26
CONTROL
26.1 INTRODUCTION
Consolidation is an important step that occurs
in almost every process used to make an
advanced composite article. Consolidation is
usually brought about by the application of
pressure at a boundary which squeezesair and
resin out of the composite thereby changing
both its microstructure and dimensions.
Improper consolidation can lead to voids,
residual stresses,warping and other unwanted
effects which could ultimately lead to the rejec-
tion of the part. A comprehensive discussion of
consolidation in composites would include
many complex phenomena. Simultaneously,
there is heat, momentum and mass transfer,
accompanied by the chemical curing reaction
of the resin and the deformation and motion of
fibers.
Consolidation techniques have been used in
the fabrication of both thermoset and thermo-
plastic composite parts, but are more crucial
steps in thermoset composite processing. The
traditional composite manufacturing process
for aerospaceindustry products usually starts
with the B-stage impregnated prepregs con-
sisting of fiber preforms and staged resin
matrix. Usually the resin content is relatively
high. In order to achieve the required compos-
ite material properties which are dominated
by the fibers, consolidation is used as an
important processing step.
Figure 26.1 shows a setup of the prepreg
Handbook of Composites. Edited by S.T. Peters.Published
in 1998by O1apman & Hall, London. ISBN 0412 540207
Fig. 26.1 Schematic of the prepreg lay-up used in
autoclave cure (Springer, 1986).
lay-up used in autoclave cure. In a traditional
lay-up process, prepregs with different fiber
orientation and architecture are placed in cer-
tain order forming a near-net-shape composite
structure. During the lay-up operation,
whether it is done manually or using a robot,
the trapping of air pockets within the structure
is unavoidable. Thus a consolidation step after
the lay-up operation is necessary.Prepregs are
usually provided with relatively low fiber vol-
ume fraction. With the consolidation step, the
fiber volume fraction of the composite product
can be increased and excessive resin can be
removed.
The basic mechanisms involved in a consol-
idation process are the fiber deformation and
resin flow, which are coupled with thermal
effects and the resin cure reaction. A similar
consolidation process can also be seen in soil
mechanics such as the settlement of a founda-
tion. However, the deformation behavior of
fibrous materials is substantially different
from that of granular structures and resin flow
behavior is strongly affected by thermal effects
 Introduction 577

and chemical reaction of the resin. Thus, the surface roughness. Metals are widely used as
study of the consolidation process of fibrous tooling materials for composite processing.
composite materials involves many disciplines. However, their heavy weight and high cost of
To effectively control a consolidation machining become disadvantages when com-
process, the selection of the equipment and plex geometry is involved. Composite tooling
tooling materials is crucial. Major process materials have been used as alternatives in
parameters for a consolidation process include various consolidation processes.
pressure and temperature and both are func- Another tooling component for the consoli-
tions of time and are usually set as operation dation process is the bleeder, which is usually
cycles. Thus the system setup should be able a nonstructural layer of porous cloth or paper
to effectively control the pressure and temper- which allows the escape or bleed out of exces-
ature profile and transfer heat and pressure to sive gas and resin during the consolidation
composite parts. Figure 26.2 illustrates the process. Sometimes the process is called
process variables applied during autoclave migration. The bleeder cloth or paper is
consolidation and cure. removed after the curing process and is not
part of the final composite.
TEMPER ATU RE Breather material is used to provide a vac-
PRESSURE uum path over the surface of the part. Typical
materials are glass and mat. They can be
stretched over the part contours to ensure an
effective vacuum path and sometime also to
provide a cushion effect to matched metal tools.
Bagging and sealing are crucial to the qual-
ity of the composite parts. General
requirements for the bag are: (1)the bag must
apply curing pressure uniformly; (2) the bag
must not leak under molding conditions; and
t t i t t (3) a good vacuum path must be provided in
bagging. Silicone rubber vacuum bags are
Fig. 26.2 Illustration of the process variables (tem- widely used because of their long service life.
perature, pressure) applied during autoclave Moreover, they are repairable and self-healing
consolidation and cure (Springer,1986). with respect to pinholes. The initial cost of fab-
rication is relatively higher. Nylon is an
One of the commonly used facilities is an auto- alternative bag material for up to 193°C
clave, which is a closed pressure vessel with (380°F) and is usually discarded after use.
means for heating and applying pressure and The commonly used form of resin matrix
vacuum to its contents. The dimensions of the prepreg has a resin content beyond 40% and
composite parts are limited by the size of auto- requires a significant amount of resin bleedout
claves. Thus, for large size composite during cure to achieve a cured laminate resin
structures, alternative processing techniques content of 28-32%0.Low resin content prepregs
have been used, such as vacuum bag molding. have been developed which can be used with-
In addition to the equipment, tooling mate- out resin bleedout processes. Since there is no
rial has direct influence on the composite part bleedout process, less resin and less bleeder
surface quality, dimensional accuracy and material are needed for a consolidation and
residual stress. The main considerations for cure process. However, the removal of
tooling material include strength, stiffness, entrapped air becomes a more critical aspect of
thermal expansion coefficient, hardness and process control.
578 Consolidation techniques and cure control

