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INTRODUCTION
decade
advances have been made in the developon organic polymer matrix systems reinforced with high performance fibers as metal replacements in aerospace, automotive, recreational and industrial applications. As a result of continuous improvements in fiber/matrix properties and development of innovative fabrication
technologies, advanced composite structures offer possibilities for major leaps in
design, manufacturing, energy conservation, product utility and diversity [1].
In the course of organic polymer matrix development the thermoset systems
such as 350F cured epoxies reinforced with high strength boron or graphite
fibers were initially evaluated for primary structure of subsonic military aircraft.
Although the thermoset systems showed superior tensile, shear and compressive
strengths, several deficiencies were uncovered with the epoxy-based composites,
major
URINGof advanced composites
ment
based
THE PAST
Journal
J1J1.
1-,Iuly 1988
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277
278
manufacture
cost
phous polyamide) and PEKK (a semi-crystalline polyether-ketone-ketone) covering a wide range of end-use temperature applications have been demonstrated for
advanced composites with superior performance in mechanical properties, fracture toughness and damage tolerance [2-4]. Several additional thermoplastic
matrix systems with high T. have been developed by other material suppliers
[5-9]. Innovative processing methods have been developed to produce a variety
of thermoplastic prepregs and preforms. This paper will review the recent
development in thermoplastic material systems and processing/fabrication
methods including the development work performed at DuPont.
THERMOPLASTIC MATERIAL SYSTEMS DEVELOPMENT
Attributes of
J-polymer, K-polymer,
etc.
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Table 1.
279
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280
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281
Other
high performance
matrix systems
including polyimide
LARC-TPI
(Mitsui Toatsu) and polyamideimide &dquo;Torlon&dquo;-C (Amoco) [12] with dry Tgs of
264C and 288C, respectively, also show excellent mechanical properties and
melt viscosity requiring high processing temperature. Due to presence of
amide groups in the polymer chains, &dquo;Torlon&dquo;-C is more sensitive to moisture
than the polyimide or polyetherketone systems previously discussed. Recently,
a new derivative of polyamideimide with less moisture sensitivity such as
AMCOs AI-696 was reported with a dry T, of 243 C and equilibrium water
sorption at 1.8% by weight of polymer. However, the flexural modulus (2.83
GPa) and the tensile strength (90 MPa) of this resin are lower than those of
&dquo;Torlon&dquo;-C PAI neat resin [8,12].
The neat resin properties of various thermoplastic matrix systems mostly
obtained from sources cited in the reference list are given in Tables 2 and 3. The
performance comparison of matrix systems is given in Table 4.
high
bMelt temperature
Nominal processmg temperature
dX-ray diffraction
eAt processing temperature, 10 sec shear rate
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resins.
atensile
or
flexural modulus
bTensile strength
ctensile elongation
thermoset
Table 4. Performance
+ +
+
-
Excellent
Fair.
Poor.
282
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resins.
283
Table 5. Mechanical
cFlexural/compression strengths
from References
[6]
and
or
equivalent)
[7]
Avimid* K
or
N-polymer
matrix were processed using vacuum bag layup and autoclave technology [2,10].
The carbon fiber reinforced composites with other matrix systems were prepared
and tested by manufacturers of these polymer resins. Several matrix-dominated
mechanical properties of the thermoplastic composite laminates at room temperature (mostly obtained from various sources cited in the reference list) are given
or
in Table 5.
The most
*DuPont
Registered Trademark.
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284
Thermoplastic Composites
thermoplastic resins including J-polymer, nylon 66,
PET reinforced
bFiber
zero
twist yarn
mth
polyurethane size for J-polymer and PEKK, fiber mth epoxy size for &dquo;Epon&dquo; 828.
%hree point bendmg mth span-depth ratio 32 for flex modulus, 16 for flex strength, 4 0 for short beam
shear strength.
