma de organizlo aqui fosse nica; a inteno foi apresentar um mtodo fundamentado em instrumentos gerenciais amplamente utilizados em ambientes complexos, como o do DCTA, para facilitar o processo de tomada de deciso voltado inovao tecnolgica. No entanto, considerando a complexidade envolvida na gesto da inovao tecnolgica em uma instituio pblica de pesquisa com a peculiaridade do DCTA, o mtodo proposto representa uma forma de organizar atividades em prol da construo de instrumentos facilitadores que orientem as aes para a explorao econmica do conhecimento tecnolgico desenvolvido nessa instituio. Finalizando, os autores acreditam que a melhoria do desempenho organizacional deve ser constantemente buscada nas instituies, pois a essncia do gerenciamento, considerada, assim, elemento estratgico. Nesse sentido, fundamental a implementao de instrumentos gerenciais que auxiliem e promovam as competncias organizacionais. REFERNCIAS Associao das Indstrias Aeroespaciais do Brasil (AIAB), s/d., Nmeros da Associao das Indstrias Aeroespaciais do Brasil, Dados disponveis em: <http:// www.aiab.org.br/portugues/index.php?option=com_co ntent&task=view&id=17&Itemid=31>, Acesso em: 07 janeiro 2009. Valores de 2008 atualizados em 03 de maio de 2010. Brasil,2005, Poltica de Defesa Nacional, Ministrio da Defesa, Braslia, DF, Brasil. Brasil, 2002a, DCA 14-3 Poltica da Aeronutica para o desenvolvimento da indstria aeroespacial, Departamento de Pesquisas e Desenvolvimento, Braslia, DF, Brasil. Brasil, 2002b, Livro branco: cincia, tecnologia e inovao, Ministrio da Cincia e Tecnologia, Braslia, DF, Brasil. DIEESE/CNM/CUT, 2007, Projeto Laboratrio Sindical Industrial. Setor Aeroespacial nos pases do MERCOSUL, Disponvel em: <http://www.sindlab.org/

download_up/aeroespacialMercosul.pdf . Acesso em: 03 maio 2010. Etzkowitz, H., Leydesdorff, L., 2000, The dynamics of innovation: from national systems and mode 2 to a triple helix of university-industry-governnment relations. Research Policy, Vol. 29, No 2, pp.109-123. Fundao Casimiro Montenegro Filho (FCMF), 2010a, Capacitao tecnolgica, Disponvel em: <http://www. fcmf.org.br/sitenovo/cap_tecno.php>, Acesso em 10 de abril de 2010. Fundao Casimiro Montenegro Filho (FCMF), 2010b, Desenvolvimento tecnolgico, Disponvel em: http:// www.fcmf.org.br/sitenovo/desen_tecno.php, Acesso em 10 de abril de 2010. Garcia, M.L.; Bray, O.H., 1997, Fundamentals of technology roadmapping. Sandia National Laboratories, New Mexico, USA, Disponvel em: <http://citeseerx.ist. psu.edu/viewdoc/download?doi=10.1.1.31.1385&rep=re p1&type=pdf>. Acesso em: 20 Mar 2010. Godoy, R., 2010, Tigre renovado o principal caa da FAB, O Estado de S. Paulo, 7 de Junho Caderno Nacional, p. A8. Maciel, M.L., 1997, Inovao e Conhecimento, In: Sobral, F., Maciel, M.L., Trigueiro, M. (Orgs.), A alavanca de Arquimedes: cincia e tecnologia na virada do sculo, Paralelo 15, Braslia, DF, Brasil, p. 109. Organisation for Economic Co-operation and Development (OECD), 1997, Manual de Oslo. Traduzido em 2004 sob a responsabilidade da FINEP. Disponvel em: http:// www.finep.gov.br/imprensa/sala_imprensa/manual_de_ oslo.pdfhttp://www.finep.gov.br/imprensa/sala_imprensa/ manual_de_ oslo.pdf<http://www.finep.gov.br/imprensa/ sala_imprensa/manual_de_oslo.pdf>. Acesso em: 05 Abr 2010. Rothwell, R., 1994, Towards the fifth-generation innovation process. International Marketing Review, MCB University Press, Vol. 11, No 1, pp. 7-31. Tigre, P.B., 2006, Gesto da inovao: a economia da tecnologia no Brasil. Campus, Rio de Janeiro, Brasil, 282 p. Zackiewicz, M., Salles-Filho, S., 2001, Technological foresight: um instrumento para poltica cientfica e tecnolgica, Revista Parcerias Estratgicas, Ministrio da Cincia e Tecnologia, N 10, pp. 144-161.

