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**Industrieanlagen-BetriebsgesellschaftmbH(IABG) High Temperature Technology and Advanced Materials D-85521 Ottobrunn, Germany
MANUFACTURING PROCESSES
The typical C/SiC manufacturing process used at IABG for rocket propulsion components is shown in Figure 3.
Both long and short fibre materials are included.
1 1 1
Figure 2: Cryogenic subscale test on test facility P59.1 at Dasa (MBB) in Ottobrunn, Germany
Pre-Grinding
PVD/CVD Oxidation/Erosion
Since then, new CMC materials and manufacturing processes have been developed by various institutions throughout Europe [1], and SEP has meanwhile demonstrated the feasibility of their material in hot fire tests with a full-scale radiation cooled HM7-engine nozzle extension,
Protection Coating (SiC, SiC>2\
1 |
and has developed the radiation cooled C/C-extensible nozzle for Pratt & Whitney's RL 10B-2 engine [2/3/4].
This paper describes the development and fabrication of new high quality/high performance rocket engine components like 400 N combustion chambers for small bipropellant engines and nozzle extensions for present and future engines made of C/SiC composites. Chapter 2 focuses on the C/SiC materials and capabilities at Dasa/IABG, and chapters 3 and 4 discusses present and future applications.
JOINING TECHNOLOGY
Depending on the requirements from different propulsion applications, different types of carbon fibre reinforcement (continuous and short fibre reinforcement) have to be considered. Propulsion units with continuous fibre reinforcement (2D-C/SiC) can be realized with woven C/C-prepregs or C-rovings in different winding techniques up to diameters of 2000 mm (see Figure 4).
The raw material used for the short carbon fibre reinforcement (isotropic C/SiC) is a porous C/C rigid felt, made of
short and isotropically (random) oriented carbon fibres, which are moulded with phenolic resins or pitch at high pressures to a kind of CFRP blank, which is available in various sizes. Dependent on the moulding process, the short carbon fibres are randomly orientated in the blank body and, hence, an isotropic mechanical behaviour is achieved [5/6/7].
C/C-felt
The typical CVD coating process needed to protect the C/SiC from the oxidizing atmosphere in a combustion device is shown in Figure 6.
During pyrolisation/carbonization heat treatment up to 1000C, the phenolic matrix reacts to carbon matrix (C/C). The density of these C/C compounds is between 0.7 and 1.5 g/cm . A graphitization process in inert atmospheres (by heat treatment at temperatures up to 2100C) and a CVI (Chemical Vapour Infillration)-process with pyrolitic
carbon reduces the chemical reactivity of the carbon fibres with liquid silicon. This process has a decisive influence on the physical and mechanical properties of the C/SiC composites. These C/C-raw materials are deliverable in blanks of diameters up to 2500 mm. However, the short fibre reinforced C/C felt is sufficient rigid to mill it to virtually any shape, as shown in Figure 5 with a rather sophisticated support rear structure all cut out of a single "base" by standard NC milling. The ribs shown here are not thicker than 1.25 mm with 0.1 mm tolerance. This is one of the most significant advantages of this material since it drastically reduces the forming costs [8/9/10].
quently the temperature is increased to 1800C and the silicon reacts with the carbon matrix and the surface of the
carbon fibres to form silicon carbide matrix (conversion process). Dependent on the amount of carbon and infiltrated silicon the resulting ceramic matrix composite consist of carbon fibres plus two matrix constituents (SiC and Si) in various concentrations. As mentioned before, the amount of carbon and silicon has to be apportioned exactly to prevent a chemical reaction with the silicon and the reinforcing carbon fibres. However, the fraction of metallic silicon contained in the blank after conversion amounts to 5 - 25% by weight. The density of the infiltrated C/SiC composite is typically between 2.1 g/cnr (2D-C/SJC) and 2.7 g/cnr (isotropic C/SiC). The use of vacuum conditions is not mandatory for all applications, yet was found mandatory for pore-free surfaces. The process will work at ambient pressure also with Argon. The duration of the thermal infiltration process is a direct measure of the extent to which the carbon matrix and carbon fibres react with Si to SiC, i.e. how much of the carbon fibre reinforcement will remain in the item. This parameter together with the temperature control to some extent the ratio of stiffness and strenght versus ductility of the C/SiC. After controlled cool-down of the item, it will be carefully examined again microscopically and by NOT methods (X-ray radiography) with respect to density variations, pores, microcracks etc. [11/12/13]. The main material properties of short (Iso) and continuous (2D) fibre C/SiC are summarized below in section 2.4.
Currently the C/C greenbody joining technology has been demonstrated on C/SiC burner components with a lenght of 3000 mm. No ageing and creeping effects (since 1 year at an application temperature of 1400C) were determined. Rapid manufacturing and breadboarding is achieved by
direct data link of the CATIA design stations for the NCprogramming for net-shape C/C-milling. Of all of the high performance, commercially feasible and advanced materials, only C/SiC offers the freedom to be moulded into
intricate "sculpture-like" shapes. It can be easily applied to very small and very large propulsion structures. The main
features and material properties of C/SiC manufactured by the above described processes are listed in the next section.