26.2 CONSOLIDATION MODELS portion of the load, then Gutowski’s and

Kardos’ models are applicable.
As composite applications were expanded In the following discussions, both
rapidly in the late 1970s and early 1980s, stud- Springer’s model and Gutowski’s model will
ies on the process science of composite be presented. Kardos’ model is equivalent to
materials became very active, especially in the Gutowski’s model but different process vari-
areas of consolidation and cure (Lindt, 1982, ables are used in the modeling.
1986; Springer, 1982,1986; Loos and Springer,
1983a,b; Halpin, Kardos and Dudukovic, 1983;
26.2.1 RESIN FLOW
Loos and Freeman, 1985; Gutowski et al.,
1987a,b; Gutowski and Cai, 1988; Dave, The problem of resin flow in composite pro-
Kardos and Dudukovic, 1987a,b; Tang, Lee cessing can be treated as flow through fibrous
and Springer, 1987; Batch and Macosko, 1988; porous media. In general it can be handled by
Kim et al., 1988 and 1989; Connor et al., 1993). Darcy’s law which states that the flow rate is
The purpose of these studies has been to find proportional to the pressure gradient applied
out the most suitable process parameters and and is related to the porous medium perme-
then through scientific process modeling to ability and fluid viscosity. The general form of
achieve the optimized composite product Darcy’s law in a one-dimensional case is:
quality.
Pioneering work in composite consolida- (26.1)
tion and cure modeling was led by Springer
(Springer, 1982; Loos and Springer, 1983a). where q is the average resin flow rate, K is the
Laminated composite structure was consid- preform permeability with the units of length
ered with bleeder layers placed on top of the squared, p is the resin viscosity and dp/dx is
composite laminates. When pressure was the imposed pressure gradient. In the case of
applied transversely to the laminate plate, resin flow into the bleeder, the consolidation
excessive resin material which was in a fluid pressure is established between the advancing
state was squeezed out from the laminate. flow front and the tool or mold surface.
Similar consolidation models have also The main issue involved in using Darcy’s
been developed by Gutowski’s group and law in the consolidation process is that neither
Kardos’ group (Gutowski, Morigaki and Cai the fiber preform permeability nor the resin vis-
1987a; Gutowski et al., 1987b; Dave, Kardos cosity is constant over the process. The preform
and Dudukovic, 1987a,b). In these models, permeability is a function of the porosity or
both the fiber material deformation which is fiber volume fraction, fiber diameter, fiber ori-
highly nonlinear and the outgoing flow of the entation and fiber architecture. Among them
resin are considered. the fiber volume fraction changes substantially
As can be seen from the discussion pre- during a consolidation process. Resin viscosity
sented later, both approaches are valid within is related to temperature, the cure status and
the ranges of parameters considered. cure time and changes dramatically in the
Experimental verification results show good process. Usually at the start of a cure process,
agreement with these model predictions resin is in the semi-solid state. With the rise of
(Gutowski et al., 1987b; Kim et al., 1988; Cai temperature, it becomes fluid. As the degree of
and Gutowski, 1989). When resin content is cure increases, it gels and becomes solid.
relatively high and fiber-to-fiber contact is The permeability of fibrous preforms has
insignificant, Springer’s model can be applied. been studied both analytically and experimen-
On the other hand, if fiber volume fraction is tally (Williams, Morris and Ennis, 1974;
relatively high and fibers carry a substantial Gutowski et al., 1987b; Lam and Kardos, 1988,
 Consolidation models 579