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Thesis abstracts
This section presents the abstract of most recent Master or PhD thesis related to aerospace technology and management

Launch vehicle guidance algorithm insensitive to the dispersion of burnout time


Saulo Peixoto Campelo Technological Institute of Aeronautics spcampelo@hotmail.com Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisors: Prof. Dr. Waldemar de Castro Leite Filho and Prof. Dr. Luiz Carlos Sandoval Ges Keywords: Guidance, Solid Propulsion, Orbit injection. Abstract: This work describes a study of guidance of solid propelled space vehicles like the VLS the Brazilian satellite launcher. Such vehicles do not have control over the thrust level, then its trajectory must be controlled through the attitude angles. The VLS guidance is based on the instantaneous velocity and position, the remaining propulsive energy and the nominal trajectory required for the satellite orbit injection. However, the current guidance algorithm does not take into account the actual thrust profile, leading to uncertainty over several propulsive parameters, mainly in the burnout time of the engines. To provide better guidance performance, an algorithm insensible to the dispersion in the burnout time was developed. This is achieved through an additional guidance condition that leads the vehicle to perform a trajectory which is tangent to a surface solution defined by some orbital parameters at the injection time. Thus, the vehicle will reach the desired surface solution independently of the burnout time of the 3rd stage. Obviously, this new condition must not violate the injection condition, so the algorithm was built in accordance with both requirements.

Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisors: Dr. Alfredo Rocha de Faria and Dr. Algacyr Morgenstern Jnior Keywords: Numerical simulation, Computational fluid dynamics, Aerodynamics. Abstract: The characterization of aerodynamics of rockets is prerequisite for the design and operation of these vehicles. Knowledge of the aerodynamic forces acting determines the loading to which the structure is subjected and thus guides the structural design. Similarly, in order to determine its trajectory, it is necessary to know the aerodynamic characteristics in all phases of flight. One way to obtain the aerodynamic characteristics of a rocket is by means of numerical simulations of the flow over the rocket. In order to do that, the region around the rocket is discretized in a computational mesh that is then used for the numerical solution of the governing equations of the flow. The objective of this dissertation is to generate computational meshes in rockets and assess their suitability for the simulation of flow in different regimes of velocity. These simulations will be made using the program NS3D of the Aerodynamic subdivision of ASE, which numerically solves the 3-D Navier-Stokes equations of turbulent flows. These simulations will be validated by comparing the results computed with experimental data.

Analysis of fabrication and insulations of an S-30 motor case in composite


Rafael Fernando Heitkoetter Technological Institute of Aeronautics rafaelh@iae.cta.br

Numerical simulation of the flow field over sounding rockets


Frederico Rodrigues Ferreira de Farias Technological Institute of Aeronautics frfarias@ig.com.br

Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisor: Prof. Dr. Srgio Frascino Muller de Almeida and Dr. Lus Eduardo Vergueiro Loures da Costa
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Keywords: Motor case in composite, Rocket motor insulations, Filament winding, Computational simulation. Abstract: The rocket motor S-30 is used in the sounding vehicles VSB-30, VS-30 and Sonda III, of the Institute of Aeronautics and Space (IAE), such motor uses solid propellant and the motor case is manufactured in steel SAE 4140. The present work has the objective of analyzing the filament winding and the internal and external insulations of a composite motor case S-30 that can be used in the vehicles VSB-30 and VS-30 of IAE. The composite motor case aims at maintaining the interfaces with qualified parts of the vehicle, as tail can, igniter, nozzle and devices of propellant shipment with the objective of replacing the metallic motor case preserving the propulsive characteristics of the motor S-30. In this work, the geometry design and the thickness design of the domes and cylindrical part were performed. Also, the analysis of filament winding using the software CadWind and analysis of the internal and external insulations were performed. The analyses were performed for two configurations: the first for a motor case with same polar holes using an isotensoidal geodesic helical winding, and the second for a motor case with different polar holes, using a non-geodesic winding. The main conclusion based on analysis obtained from the two studied configurations indicates a composite motor S-30 with a better performance than a motor S-30 with metallic motor case, due to its smaller mass. This implies that a higher apogee may be reached for a same payload or a larger payload is possible for the same apogee.