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285
with Kevlarg aramid fibers were evaluated with the composites prepared from
the proprietary melt impregnated tows developed at DuPont [3,13]. The melt
impregnated tow as a precursor can be woven into a variety of fabric constructions for consolidation into porosity-free final components or for subsequent
thermoforming operation. Due to inherent fiber/matrix compatibility, attractive
mechanical properties of Kevlar®/J-polymer composites were obtained for the
unidirectional or fabric composite laminates [13]. Recently, preliminary tests
also showed good consolidation for the composite laminates prepared from the
melt impregnated tows of Kevlarg aramid with PEKK matrix. The matrixdominated mechanical properties such as flex and short beam shear strengths of
Kevlar21/J-polymer and Kevlar®/PEKK are given in Table 6. The mechanical
properties of a conventional epoxy system (&dquo;Epon&dquo; 828) reinforced with Kevlar
fiber are also given for comparison.
E-Glass Fiber Reinforced
Thermoplastic Composites
Thermoplastic
The shift from using thermosets to using thermoplastics requires a shift in our
thinking regarding the processes required to make parts. In thermoset technology the key to success is control of the crosslinking reaction which directly
affects the properties in the composites. Hence, we must deal with this issue
throughout the process stream from making prepregs to storage and shipping of
prepregs, during the layup process and finally during the autoclave process. Our
investment plan and process considerations are all affected by this chemical reac-
tion.
In thermoplastics, the
emphasis
shifts from
controlling
the
chemistry
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to con-
286
the rheology. Thermoplastics at their processing temperature have viscosities of 500-5,000 pa.s compared to thermosets which are less than 100 pa.s.
Hence the critical process elements must deal with the effects of this high viscosity. In the impregnation step viscosity affects both fiber/resin uniformity as
well as fiber wet-out which is critical for good load transfer in the final part. In
processing the final part, viscosity affects consolidation rate, fiber wash or
movement of the fibers in the part and cycle time.
The most critical phase in processing of thermoplastics is the impregnation
step. Here the fiber and resin are brought into intimate contact and the
fiber/matrix distribution is essentially set. For most thermoplastic systems this is
accomplished first before proceeding to make a part.
Several methods are used for bringing the fiber and matrix together: melt impregnation, commingling of matrix fibers and reinforcing fibers, powder impregnation and solvent impregnation. Each of these has their strengths and
weaknesses. In all cases the one-dimensional penetration of a thermoplastic melt
into a uniaxial fiber bundle may be modeled by Equation (1) derived from
Darcys law of flow through porous media [14]. By integrating the Darcy equation (over the media thickness with the time), the following relation for the onedimensional penetration is obtained:
trolling
where
x
k
P
tt
penetration depth
media permeability
coeflicient
pressure
time under pressure
media viscosity
Equation (1) shows that the penetration depth is proportional to the media
permeability, the applied pressure and inversely proportional to the viscosity.
Since the viscosity of the resin system is given and is little affected by process
conditions, then all we can hope to change is the permeability through the
porosity of the fiber bundle and the applied pressure. Hence, the most favorable
conditions for good flow required for uniformity occur at high porosity and high
applied pressure.
Thus, attempts made to simultaneously complete the impregnation process and
part forming would lead to poorer than desired fiber-resin distribution; therefore, it is important to establish the distribution early. In each of the non-solvent,
non-melt cases this is done by matching the matrix resin size to that of the reinforcing fiber to obtain a good distribution in the dry state. In the case of melt
processing this is accomplished by simultaneously controlling the resin feed
pressure and the density of the yarn bundle. When solvent is used, one can in
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287
effect reduce the viscosity to achieve the desired distribution. However, the
presence of the solvent, particularly polar solvents, can modify the fiber surface
resulting in an undesirable shift and ultimately in reduction of the fiber/matrix
shear strength.
The other variable that affects impregnation quality is the ability of the resin
to wet the fiber. This wetting is necessary for fiber-matrix adhesion needed to
achieve the desired level of stress transfer for dynamic, mechanical performance. This problem is particularly critical in the case of carbon fibers where
the carbon fiber cross section is not round but serrated. Inadequate wetting of the
fiber by the matrix resin can increase void concentration at the interface and
result in poor composite properties.
Fiber wetting is effected by the resin viscosity, surface tension and the character of the fiber surface. One can alter the resin surface tension either through
the addition of solvents or through a change in the polarity of the fiber surface
by plasma etching, chemical treatment, ozone treatment or with oxidative attack
at the fiber surface. Considerable work is being done to study the effects of these
treatments on all the major fibers using both micro techniques, such as the
Whilemy balance to study surface tension force between the resin and fiber as
well as macro studies using chemical treatment such as DuPonts high temperature polyimide sizing for carbon fiber or the amino silanes frequently used with
glass fiber. A variety of characterization methods such as surface spectroscopy,
thermal desorption, surface free energy, interfacial shear strength, photoelectric
observation, etc. to study the chemical and physical nature of the fiber-matrix interface as affected by the surface treatment were reviewed by Drzal [ 15] . This
science is still in its early stages and will continue to be a fruitful area for investigation, particularly in the area of the fiber-reinforced thermoplastic matrix
composites.