1989; Van Den Brekel and De Long, 1989)

using the well-known Kozeny-Carman equa- 0 20 ply somple (0.002in/min.carn oill
tion. The estimation formula using the fiber x 20 ply sample (0.005 in/rnin.com oill

structural variables can be written as:

r; (1- VJ3
K = -~ (26.2)
4k0 v; Carman- Kozeny Eq, kxx=0.7
where rf is the fiber radius, V, is the fiber vol-
ume fraction so that (1- VJ is the porosity and x 5
k, is an empirical constant, called the Kozeny
constant, which is usually determined experi-
mentally. For different textile architecture and
orientation, the value of k, will be different.
Reported experimental data show that for an
aligned fiber bundle, k,,= 0.5-0.7 for the longi-
tudinal flow and k, = 11.0 for the transverse
flow. For f 45" cross plies, k, = 2.70. For woven
Fiber Volume Fraction (Vf)
type textile preforms, ko = 5.5. It should be
pointed out that many experimental results
Fig. 26.3 Comparison of measured axial permeabil-
have been reported and the variation of the
ity values for aligned AS-4 fibers with
Kozeny constant in some cases is significant. Carman-Kozeny equation (Gutowski et al., 198%).
Also in the transverse direction, a modified
Kozeny-Carman equation has been proposed
to account for the stop-flow phenomenon
when fiber volume fraction reaches the maxi-
mum packing efficiency (Gutowski ef al.,
198%). Figure 26.3 shows a comparison of
measured axial permeability values for aligned
fibers with the Kozeny-Carman equation.
Resin viscosity can be expressed as an
empirical function of temperature and degree
of cure (Lee, Loos and Springer, 1982). The
expression can be written as:
p = p-exp (U/RT+Ka) (26.3)
where p- is a constant, U is the activation
energy for viscosity, a is the degree of cure
and K is a constant which is independent of Fig. 26.4 Measured viscosity of 3501-6 resin as a
temperature. function of time (Lee et al., 1982).
Experimental study has been performed for
the Hercules 3501-6 epoxy resin which is at a constant temperature. Thus the value of K
widely used in composite fabrication. Figure *
is found to be 14.1 1.2. The values of p, and
26.4 shows the viscosity measurement as func- U are found to bep- = 7.93 x Pa s, U = 9.08
tions of temperature and time. To match the x 104J mol-'.
model predictions and experimental data, the The degree of cure a and the rate of degree
constant K is found by fitting a linear least of cure da/dt were determined from the
square curve to the p versus a data generated results of 'isothermal scanning experiments.
580 Consolidation techniques and cure control
Efforts were made to describe the d a l d t ver-
sus a data with a modified Arrhenius type
equation. The proposed empirical equations
are
d a l d t = ( K , + K,a) (1- a ) ( B - a) (26.4) tional. Thus 2-D or 3-D flow equations have to
a 10.3
da/dt = K3 (1- a )
a > 0.3
where
K , = A, exp (-AE,/RT)
K2 = A, exp (-AE,/RT)
K, = A, exp (-AE,/RT)
A,, A, and A, are the pre-exponential factors,
AE,, AE, and AE, are the activation energies, R
is the universal gas constant, and T is the
absolute temperature. The constants in the
expression are found as:
B = 0.47
A, = 2.101 x lo9 min-'
A, = - 2 . 0 1 4 ~ l O ~ r n i n - ~
A, = 1.960 x lo5 min-l
AE, = 8.07 x lo4J mol-'
AE, = 7.78 x 104 J mol-'
AE, = 5.66 x lo4J mol-'
As can be seen from the discussion, all the con-
stants involved in the model are determined
experimentally through a specified process.
Similar treatment can be used for other types of
resin systems, and experimental investigation
results have been reported, including Hercules
HBRF-55 Resin (Bhiet aI., 1987)and Fiberite 976
Resin (Dusiet al., 1987).A similar process model
has also been discussed by Roylance (1988).
When the permeability and the resin viscos-
ity are known, with the imposed applied
pressure condition, the rate of the outgoing
resin flow can be calculated using the Darcy
equation. In general, flow may be multi-direc-
be solved. In practice, resin flow in one partic-
ular direction may be dominant, and the
(26.5) analysis can be handled as 1-D permeable
flow.
26.2.2 FIBER DEFORMATION
The main contribution from Gutowski's model
is the description of fiber deformation behav-
ior. Instead of treating fibers as separate layers,
a network concept is introduced. In other
words, fiber-to-fiber contact is assumed within
a fiber assembly, even in the case of aligned
fiber bundles. Thus a fiber filament span
between the neighboring contact points
becomes a small bending beam. During a con-
solidation process when fibers are pushed
closer, more and more fiber-to-fiber contacts
take place, and the span length reduces. Thus
the bending stiffness of these small fiber
beams increases rapidly, resulting in nonlinear
elastic deformation response. The nonlinear
elastic response of a fiber assembly under a
compressive load has been also studied in the
textile field, and an empirical formula was
proposed (van Wyk, 1946).
A proposed fiber deformation model for
aligned fiber bundles considers the deforma-
tion status variable, the fiber volume fraction
V f ,as a function of the consolidation pressure
(Gutowski, 1985).The expression is
where V , is the maximum obtainable fiber vol-
ume fraction for a given fiber network
configuration, and V , is the fiber volume frac-
tion below which the fiber network carries no
load. The empirical constant As is obtained
from curve fitting on available measurement
data. A typical fiber deformation curve for