manufacturing carbon/epoxy composites combined with the previous resin flow simulation into the preform by using the commercial software known as RTM-Worx. The use of this software aimed to help the complex task of determining the resin inlet and vacuum outlet predicting possible dry spots on composite part. The simulation of the resin flow through porous preforms was performed to obtain one plate and one C spar. In order to run the simulation, the viscosity resin and the permeability and fiber volume fraction of the carbon preform were previously determined by experimental trials. Using the resin flow simulation to obtain a C spar, three strategies for positioning the resin inlet and vacuum outlet on the mold were evaluated. Once the simulation had led to the best proposal of infusion, the C spar was manufactured. The experimental results showed that the unidirectional permeability was suitable for the application in this work, with a good linear fitting of points. The comparison between the experimental and simulated infusion times for the permeability plate (6%) and for the C spar (11%), even though some inputs of software were estimated, shows slight deviations and they are within an acceptable range according to the literature.

Development and characterization of radar absorbing materials based on polypyrrole/epoxy


Regiane Aparecida Medeiros de Campos Technological Institute of Aeronautics remedeiroscampos@gmail.com Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisor: Dr. Mirabel Cerqueira Rezende Keywords: Polypyrrole, (Chemical) Synthesis, Absorbing (Materials), Electromagnetic radiation, Epoxy resin, Engineering of materials. Abstract: This work shows the study performed in the dielectric radar absorbing material area based on the polypyrrole (PPy) conducting polymer use. Six different PPy samples were synthesized by chemical route using different combinations of two oxidants (FeCl3 e Fe2(SO4)3) and two anionic surfactants (sodium dodecylbenzenesulfonate DBSNa e 4-dodecylbenzenesulfonic acid DBSA). Blends of the synthesized polymers with epoxy resin were obtained. Infrared spectroscopy (FT-IR) analyses of the obtained conducting

Characterization and simulation of resin flow of VARTM process in the carbon/epoxy composites manufacture
Priscila Prado Gomes Technological Institute of Aeronautics ppgomescachu@gmail.com Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2010. Advisors: Dr. Mirabel Cerqueira Rezende and Orestes Antonio Guedes Ferro Keywords: VARTM, Unidirectional permeability, Resin flow simulation, Composite. Abstract: The present work comprises the VARTM (Vacuum Assisted Resin Transfer Molding) process for
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polymers confirm the success of the syntheses made. Electrical conductivity and scanning electron microscopy analyses show clearly the influence of the oxidant and surfactant used on the final characteristics of the obtained polymers. In this way, it is also observed that the sulfonate oxidant and the DBSNa surfactant favor the production of more conducting samples (13 S.cm-1) and the PPy/epoxy blends with the best behavior as radar absorbing materials (95% of attenuation, near 11 GHz).

DSC methodology developing for high heating rate experiments


Carlos Isidoro Braga Technological Institute of Aeronautics braga@srgrupo.com.br Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisors: Dr. Mirabel Cerqueira Rezende Keywords: DSC, High heating rates, Calibration, Thermal analysis, Polymer processing. Abstract: The present work aims to purpose a DSC (differential scanning calorimeter) thermal analysis methodology under high heating rates (>36o C.min-1). To reach such purpose, an instrument calibration method is established utilizing traceable metallic materials as indium, zinc, tin and lead, in order to evaluate the DSC furnace symmetry and linearity. Indium masses with different weights, from 0.570 to 20.9 in the milligrams range, are submitted to several heating rates (4 to 324 oC.min-1). Experimental results of melting temperature and enthalpy of fusion values are very close when compared with literature data. The polypropylene and polyamide 66 melting and crystallization thermal events are also studied using the conventional DSC method and the high heating rate method. The experimental results show that the indicated methodology is able to characterize traditional thermodynamic events as melting temperature, crystallinity and heat of fusion, based on the DSC instrument under high heating rate. In a short period of time, it is possible to characterize thermal events in a faster way, thus increasing the sensitive and resolution in just one shot and attending the ASTM specifications, with a great advantage of using actual DSC already available into the laboratories.