2.4 C/SIC MATERIAL PROPERTIES AND MAIN FEATURES
The C/SiC features and advantages can be summarized as follows:
Low specific density (2.10-2.70 g/cm )
All required facilities to perform the development and manufacturing work are available at IABG and Dasa in Ottobrunn. The various development and manufacturing
steps are accompanied by analytical work at the IABG laboratory, like SEM investigations of materials, mechanical tests including fracture toughness analysis and investigations of polished sections to estimate the received quality. The required equipment is available, including
SEM's, CTE-measurcment system, room and high temperature mechanical test devices and NdE (Non-destructive Evaluation) devices etc.. The manufacturing of C/SiC propulsion structures up to diameters of 1500 mm are state of the art. The fabrication of such propulsion structures can proceed immediatly without upgrading existing facilities. The facilities for propulsion unit manufacturing/processing up to > 2500 mm are also available (see Figure 7).
Low CTE (3.5-6.5 lO^K' 1 ) Good and tuneable thermal conductivity (5-135 W/mK)
Chemical and erosion resistant High temperature resitance (> 1700C) No detected ageing and creep deformation under stress
No open porosity Fast and low-cost near net shaping Short time manufacturing processing High flexibility in structural design, ultra-light
weight and up-scaling capability High and to some extent tunable stiffness (90-250 GPa) and strenght (140-350 MPa)
Note that for some parameters only the typical values are listed, e.g. the stiffness and strenght. The C/SiC structure in
this state has to be with suitable diamond tools to achieve the required surface quality [11/12/13].
Material Properties Haynes 25 Al Iso-C/SiC 2D-C/S1C AISI347 (short fibre) (cont. fibre)
Max. Operating
Temp. (C) Density (g/cm-'') Young's
IKK) 9,1
225
300
2,7 70 250 25 170
900
7,9 200 620 18 13
1600
2,7
Modulus (GPa)
Tensile Strenghl (MPa) Thermal Expansion (10- 6 /K) Thermal Condutivity (W/rnK)
980 13 10
3.
A typical field of application for CMC has been the area of solid-propulsion nozzles. IABG developed and produced CMC-components (nozzles, thruslers, etc.) for solid-propellant propulsion systems for tactical missiles funded by the German Ministry of Defence. C/SiC composite-based HT-structures offer numerous advantages, obviously led by high temperature resistance significant weight savings. Figure 8 shows C/SiC thrust nozzles for solid rocket propulsion.
In experiments the thermoshock, temperature and mechanical resistance of different nozzles (average chamber pressure to 80 bar) was demonstrated. The original matallic nozzles were exchanced by CMC-nozzles without any redisign in the nozzle mounting. Because nozzles or nozzle
throat inserts of CMC have the advanlge of a low abrasion,
The small bipropellant engines in operation tools use metallic combustion chambers, which are more or less refractory according to the type of cooling used. An engine using regenerative cooling may very well be made of stainless steel, but film or radiation cooled engines require higher performance materials. Beryllium may be used up to maximum temperlures up to 1100C. Another candidate, niobium, is limited by its susceptibility to oxidation, resulting in a demand for additional surface coating rather than by its melting temperature (2400C). Typical operating conditions are chamber pressures of 10 bar and combustion temperatures around 3000 K. The propellants are MMH and NTO. The chamber walls arc typically film- and radiation cooled; some systems requires in addition regeneratively cooled throut sections. Increased wall temperatures by reduced active cooling result in higher performance engines. While preparing a new generation of small high-performance bi-propcllanl engines, Dasa and IABG have investigated CMC's. The main advantage of these CMC composites is the increased maximum operating temperature up to 1700C with improved resistance to thermal cycles . Figure 9 shows a ION C/SiC bipropellant engine combustion chamber/nozzle, made with short carbon fibre reinforced silicon carbide. First laboratory hot tests with 10 N combustion chambers show no significant thermal ageing or erosion effects after 400 thermal cycles (cumulative operating time: 50 h, corresponding time 6 h, see Fig. 10) [6/7/8].
the loss of thrust by nozzle throat expanding during operation is less severe with C/SiC nozzles.
reinforcement
(experimental)
In a further step, Dasa and IABG will test in the near future different 400 N bipropellant engines on the satellite
propulsion test facility in Lampoldshausen, Germany.
These 400 N combustion chambers will be made of different C/SiC like short and continues fibres with different protection systems.
The 400 N bipropellant test engines made of C/SiC at IABG are shown in Figures 11 and 12. It is also foreseen to test chambers with continuous fibres, made at Dasa-Dornier/Friedrichshafen.
weight and cost savings in scene applications. The requirement for materials for liquid propellant engines are extremely high. Materials for an engine with storable propellants, are exposed to combustion temperatures about 3000 K at combustion pressures up to 50 bar (for the combustion chamber) and have to be chemically and erosion resistant. The nozzle extension of such a thrust chamber is typically exposed to temperatures of about 1300 K (metallic version).