well aligned graphite fibers is shown in Fig.
26.5 with the- co-mparison of measured data
points.
In
,Q 700
b
In
v)
? 500 Data Point-
al
-1 300
e
:200
.c
100
n-
0.4 0.5 0.6 0.7 0.8 0.9
Fiber Volume Fraction ( V f )
Fig. 26.5 Typical fiber deformation curve for well-
aligned XA-S and A S 4 graphite fibers (Gutowski et
al., 198%).
The proposed relationship between the com-
pressive fiber stress ofand fiber volume fraction
V , provides a tool to estimate the finished con-
solidation status of the composite products. If
the time window for the consolidation is long
enough, and excessive resin is completely
squeezed out from the structure, the consolida-
tion pressure is then balanced by the fiber
stress. However, because of the dramatic
change of the resin viscosity and preform per-
meability during a consolidation process, resin
flow may not be complete. Thus, developed
consolidation simulation models are needed for
the process analysis and improvement.
During the compression of fibrous pre-
forms, structural relaxation has been observed
(Gutowski, 198%). Thus the deformation to
some extent is not elastic but viscoelastic. This
issue has been addressed by using a Maxwell
type model (Kim, McCarthy and Fanucci,
1991).
Consolidation models 581
26.2.3 CONSOLIDATIONMODELS
As discussed above, in Springer’s model, it is
assumed that there is no fiber-to-fiber contact.
Thus a dynamic fluid pressure exists between
the consolidated layers. The consolidation
time, which is crucial to the cure process, is
related to the permeability of the fibrous pre-
forms, resin viscosity, and the applied
consolidation pressure. In Gutowski’s model,
the fiber reinforcement and the fluid state
resin are considered as a system. Both fiber
network deformation and fluid resin flow are
solved together. Both models are presented
here with a laminated composite structure as
the example.
The example for Springer’s model is the
laminate consolidation with flow in the lami-
nate transverse direction, or z direction. A
bleeder ply is assumed to be placed on top of
the composite. Figure 26.6 shows the setup for
the model. At any instant of time the liquid
velocities in the bleeder Vb and in the compos-
ite V care given by Darcy’s law. For a constant
viscosity liquid, the integrated forms are:
K c (Po - P,)
9, = 7 (26.7)
hC
where p , and pb are the pressures at the com-
posite-bleeder interface and in the bleeder
respectively, po is the consolidation pressure
and is related to the applied force or pressure,
is the instantaneous thickness of the liquid
in the bleeder, and hc is the thickness of the
resin starved layer, or the thickness of the lay-
ers through which resin flow takes place, and
K, and Kb are the permeability of the compos-
ite layer and bleeder respectively. If the
compacted composite layer thickness is h,,
then
hc = nh, (26.9)
where n is the number of layers or plies
already compacted.
582 Consolidation techniques and cure control

L Resin Flow

Fig. 26.6 Illustration of the consolidationmodel proposed by Springer (1982).

The equation of continuity gives the rate of layers. The final status of the composite is
change of volume of the composite as: dependent on the compaction of each individ-
ual layer.
-~ d(hA) = Aq, = Aq, (26.10) As a comparison, Gutowski’s consolidation
dt model combines the flow of resin through
where A is the surface area of the composite porous media and the fiber deformation
laminate, and h is the total thickness of the behavior. Similar treatment has been pre-
composite laminate. The second equation sented in studies of other fields including soil
expresses the fact that at any instant of time, mechanics (Biot, 1941,1955,1956; Gibson and
the flow out of the composite is equal to the Hussey, 1967).In general, consolidation occurs
flow into the bleeder. The pressure po is related in only one direction, but flow may take place
to the applied force as: in all three directions. Thus an element is
deformable in the z direction. A new variable 6
f
(26.11) is used to represent the deformation, and 6 = z
= + pa + w where w is the local displacement of the
where F is the applied force and pa is the fiber network. The laminate setup for the
atmospheric pressure. By combining these model is illustrated in Fig. 26.7. If the initial
equations, the consolidation equation fiber volume fraction for the composite is V,
becomes: and the fiber volume fraction at any instant is
Vf, the fiber continuity condition states
vo=-v,
36 (26.13)
aZ
Therefore for each individual layer, the consol-
idation time can be calculated. The total Resin flow continuity condition requires:
consolidation time is the summation for these
 Consolidation models 583