Synthesis of poly(o-methoxyaniline) in situ with carbon black and its use as radar absorbing materials
Simone de Souza Pinto Technological Institute of Aeronautics simonesouza.pn@gmail.com Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisor: Dr. Mirabel Cerqueira Rezende Keywords: Conducting polymers, Radar absorbing materials, Synthesis (Chemistry), Polymer matrix composites, Absorbers (materials), Material engineering. Abstract: The main objective of this study was to investigate and produce radar absorbing materials (RAM) using conductive composites. These composites were produced using carbon black (CB) impregnated in situ with poly(o-methoxyaniline) (POMA)polymerized by chemical route using o-anisidine in an acid solution. Fourier transforms infrared spectroscopy (FT-IR), Raman spectroscopy, and X-ray diffraction confirmed that POMA was successfully obtained in its conductive form. After determining the chemical route to POMA, the production of the conductive composites combining CB and POMA was studied. Scanning electron microscopy (SEM), FTIR and Raman spectroscopy confirmed that CB/POMA composites were also successfully prepared. The comparison of RAMs prepared using POMA with those using CB/POMA (both dispersed in epoxy resin) for electric conductivity and attenuation of electromagnetic radiation showed that CB/POMA/epoxy RAMs were better absorbers of electromagnetic radiation than POMA/ epoxy RAMs. The electric conductivity of CB/POMA/ epoxy composites was up to 100 times smaller than POMA/epoxy composites. RAM materials produced with CB/POMA/epoxy composites attenuated the energy of microwaves (8 to 12 GHz) up to 99.5%.

Study of convergence of parameters permittivity and permeability of RAM for X-Band and experimentally obtained from simulation
Adriano Luiz de Paula Technological Institute of Aeronautics alpaula@iae.cta.br

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Thesis abstracts

Thesis submitted for Masters in Space Engineering and Technologies at National Institute for Space Research, So Jos dos Campos, So Paulo State, Brazil, 2010. Advisor: Dr. Joaquim Jos Barroso de Castro Keywords: Scattering parameters, Nicolson-Ross-Weir method, Inverse problem, Electromagnetic simulation of rectangular guides, Electromagnetic absorber. Abstract: Widely used for retrieving complex permittivity and permeability from scattering S parameters over a broad frequency range, the transmission-reflection method diverges for low-loss electromagnetic materials at frequencies corresponding to integer multiples of one-half wavelength guided in the sample. In addition, S-parameter measurements produce multi-valued solutions for the complex wave number when the electrical length of the sample exceeds a wavelength. These effects lead to uncertainty in the phase of the reflection coefficient G, thereby producing undesirable ripples in the retrieved quantities. To resolve such drawbacks in the inverse problem, the present work proposes a non-iterative method based on the Nicolson-Ross-Weir (NRW) algorithm by properly accounting the algebraically unstable term (1+G)/(1-G). Using S parameters obtained from a 3-D electromagnetic field simulation of a waveguide setup, the method shows to be stable over the whole frequency range considered (8,20-12,40 GHz) with no divergence at halfwavelength resonant frequencies for either dielectric or magnetic materials. Consistent with results in the literature, effective complex magnetic permeability and dielectric permittivity spectra are given for slab samples of Teflon, nylon, epoxy, and carbonyl iron with arbitrary lengths.

Abstract: The attitude profile of the Brazilian Satellite Launcher - VLS is based on a nominal thrust used as reference during the execution of flight. Many propulsive and atmospheric dispersions can occur during the flight so that the launcher can deflect from the nominal trajectory. This work presents two approaches to compensate the propulsive dispersions of a satellite launcher through the attitude control system, increasing the nominal trajectory tracking along the flight. These methodologies are particularly useful for VLS, a four-stage solid propelled vehicle. Initially, an attitude correction through the apparent velocity feedback is proposed; it produces an attitude angle reference that is a function of the linear velocity. The other correction technique is based upon the creation of an off-line attitude table as a function of apparent velocity. Since the apparent velocity is related to the propulsive profile, a corrective action over this variable should perform a better treatment of the thrust dispersion. In both cases, specific software called ADAGA was used to produce several propulsive scenarios for the VLS flight. This software is also able to perform stochastic simulations through a Monte Carlo routine that produces dispersive profiles expected to occur in a real flight.