Proceeding forward in the process area we can use either a fully consolidated
prepreg (one in which all the air has been removed) or an unconsolidated form
that contains greater flexibility. Materials of both types can be made using any
of the four prepreg methods described earlier. At this stage in the process we
must focus on resin flow to provide a good interlaminate structure or to allow the
laminate to be reformed. The work of Cogswell and Leach [16] deals with the
various flow processes that occur in a direct forming process in which a flat sheet
is transformed to a complex shape. Here they define three types of shear, transverse intraply, axial intraply and interply, that take place, allowing resin flow to
occur during the shaping. This is necessary since the fibers are essentially noncompliant in this regime. This approach represents a good model for forming by
any number of processes such as match-die molding, press forming, bladder
molding or super plastic forming. The processes for thermoplastic composites
forming are described in various publications [17-23].
Thermoformable Sheets
An alternate method for handling the manufacture of formed complex shapes
is to use a thermoformable sheet with oriented discontinuous fiber structure as
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288
DuPont [24,25]. The sheet is designed such that the filament reinforcement (3-15 cm length) is aligned in each layer to such a degree that continuous fiber-like properties result. The discontinuous fiber reinforcement, however, does permit drawing required to form complex shapes. In this case the
matrix shearing differs from the earlier case because the movement of the fibers
allows axial draw to occur in the fiber structure as well as the resin. Performance
of these parts relative to parts made from continuous fibers is heavily dependent
on the quality of the fiber orientation, rather than the use of discontinuous fiber.
This is verified theoretically using shear lag theory where the length-to-diameter
ratio of the fiber (AS-4 carbon) is greater than 1000 with &dquo;critical&dquo; fiber length
L~ well below 0.1mm. In addition, experimental work in this area, although
limited, confirms this expectation as shown by comparison of mechanical properties between the composites from continuous filament and discontinuous formable sheets in Table 7.
developed at
Filament
Winding
Other methods for making parts involve processes, such as filament winding
and 3D braiding. In filament winding, as in tape lay down, we can begin with a
fully or partially impregnated prepreg. If post processing is to be used it is possible to use a partially impregnated prepreg and complete the impregnation process at the same time as one does the consolidation. In this case the rate limiting
step will be the impregnation step and will depend on the quality of fiber-resin
distribution and the wet-out required to meet the structural requirements. If the
prepreg is fully impregnated it is possible to reduce the post processing to
minutes. Here the rate limiting step is the time required to heat the part up to the
flow temperature of the resin.
For the most effective and low cost process it is desirable to directly consolidate the prepreg during the winding step such as in-situ consolidation being
Table 7.
Comparison
Quasi-isotropic layup
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vs.
289
In this particular case the time for heat up and consolidation is in the order of seconds. This can only be accomplished with fully
impregnated feed material. However, full consolidation of the feed is not required but may eventually limit the winding speed. To date little has been published on the subject but it appears the fiber winding at economically attractive
rates is possible. Tubes with both thin (less than 0.25 mm) and thick (approx. 5
cm) sections have been made with acceptable translation of properties.
3D
Braiding
Finally in 3D structures the primary focus has been on the formation of the
structure with high fracture toughness. While this focus is possible for use in
thermosets which have low viscosity and can penetrate the 3D network when it
is opened up, it requires additional technology for use with thermoplastics.
Work has been done at DuPont and by a number of speciality companies to both
braid and weave pre-impregnated yarns in order to make thermoplastic 3D structures. Again the degree of impregnation plays an important role in deciding on
the process techniques required to fully consolidate the structure. For in-line
consolidation a fully impregnated yarn is required. For off-line post consolidation, the cycle times will again be controlled by the impregnation flow equation.