Here it is assumed that the inertial effects in

the process are small. Therefore the applied
pressure is balanced by a combination of the
average resin pressure and the fiber stress. In
(26.14) other words, any load which is carried by the
fibers is then unavailable for pressurizing the
With the application of Darcy's law, a consoli- resin.
dation equation using the fluid pressure p , and Since both the permeability and the fiber
fiber volume fraction Vf as variables can be stress are expressed as functions of fiber vol-
written as ume fraction V , with the given initial and
boundary conditions, the variables V ,and p , as
a function of time and location can be solved.
In general numerical calculation procedures
have to be developed for solving the partial
differential equations. In some simplified
cases, analytical solutions are possible.
This equation gives a relationship between the
spatial and time-varying nature of the pres-
Example problem 1: One-dimensional flow
sure in the resin and the fiber volume fraction
in compression molding
of the composite. The equilibrium statement
for the consolidation is: A simplified example of composite consolida-
tion is the compression molding of a flat
(26.16) rectangular laminate. The composite part is
A pressed between two solid dies. Therefore
only in-plane flow is possible. In other words,
flow components are in the x and y directions
only. If the initial fiber volume fraction is uni-
form, the equation of the resin flow and fiber
deformation becomes:

P av, = 0 (26.17)
J2Pr + K - a2pr + -~
K X ~y ay2 v, at
ho Here it is also assumed that there is no signifi-
cant pressure gradient in the z direction, and
the viscosity p does not vary spatially.
In some cases, K Z / a 2>> Ky/b2 where a and b
are the dimensions of the laminate in x and y
directions respectively. The compression
molding results in primarily one-dimensional
a€ flow in the x direction. Then the equation can
be solved analytically. With the assumed
boundary conditions of p , = 0 at x = M and
ap,/ax = 0 at x = 0, the result is a parabolic
pressure distribution as

Fig. 26.7 Illustration of the consolidation model

proposed by Gutowski et al. (1987a).
584 Consolidation techniques and cure control

The solution for the fiber volume fraction Vf as Example problem 2 Compression molding
a function of time is: with two-dimensional flow
Here the case of compression molding of a rec-
Po = Of(Vf) 3 pa'
+ K _ Vdvf
,T (26.19)
* L
tangular laminate with an isotropic in-plane
permeability is considered. In other words, Kx
This expression shows how the applied pres-
= Ky = K. This may correspond to a quasi-
sure p, is carried by the fiber stress G~ and the
isotropic lay-up. The flow equation becomes
average pressure in the resin. The load sharing
Poisson's equation, which can be solved by the
in a composite is directly analogous to how the
separation of variables technique. The solution
load is shared in a parallel spring and damper
for the pressure distribution in a laminate with
set. For example, initially if Vf is less than V,,
zero pressure at the boundaries is:
then there is no deformation in the spring
(fibers) and the entire load is carried by the
resin. On the other hand, at long times and
finite viscosity, if the rate of change of Vf is
close to zero, then the pressure in the damper
(resin) goes to zero and the total load must be
carried by the fibers. Figure 26.8 shows an
example of the one-dimensional flow in com-
With the applied load balance condition, the
pression molding with the comparison of
final result is:
computer simulation results.

It can be seen that the result is analogous to the

previous case except for a geometry effect
term which is shown in the bracket.