Real time energy estimation of the third stage of the Brazilian Satellite Launch Vehicle (VLS-1)
Erick Roberto dos Santos Netto Technological Institute of Aeronautics ersnetto@terra.com.br Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisor: Prof. Dr. Waldemar de Castro Leite Filho Keywords: Guidance, Solid propulsion, Energy estimation. Abstract: The control system design of a satellite launcher is done based on an algorithm that takes into account, among other parameters, the propulsion generated by the rocket motor and the mass consumption of propellant, given in the form of three curves, called the nominal, superior and inferior. These curves are used as limiters among which the actual curve of thrust and mass must remain. Currently, the algorithm uses a constant thrust profile and a mass profile that depends on the rate of mass consumption, though the algorithm using these data, they do not match the profile of thrust and mass real, because during the burning of the propellant, these data can vary

Correction of the launcher vehicle attitude profile as function of the apparent velocity
Srgio Mendes de Frana Technological Institute of Aeronautics sergio_mf11@hotmail.com Thesis submitted for Masters in Aerospace Engineering at Technological Institute of Aeronautics, ITA, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisors: Prof. Dr. Waldemar de Castro Leite Filho and Prof. Dr. Luiz Carlos Sandoval Ges Keywords: Apparent velocity, Attitude control, Guidance.

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considerably. The simulations of the algorithm takes into account the nominal profile of thrust and mass. The ideal case occurs when the actual profile is equal to nominal, but it is not due to variations occurring in the rocket engine. So it needs a good estimate for the profile of thrust and mass so that it closely matches the actual profile. This work presents an on-line estimation, during the vehicle flight, which estimates the values for the profile of thrust and mass closer to the actual values, thus obtaining an algorithm with results that are more consistent with reality.

Development and simulation of the embedded logic to the SARA recoverable orbital platform rendezvous and docking maneuvers
Jonas Gentina National Institute for Space Research jgentina@gmail.com Thesis submitted for Masters in Space Engineering and Technologies at National Institute for Space Research, So Jos dos Campos, So Paulo State, Brazil, 2010. Advisors: Prof. Dr. Ijar Milagre da Fonseca and Dr. Paulo Moraes Jr. Keywords: Attitude and Orbit Control Systems (AOCS), Embedded logic, Embedded software, Rendezvous and docking, Recoverable orbital platforms, Distributed simulation environments. Abstract: In this work, the possibilities of making computationally viable the space rendezvous and docking maneuvers implementation between the recoverable SARA satellite and another permanent orbital segment are analyzed. More specifically, the software needs and the flight algorithms that have to be developed to accomplish procedures like these were raised. Besides the reviews about procedures and technologies approaches involving this kind of maneuver, we developed a simulation of architecture made by a distributed virtual environment, which was capable to supply integrated simulation in near real time, together with another environment for controlling and monitoring which was implemented by interpreted language, in order to ease its using as a software tool for space engineers and space software engineers. Based on that virtual simulation environment, some algorithms that simulate the embedded logic in each vehicle acting on the scenario were also developed, as well as the remote operation and monitoring routines that reside on tracking ground stations. That communication methodology between two simulated environments can run a simulation scenario in a totally interactive and easy-understanding way to the user, because 3-D graphical outputs are generated showing all the simulation execution evolution. The results showed that the rendezvous and docking scenario development inside that kind of architecture turns the embedded software procedure analysis more precise and dynamic, without the need to develop simulators or virtual environments from scratch. All of those subjects were related to their respective applications within the SARA Project, addressing to the development principles of an embedded software prototype to be implemented onboard the mission vehicles computational subsystems that will accomplish the referred maneuvers.