To use CMCs like C/SiC for high pressure cryogenic engines the requirements concerning heat fluxes, thermalschock resistance, engine loads and thermo-mcheanical behaviour are even higher in comparison to storable engines (chamber pressures up to 200 bar, combustion gas temperatures around 3500 K).
As described in the introduction, the feasibility of a CMC nozzle extension has already been demonstrated, and a next potential application of C/SiC is seen as film/radiation cooled nozzle extension in storable propellant upper stage engines (low structural loads) [9/10]. One application of C/SiC in a flight engine is the thermal protection coating of the Vulcain engine igniter How path, see Figure 13. The figure shows cut of the igniter el vow after 16 ignitions. No delaminations or significant erosion of the C/SiC coating were detected.
Polenlial CMC-componenls in ramjels are hoi parls such as shock diffusor, subsonic diffusor, inlel cone combustion chamber insulation, flame holder and thrust nozzle. The material requirements of ihesc componcnls are Ihermalshock , temperature, mechanical and erosion resistance. The level of pressure and slresses depend on ihe operaling allitude of cruise missiles. Gas lemperatures with more than 2000C are possible in ramjels depending on Ihe lype of liquid and solid propellanl and ihe combuslion chamber pressure.
A C/SiC inlel ramp flap of a hypersonic Sa'nger Iransporlalion system was designed, buill, and Icsled in Ihe frame of
ihe German ramjet propulsion technology Sa'nger program. Figure 16 shows ihis inlel ramp Hap [14/15].
Figure 14: Igniter elbow with C/SiC thermal protection of the Vulcain engine after engine testing
A hot fire feasibility demonstration test of this flight qualified short fibre reinforced C/SiC coaling of the igniter elbow are shown in Figure 15 (hot fire feasibility demonstration test) [1 1/12/13]. This C/SiC hot gas pipe withstand in 30 tests gas temperatures up to 2000C combined with abrasive particles and thermalshocks of 2100K/sec without any ageing, abrasion effects or damages.
Before presenting ihe use of C/SiC for rockel propulsion applicalion in the next chapter, two oilier areospacc examples of successful! applicalion of C/SiC components will be
described.
field of ihrust vector control systems for jels and laclical missile propulsion, where tests of new concepts have been made possible by the use of C/SiC composites (thruslers, movable nozzles, valving of hoi gases, jcl blasts, etc.).
Figure 16 shows the 2D-C/SJC Ihrust deflector for the X-31
experimental aircraft which successfully demonstrated the use of this material under aclual flight condition.
The successful experimental verification of thcrmalshock and Icmpcralurc resistance of C/SiC Ihrustcrs give legilimalc hopes for short-lime applications of CMC lo olhcr
components of high velocity missiles. All exposed surface components of high velocity missiles are set out high temperatures and mechanical stresses by effects of aerodynamic heating and friction [16/17/18].
Figure 16: 2D-C/SiC thrust deflector for the X-31 aircraft 4.2 ULTRA-LIGHTWEIGHT C/SIC MIRRORS C/SiC with short fibre reinforcement has high application potential for optomechanical, especially ultra-leightweight applications (e.g. mirrors, antennas, optical benches, ^ telescope structures) with a mass of < 18 kg/m . C/SiC for mirror and telescope structure applications actually resulted from an extended trade of available materials in context of the FIRST reflector (diameter: 3500 mm) and of the MSG (Meteosat Second Generation Satellite) imager scan mirror which revealed that none of the "classical" materials would fulfill all given requirements, such as mass versus size, stiffness, CTE radiation resistance, thermal conductivity etc.. These mirrors will operate under extreme conditions: in geostationary orbit, exposed to hot and cold space, radiation, and worst: rotating with the satellite. One of the most advantageous features for experienced space-borne optomechanical instrument designers is the combination of high stiffness, low CTE and good thermal and electrical conductivity, particulary in contrast to Zerodur, Aluminium and Beryllium [19/20/21/22/23/24]. Figure 17 shows the ultralightweight C/SiC-Scan Mirror for MSG.
Different space propulsion and related components made of different CMC materials are being introduced into flight systems. Examples are solid propulsion nozzles, thrust deflectors, hot gas flow path components, thermal protection systems, and in-space high precision mirror supports. Nozzle extensions are on the verge of being used in large liquid propulsion upper stage engines. This paper described advanced C/SiC materials developed at IABG and Dasa in Ottobrunn, Germany. These materials and processes are available for future combustion chamber/nozzle assemblies for small bipropellant thrusters (Dasa 10 N and 400 N class) and for storable upper stage nozzle extensions (film/radiation cooled). Other potential future applications include the use of C/SiC as combustion chamber material for low pressure storable propellant engines with regenerative cooling.
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