600
- PR,Theory Example problem 3: Bleeder ply molding

- 400 0 PR,Measured This has been presented with the Springer's

-
'3
0
model. In this case, a porous bleeder ply is
placed on top of the composite, and flow is
principally in the z direction. With the intro-
duction of a new variable, the void ratio
e = (1- Vf)/V, one may obtain the nonlinear
one-dimensional consolidation equation. An
equation similar to this was first derived by
Gibson et al. (1967) for the consolidation of sat-
Time ( m i d
urated clays. The expression is:
Fig. 26.8 Example of one-dimensional flow in com-
pression molding and computer simulation results
(Gutowski, et al., 198%).
-
at
(
de = (e, + 1)2- a - Kz 'Of ")
3.z p ( l + e ) ' e az
(26.22)
 Consolidation models 585

The void ratio e or the fiber volume fraction V,

is a function of both time and location. An
equivalent equation using variables Vf and p ,
can be written as

With similar pressure equilibrium conditions,

the distribution and time history of Vf or e can
be solved numerically. Figure 26.9 shows an DT
example of the bleeder ply molding measure-
ment setup, and the comparison of the TRANSDUCER
computer simulation results with the mea-
sured data.
It is interesting to see that, with Gutowski’s
600
consolidation model, the final status of the /Applied Pressure
composite in terms of the average fiber volume o doto
500 - -theory
fraction can be estimated from the proposed Modified
fiber deformation model if the consolidation
process is complete. The consolidation time for -.-
v)
400-
Cormon-Kozemy

a particular setup can be solved through a

v
300 -
numerical simulation.
3
As can be seen from the analysis, the total
consolidation time for a composite structure is L

strongly dependent on the dimension in the a \o

resin flow direction. For laminated composite IO0 \O

structures, usually the dimensions in x and y P

directions (directions within the laminate
structure) are much larger than that in the z
direction (direction transverse to the laminate
plane). For example, many aerospace struc-
tural parts range from a few inches to several
feet in x or y direction, but only have a thick-
ness of a fraction of an inch in the z direction.
Thus the bleeder ply molding process is pre-
ferred and is widely used in many part
fabrication processes. However, for the so-
called thick composites, for example with
lay-up of 64 or 96 plies, the consolidation time
required increases dramatically in the bleeder
ply molding cases. With the selected cure cycle
for thin composites, complete consolidation
may not be achieved for thick composites.
Thus the final fiber volume fraction of the thick
composite tends to be relatively lower. This has
been observed in experiments involving thick
0
0 10 20 30 40 50 60
Time (rnin)
Fig. 26.9 Example of bleeder molding and com-
puter simulation results (Gutowskiet al., 198%).
composites (Kim, Jun and Lee, 1989).
It can also be seen from the comparison of
the two models that with relatively low fiber
volume fraction, fibers carry almost no load.
Thus the consolidation process is dominated
by the resin flow through the fiber network.
Then the difference between the two models is
very minor. Springer assumes the consolida-
tion is done layer by layer, while Gutowski
treats the fiber network as a whole system.
However, in both cases the top layers are con-
solidated first. When the fiber volume fraction
becomes high, then the predictions from the
586 Consolidation techniques and cure control
two models show significant different results.
On the other hand, the numerical schemes of
the two models are different. Springer’s model
requires only the solutions of a series algebraic
equations, while in Gutowski’s model nonlin-
ear partial differential equations have to be
solved. A comparison study has been pre-
sented by Smith and Poursartip (1993).
26.3 CURE CONTROL
Fiber reinforced thermosetting resin compos-
ites manufactured in autoclaves are made by
forming the uncured fiber-resin mixture into
the desired shape and then curing the mater-
ial. Curing requires the application of heat and
pressure. Heat is used to facilitate and control
the chemical reactions of the resin, and pres-
sure is used to consolidate the composite,
squeeze out the excess resin, and minimize the
void content. A cure cycle usually means the
magnitude, duration, and profile of the tem-
perature and pressure applied during a curing
process. Selection of the cure cycle directly
affects the quality of the finished composite
product, such as fiber content, fiber distribu-
tion, and void percentage.
Viscosity
/
Reaction kinetics
\ Heat transfer
Fig. 26.10 Schematic of overall cure process model (Dave et al., 1990).
Specifically, a selected cure cycle must
ensure that:
the temperature inside the material does
not exceed a preset value at any time during
the cure;
2. at the end of the cure the resin content is
uniform and has the desired value;
3. the material is cured uniformly and com-
pletely;
4. the cured composite has the lowest possible
void content;
5. the cured composite has the desired ther-
mal and mechanical properties;
6. the curing is achieved in the shortest time.
Figure 26.10 shows schematically the overall
cure process model structure. In an early study,
Loos and Springer (1983a)proposed a thermo-
chemical model. Heat transfer from the
environment to the composite material deter-
mines the temperature distribution, the degree
of cure of the resin, and the resin viscosity
within the composite structure. The tempera-
ture inside the composite can be calculated
using the law of conservation of energy. By
neglecting the energy transfer by convection,
the energy equation can be expressed as:
b Flow
Residual stress
 Cure control 587