Vision-based control of fixedwing Unmanned Aerial Vehicle for autonomous road-following


Joo Paulo de Souza Technological Institute of Aeronautics joaopaulojj@bol.com.br Thesis submitted for Masters in Electronics and Computer Engineering at Technological Institute of Aeronautics, So Jos dos Campos, So Paulo State, Brazil, 2009. Advisors: Dr. Elder Moreira Hemerly Keywords: Unmanned Air Vehicles, Tracking trajectory, Lateral visual guidance. Abstract: Navigation and control techniques using the GPS signals have problems in areas where obstacles can block the satellite signal. In some applications, an alternative is using navigation systems based on vision, for they do not emit signals, are passive and have low cost. This work aims to investigate the navigation of a fixed-wing unmanned aerial vehicle (UAV) for roadfollowing through computer vision and inertial sensors. Simulation of the computer vision algorithms were also used to generate the waypoints after the road search as well as to project them from the image reference frame to the world reference one. With this procedure, it is possible to implement lateral and altitude controllers. The performance evaluation was carried out with a realistic UAV model and virtual scenarios using the FlightGear Flight Simulator. Two approaches for lateral control were implemented. Their behaviors were similar and presented satisfactory tracking performance. The simulator provides visualization of the three-dimensional aircraft models, which is updated in accordance with the information of position and attitude received from the control algorithms implemented in MatLab.

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INSTRUCTIONS TO THE AUTHORS

Scope and editorial policy


The Journal of Aerospace Technology and Management is the official publication of Institute of Aeronautics and Space (IAE) of the Department of Aerospace Science and Technology (DCTA), So Jos dos Campos, So Paulo State, Brazil. The journal is published three times a year (April, August and December) and is devoted to research and management on different aspects of aerospace technologies. The authors are solely responsible for the contents of their contribution. It is assumed that they have the necessary authority for publication. When submitting the contribution the author should classify it according to the area selected from the topics: Acoustics Aerodynamics Aerospace Systems Applied Computation Automation Chemistry Defense Electronics Management Systems Materials Mechanical Engineering Meteorology Propulsion Structures Vibration

The journal uses the double blind peer review process for evaluation of the manuscript. The submissions, except thesis and book reviews, will be evaluated by three Editorial board members or ad hoc referees, and may be selected for publication according to the editorial policy of the journal.

Mandatory requirements
All papers must include: type of contribution (review article, original paper, short communication, case report, book reviews or theses), title, authors names, abstract and key words (three to six items that should be based on NASA Thesaurus volume 2 Access Vocabulary). All authors should be identified with full name, e-mail, institution to which they are related, city and country. One of them should be indicated as the author for correspondence.

Contents
Editorial Any researcher may write the editorial on the invitation of the Editor-in-Chief. The article should not exceed two pages. Review articles They should cover subjects falling within the scope of the journal. These contributions should be presented in the same format as a full paper, except that they should not be divided into sections such as introduction, methods, results and discussion. However, they must include a 150 to 200-word abstract, key words, concluding remarks, acknowledgment and references. The article should not exceed 20 pages. Technical papers These articles should report the results of original research and must include: a 150 to 200-word abstract, key words, introduction, methods, results and discussion, acknowledgment, references, tables and/or figures. The article should not exceed 16 pages. Communications These articles should report previous results of ongoing research. They should include a 150 to 200-word abstract, key words, tables and/or figures, acknowledgment and references. The communication should not exceed eight pages. Thesis abstracts The journal welcomes Masters and PhD thesis abstracts for publication.