A new process with &dquo;in-line&dquo; consolidation was developed at DuPont for forming 3D braids with thermoplastic melt impregnated tows that can form a wide
range of structure shapes [27]. A rectangular slab with 50 % fiber volume was
demonstrated, using axial AS-4 carbon tows which was melt impregnated with
a thermoplastic matrix (J-polymer) and braiding Kevlarg aramid tows melt impregnated with the same matrix. The ratio of AS-4 to Kevlarg aramid was 6 to
1. The consolidated structure showed good flex/shear properties with high interlaminar fracture toughness.
Impregnation
Because of the importance of the impregnation step to both the economics and
part quality, it is worth looking into this process step in more detail. As noted
earlier there
melt im-
SOLVENT IMPREGNATION
This process is employed by several firms such as American Cyanamid and
Ten Cate in Europe. In both of these cases the matrix resin is a polyetherimide
(PEI). The benefit of this process is derived from the low viscosity of the resulting resin solution which allows both unidirectional tapes and woven fabrics to be
used as feed material. However, there are two big drawbacks: the potential for
residual solvent in the prepreg, and inability to use higher performance resins
that have excellent solvent resistance. In the case of PEI the solvent used is NMP
(N-methyl pyrrolidone). For other resins like polyamides solvents as aggressive
as formic acid would have to be used and for polyetherketone like ICIs PEEK
or DuPonts PEKK, there are no good solvent systems. In addition to en-
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290
vironmental restrictions, investment would be required to
As a result this approach is in limited use today.
recover
the solvent.
MELT IMPREGNATION
The second approach &dquo;melt
approaches.
COMMINGLING PROCESS
This is a relatively easy process to use. Any thermoplastic resin can be made
to work if it can be made into a fiber. Here the trick is to insure that the fiber diameter of the matrix fiber is matched to that of the reinforcing fiber in order to
assure good distribution of the two fibers. It also requires a texturing process to
open the yam bundle without damaging the brittle fiber. This is particularly
difficult to accomplish for a high filament count carbon tow such as 6K or 12K
AS-4 or IM-6. In addition, there is an added cost to make the fiber form of the
matrix. Resins like polyester that are inexpensive in fiber form dont suffer this
added cost, but conversion of resins like PEEK into fiber in small lots will increase the resin cost by 2X. This concept has been practiced by BASF in its joint
development with Concordia. Recently, the advances in commingled yarn technology with a wide range of polymer matrices and reinforcement fiber types
were
reported [28].
The commingled product cannot be used effectively in high speed process like
filament winding because of the lack of bundle integrity. It was observed during
filament winding of a 3K AS-4/PEEK commingled tow in our laboratory that the
PEEK filaments in the tow were separating from the carbon filaments as tension
was applied for &dquo;in-situ&dquo; consolidation. The resulting tube showed a low torque
strength of 390 Nm with a high level of voids after post consolidation via
autoclave. In contrast, a melt impregnated AS-4/PEEK tow with good bundle
integrity was successfully processed with &dquo;in-situ&dquo; consolidation. The resulting
tube showed a high torque strength of 650 Nm.
On the positive side the commingled yarn flexibility which is derived from the
lack of connectivity since no fusion of the matrix has occurred makes this form
much easier to braid and weave, hence reducing costs in this step. Some of this
I
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291
is then lost due to the longer cycle times required to consolidate the part.
laboratory tests showed that it took twice as long to consolidate the commingled tows into a plaque as it did for the melt impregnated tows under similar
molding conditions.
gain
Our
POWDER IMPREGNATION
This process generally produces a flexible tape or tow in which the matrix
resin is held in place but stays in a powder form in the same way as the resin
stays as a separate entity in the commingling process. There are two published
methods for powder prepregs. The Atochem process encapsulates the thermoplastic resin powder in the yarn with a sheath of either the same resin or a lower
melting point resin [29]. This product can be readily woven and used in fabric
form. The disadvantage of this method is that the composite laminate produced
from the encapsulated tows may contain excessive resin-rich areas due to
presence of the sheath layer around the tows. It would be difficult to achieve a
good fiber-matrix distribution, particularly when a high fiber volume is required. The resin-rich areas are increased when a high melting-point resin
sheath is used for encapsulation.