resin viscosity, the degree of cure a and the

rate of the cure da/dt can be characterized
using a modified Arrhenius type equation,
with relevant constants in the model deter-
-k-
i ~zE)
(
+p-
dH
dt
(26.24) mined experimentally (Lee, Loos and
Springer, 1982; Bhi et al., 1987; Dusi et al., 1987;
where p and Cv are the density and specific Roylance, 1988).Figure 26.11 show an example
heat of the composite, kx, k and k, are the ther- of the rate of heat generation and rate of
mal conductivities, and ?is temperature. In degree of cure of the 3501-6 resin system as
the case of relatively thin composite structure, functions of time and temperature.
conduction heat transfer is mainly in the z It is noted that the densityp, specific heat Cy,
direction. Thus terms in the x and y directions heat of reaction Hr, and thermal conductivity k
can be dropped. The rate of heat generation are all dependent on the instantaneous and
dH/dt is defined as: local resin and fiber contents of each ply, and

(26.25)
01
c3501-6 400K 1 05 450K 1
where H, is the total heat of reaction depend-
ing on the resin type. The rate of the cure
reaction is a function of temperature and the
cure status, and can be expressed symbolically
as:
da
- = f(T,
dt
4 (26.26)

The degree of cure is then determined as:

)$(:I
a =

It is assumed that for an uncured material, a =

0, and for a completely cured material, a
dt (26.27)

o f \ , , Iojo\J
approaches unity. As discussed earlier the 0
0 02 04 06 0 02 04 06
DEGREE OF C U R E , a

TEMPERATURE ( K l

I I 1 1 I I

3501 - 6
-

-1 0 5 r n coI/sec

s\ Fig. 26.11 Rate of heat generation

and rate of degree of cure of the
I , , , , ~ , , l , l l l l
588 Consolidation techniques and cure control

can be handled using rule of mixtures (Loos pressure early in the cure cycle and the initial
and Springer, 1983c) or proposed approximate resin moisture are crucial considerations in
formulas (Springer and Tsai, 1967). producing void-free laminates (Kardos et al.,
The solution to these equations can be 1983, 1988). Since the driving force for diffu-
obtained once the initial and boundary condi- sion rises with temperature, in order to
tions are specified. The initial conditions prevent the potential for pure water void
require that the temperature and degree of growth by moisture diffusion in a laminate at
cure inside the composite be given before the all times and temperatures during the curing
start of the cure. The boundary condition cycle, the resin pressure at any point within
requires that the temperatures on composite the curing laminate must be higher than the
surfaces in contact with the tool be known as a minimum resin pressure required, which is a
function of time during cure. Therefore the function of the relative humidity and temper-
boundary condition is related to the specified ature (Dave et al., 1990).Figure 26.12 shows a
cure cycle and the equipment setup. void stability map for pure water void forma-
The objective for the cure control scheme is tion in epoxy matrices. A similar pressure
to achieve the desired composite quality. Some requirement also holds for small air/water
of the main targets are reasonable temperature voids after an initial growth period. It has also
distribution, complete consolidation, mini- been observed that the void content is reduced
mum thermal stress and minimum void
content.
(1 ATM I 101 kPI)
With a developed numerical scheme, the
temperature distribution inside the laminate is
calculated as a function of position and time. A
(RH), = 1ooO/o (RH),= 50%
good cure scheme should realize the two main
targets: (a) the temperature is reasonably uni-
form inside the material and (b) the
temperature does not exceed a preselected
maximum at any time.
For a given cure temperature and cure pres-
sure, the time window for the consolidation is
then specified. From the consolidation models,
the compaction status of the consolidated
composite can be obtained. In Springer’s
model, the result is the total number of com-
pacted plies, while in Gutowski’s model the
result is the V ,distribution across the layers. If
the consolidation cannot be completed with
the selected cure cycle, proper modifications
are then made. The compaction issue becomes
crucial to the cure process of the thick com-
posite structure. A multiple stage heating
process may be designed to defer the cure
reaction of the resin and thus prolong the con- 300 400 500
solidation time window. 1,K
Voids within the composite material are
harmful to its mechanical Performance. Fig. 26.12 Void stability map for pure water void
Experimental study shows that the resin formation in epoxy matrices (Dave et al., 1990).
 Efects of tooling and part shape 589