Paper submission
Manuscript should be written in English or Portuguese and submitted electronically. The manuscripts written in Portuguese must present the title and the abstract translated into English, with the exact same content. If there is any conflict of interest with regard to the evaluation of the manuscript, the author must send a declaration indicating the reasons, for the review process occur fairly. See the instructions on www.jatm.com.br/papersubmission.
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After submitting the manuscript, the corresponding author will receive an e-mail with the Term of Copyright Transfer, in which the author agrees to transfer copyright to the Institute of Aeronautics and Space (IAE), in case of acceptance for publication, thus being forbidden any means of reproduction (printed or electronic) without previous authorization of the Editor-in-Chief. If the reproduction is allowed, it is mandatory to mention the Journal of Aerospace Technology and Management. The author also declares that the manuscript is an original paper and that its content is not being considered for publication in other periodicals and that all co-authors participated satisfactorily in the paper elaboration as to make public the responsibility for its content. The declaration must be printed, signed by the main author and sent back by mailing to the following address: Instituto de Aeronutica e Espao (IAE)/ATTN: Helena Prado/ Praa Mal. Eduardo Gomes, 50 Vila das Accias/ CEP 12228-901/So Jos dos Campos/ So Paulo/Brazil. References References should be cited in the text by giving the last name of the author(s) and the year of publication. Either use Recent work (Smith and Farias, 1997) or Recently Smith and Farias (1997). With four or more names, use the form Smith et al. (1997). If two or more references would have the same identification, distinguish them by appending a, b etc., to the year of publication. Acceptable references include journal articles, numbered papers, books and submitted articles, if the journal is identified. References from private communications, dissertations, thesis, published conference proceedings and preprints from conferences should be avoided. Self citation should be limited to a minimum. It is recommended that each reference contains the digital object identifier number (DOI). References retrieved from the internet should be cited by the last name of the author(s) and the year of publication, or n.d. if not available, followed by the date of access. Standards should be cited in text by the acronym of entity followed by their number, and doesnt need to appear in the reference list. References should be listed in alphabetical order, according to the last name of the first author, at the end of the article. Some sample references follow: Alves, M. B., Morais, A. M. F., 2009, The management of Knowledge and Technologies in a Space Program, Journal of Aerospace Technology and Management, Vol. 1, No 2, pp. 265-272. doi:10.5028/jatm.2009.0102265272 Bordalo, S. N., Ferziger, J. H. and Kline, S. J., 1989, The Development of Zonal Models for Turbulence, Proceedings of the 10th Brazilian Congress of Mechanical Engineering, Vol. 1, Rio de Janeiro, Brazil, pp.41-44. Coimbra, A. L., 1978, Lessons of Continuum Mechanics, Ed. Edgard Blcher, So Paulo, Brazil, 428p. Clark, J. A., 1986, Private Communication, University of Michigan, Ann Harbor. Silva, L. H. M., 1988, New Integral Formulation for Problems in Mechanics (In Portuguese), Ph.D. Thesis, Federal University of Santa Catarina, Florianpolis, S.C., Brazil, 223p. EMBRAPA, 1999, Poltics of R&D, Retrieved in May 8, 2010, from http://www.embrapa.br/publicacoes / institucionais/polPD.pdf,. Sparrow, E. M., 1980a, Forced Convection Heat Transfer in a Duct Having Spanwise-Periodic Rectangular Protuberances, Numerical Heat Transfer, Vol. 3, pp. 149-167. Sparrow, E. M., 1980b, Fluid-to-Fluid Conjugate Heat Transfer for a Vertical Pipe-Internal and External Natural Convection, ASME Journal of Heat Transfer, Vol.102, pp. 402-407. Illustrations All illustrations, line drawings, photographs and graphs should be referred as Figure and submitted with good definition (1 to 2 mega pixels). References should be made in the text to each illustration using the abbreviated form Fig., except in the beginning of the phrase. Explanations should be given in the figure legends, so that illustrations are kept clean Tables Authors should take notice of the limitations set by the size and layout of the journal. Therefore, large tables should be avoided. All tables must be numbered and mentioned in the text as Table. Equations Equations should be typed on individual lines, identified by numbers enclosed in parenthesis. References should be made in the text to each equation using the abbreviated form Eq., except in the beginning of the phrase, where the form Equation should be used. Acknowledgments The financial support received for the elaboration of the manuscript must be declared in this item.

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Research Briefs

THE BRAZILIAN SOUNDING ROCKET VSB-30


The Unified Microgravity Sounding Rocket Program for the Future, was established by a consortium of organizations (DLR-MORABA, Astrium GmbH, Swedish Space Corporation e Kayser-Threde GmbH) in order to perform microgravity experiments by means of sounding rockets. Among these experiments, is included in the program TEXUS, whose launch was carried out with the vehicle Skylark 7. In 2001, the German Space Agency (DLR) has consulted the Institute of Aeronautics and Space (IAE) on the possibility of developing a booster for employment in the European Microgravity Program, replacing the vehicle Skylark 7 that left to be produced This development coincided with the interests of Brazil, not only by the commercial aspect but also because of the possibility of employment in Microgravity Project of the Brazilian Space Agency (AEB), and the agreement between the Aerospace Technical Center (CTA) and DLR/MORABA became reality. On June 15, 2004, The Institute of Aeronautics and Space, iniciated the Certification Process by the Institute of Development and Industrial Coordination (IFI), and five years later, the certificate to the prototype of the VSB-30 was obtained. The contribution of certification on the reliability for a space rocket is hard to quantify. However, a significant reduction in failures has been observed in all projects that have adopted this procedure. In the case of VSB-30, all tests performed have achieved success.