A second approach is that employed by BASF wherein the powder is put in an
aqueous suspension that is then used to impregnate the fibers. This yields a tacky
product similar to a thermoset prepreg. When a woven fabric is to be used it is
possible to make the fabric then impregnate it because of the low shear viscosity
of the slurry. The water is then driven off during the forming process. Again the
process requires a step to obtain the particle size necessary to match the fiber
dimensions. This can result in a 50% increase in the cost of the matrix resin
except in cases such as nylon 11or PEEK where the matrix is produced as a
powder.
The
ity
most important advantage of powder impregnation technology is its abilto process matrix systems with very high melt viscosity and high melt tem-
perature. BASF claims that they made consolidated laminates via powder im-
pregnation with PMR-15 and PEEK of high viscosity grades [30]. This
technology has attracted a lot of attention because most high performance ther-
moplastic matrix systems have high melt temperature with high melt viscosity.
It is difficult to process these matrix systems through the melt impregnation.
Table 8. Relative cost of prepregging for thermoset
thermoplastic tows.
versus
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292
However, there are two major concerns for the powder impregnated prepregs
currently being evaluated in the trade. First, the unidirectional carbon prepreg
lacks sufficient transverse strength. Thus, it requires extraordinary care and effort to handle the prepreg during layup to form a complex-shaped part. The
other is the use of a relatively large amount of polymeric binding agent as high
as 6 % of a polyacrylic acid by weight of matrix resin as described in a patent reference [31]. This crosslinkable binding agent may remain in the prepreg during
high temperature processing and cause undesirable effect on the matrix resin and
its composite properties. Further effort would be expected from the manufacturer to resolve these concerns.
RELATIVE COST OF PROCESSES
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293
Table 9. Effect
on
winding.
zontal and vertical stabilizers with the carbon fiber thermoplastic composites
[32]. After successful testing and demonstration, it is expected that engineers
and designers at Westland and other aerospace companies will move toward
using the thermoplastic composites in helicopter fuselage, wing structures, tail
cones and even dynamic components [33].
The Air Force Materials Laboratory has taken a lead position and initiated
several major thermoplastic composites programs to exploit unique materials
and processing characteristic of thermoplastic matrices. Major universities and
aerospace manufacturers have been jointly and actively involved with these programs including &dquo;Manufacturing Science of Complex Shape Thermoplastics&dquo;
with the objective to develop, demonstrate and validate a science base for processing thermoplastic composites. A major aerospace company will continue
under an Air Force contract to work on &dquo;Design and Development of Databases
for Thermoplastic Composites&dquo; with the projection of producing the first prototype of the computerized thermoplastic composites data base in 1991. It is
believed that completion of these programs will be most beneficial for us in
future development of advanced thermoplastic composites.
We continue to believe along with several other major users of composites and
(TS)
versus
thermoplastic (TP).
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294
the Air Force Materials Laboratory that thermoplastic composites represent a
future direction. To fulfill the promise of these systems, we need to demonstrate
the viability of the technology reviewed in this paper in real applications, not
only to meet aerospace needs, but also to serve a wide range of industrial as well
as automotive markets.
ACKNOWLEDGEMENTS
The authors wish to thank their colleagues, Drs. R. K. Okine, J. F. Pratte, M.
W. Egerton and P. Popper, for valuable discussions and/or providing test results
of thermoplastic composites process development at DuPont. The authors would
like to thank Dr. R. A. Baker for his assistance in developing the relative cost
estimates of processing with thermoset versus thermoplastic matrix systems.
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2
3.
4
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6.
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Ibid
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, 21.1017-1055 (1987)
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, 27-39 (1988)
Muzzy, J D. "Processing of Advanced Thermoplastic Composites," Ibid
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P. and R. McConnell. "A New 3D Braid for Integrated Parts Manufacture and Improved
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Popper,
(1987)
Application
PCT/US87/02867
(1987)
(1988).
33. Marsh, G.
"Thermoplastics
Invade
U.K 7(3)
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(1988).
BIOGRAPHIES
I. Y.
Chang
Kevlarg fiber.
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296
J. K. Lees
Dr. Lees received his Ph.D. in Physics from Carnegie-Mellon University. He
has worked in the field of Composites, Polymer Alloys and Blend Technology
with several departments at DuPont. Currently he is the Manager of the Composites Research and Development Group at DuPont.
Downloaded from jtc.sagepub.com at FLORIDA STATE UNIV LIBRARY on December 20, 2014