CHARACTERISTICS
Length: 12.7 m Takeoff mass: 2598 kg Propellant mass: 1548 kg Burn time: First stage (booster): 12 s Second stage: 19.7 s Maximum speed: 2000 m / s Maximum acceleration: 12 g Payload mass: 400 kg Microgravity time 360

FLIGHTS:
VSB-30 V01 (QUALIFICAO) - Outubro/2004 CLA (Brasil); VSB-30 V02 (ESA - TEXUS EML 1) - Outubro / 2005 Esrange (Sucia); VSB-30 V03 (ESA - TEXUS 43 ) - Maro/ 2006 - Esrange (Sucia); VSB-30 V04 (AEB MICROG1) - Julho / 2007 CLA (Brasil); VSB-30 V05 e V06 (ESA - TEXUS 44 e 45) - Fevereiro / 2008 - Esrange (Sucia); VSB-30 V08 (ESA - MASER 11) - Maio / 2008 - Esrange (Sucia). VSB-30 V09 e V10 (ESA - TEXUS 46 e 47) - Novembro / 2009 - Esrange (Sucia)

NEXT:
VSB-30 V07 (AEB - MICROG1A) - Outubro / 2010 - CLA (Brasil) VSB-30 V12 e V13 (Australian-Brazilian-US-German HIFire Program) - Abril / 2011 - Woomera (Austrlia) VSB-30 V14 (ESA - TEXUS 48 e 50) - 2011 - Esrange (Sucia) VSB-30 V15 (ESA - MASER 12) - 2011 - Esrange (Sucia)

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PROJECT: 14-X HYPERSONIC VEHICLE


CHALLENGES The main technological challenges to the 14-X Project are: Supersonic Combustion; The Waverider concept; Thermal protection; 14X and launch Vehicle integration 14-X VEHICLE CARACTHERISTICS Length: 2000mm Wingspan: 800mm Weight: 350kg Speed: 3,5 km/s (Mach 10 @ 50km) Propulsion: Supersonic combustion RAMJET(SCRAMJET) Fuel: Hydrogen Gas Flight test duration: 4 s

THE SCRAMJET ENGINE The airbreathing propulsive system that provides the grater specific impulse thrust in hypersonic speeds is the SCRAMJET that uses hydrogen gas as fuel. The main difference between a SCRAMJET and a conventional jet engine is that the first doesnt have movable parts to compress the air, because it is done by reflected shock waves on its internal walls. Besides, in a SCRAMJET supersonic speeds are allowed inside its combustion chamber. With these features, this kind of engine provides conditions to fly at very high altitude and in hypersonic speeds using air from the atmosphere.

THE WAVERIDER CONCEPT A waverider vehicle could be defined as a supersonic or a hypersonic vehicle which uses the high pressure zone on its lower surface caused by leading-edge attached shock wave to generate lift. The interest in hypersonic waverider vehicles lies on the promise of an air breathing reusable vehicle able to deploy a payload into earth orbit. Until now, research has shown that a waverider vehicle has superior aerodynamic performance compared with other hypersonic aerodynamic concepts as accelerators and as aerogravity-assisted maneuvering vehicles. They are also being considered for high-speed long-range cruise vehicles since their high lift-to-drag ratio becomes important in achieving global range.

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RESEARCHES ON HYPERSONICS The 14-X Program has many bases of technology research. Among them are the supersonic combustion, aerothermodynamics, waverider concept and thermal protection. A powerful test facility for this research are the Shock tunnels, that can provide high Mach number and high temperature gas flow that simulates the real environment that the 14-X would face during its flight test. One example is the T3 Shock tunnel, 24 meters long, that can provide flows with speed from Mach 7 to 28.

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