significantlywhen the applied pressure is suf- heated to a specified temperature at a speci-

ficiently high to collapse the vapor bubble fied rate under controlled conditions in the
before the gel point is reached. Therefore, after autoclave.
the time-temperature cycle is determined, it is Tooling materials may be metal (steel,
possible to obtain a profile of the minimum nickel, nickel alloys, and aluminum),
pressure versus cure time. The boundary pres- graphite-epoxy and elastomer, depending on
sure is then maintained greater than the different composite part shape, size, volume of
minimum pressure throughout the cure cycle. production and curing method. Selection of
During the cooling stage after the cure of the tooling material often reflects a compro-
the composites, residual thermal stress is mise among these considerations. Thermal
related to the difference between the cure tem- behavior of the tooling material is also crucial
perature and ambient temperature, and the in the design and fabrication. Table 26.1 lists
thermal expansion behavior of the composite the coefficient of thermal expansion of differ-
material. For a laminated structure, calcula- ent composite and tooling materials. The
tion of the thermal stress has been discussed values for the composites are dependent on
and formulated by Tsai and Hahn (1980). the ply orientation and fiber volume fraction,
Since the material shows viscoelastic behav- and typical values are shown there.
ior, stress relaxation has been observed over
time. A post-cure process is usually applied to
the structure to relieve the induced thermal
stress. Table 26.1 Coefficient of thermal expansion (CTE)
For large complex-shaped composite struc- for various materials (Borstell and Turner, 1987)
tures, non-autoclave curing methods are used.
Compared with traditional autoclave curing Material CTE ( I P / K )
methods, the component size restrictions are Structural composite material
eliminated, energy consumption is reduced, Boron-poxy 3.6-10.8
and capital equipment cost can be cut down. Aramid+poxy -2.0-5.8
The non-autoclave processes use an oven, inte- Graphiteepoxy 1.8-9.0
grally reinforced tools, and presses. Major Fiberglass-epoxy 7.2-9.0
issues related to non-autoclave curing are the Tooling material
effective compaction of the composite plies, Graphiteepoxy 4.1-9.0
and the elimination of the trapped interlami- Cast ceramic 0.81
nar or intraply air. Tool steel 11.3
Iron (electroformed) 11.9
Nickel (electroformed) 12.6
26.4 EFFECTS OF TOOLING AND PART High-temperature cast epoxy 19.8
SHAPE Aluminum 23.2
Silicone rubber 81-360
Properly designed tools that produce accept-
able parts on a reproducible basis are a must
when fabricating composite structures. The
tool design requires the consideration of as
26.4.1 TOOLING FOR AUTOCLAVE MOLDING
many factors as are studied in the design of
the part itself. The main requirement for the The traditional autoclave molding process
tools is to maintain proper geometric dimen- uses a vacuum bag to impose a pressure dif-
sional stability and surface profile during the ference on the composite lay-up. A typical
compression and thermal cycling processes. bagging system consists of the following steps
On the other hand, the tool must also be (Schwartz, 1983).
590 Consolidation techniques and cure control

1. Cover the lay-up with a perforated parting Graphite-epoxy laminate Angle caul plate
film or separator. Then lay up a layer or lay-
ers of bleeder material. The requirement of
the bleeder layers should be such as to
ensure adequate bleeding of air and excess
resin out of the part.
2. Place a strip of jute (vent material) just
beyond the edge of the lay-up and put bag-
sealing compound along the outside
perimeter.
3. Cover the lay-up, jute, and sealing com- Mold form -/ Caul plate stop

-
pound with a flexible-film diaphragm and
seal the diaphragm to the mold with the
{Resin reservoir
seal compound. cdp\
4. Connect the vacuum lines and slowly apply
the vacuum pressure while working the
wrinkles and excess air out of the lay-up,
bleeder material, and vacuum bag.
5. Check system for vacuum leaks. Mold half- .Mold half
6. Keep the part under vacuum while it is
waiting to be cured in the oven or auto-
clave.
To prevent surface irregularities on the bag
side (untooled surface) of the parts, a caul
plate may be used. The sole purpose of caul
plates is to improve the visual appearance of
the parts. They do not control part thickness. A I
flexible caul plate with a thermally stable rub- \Cao
ber such as silicone or a fluoroelastomer is
often used to accommodate the surface geom- Fig. 26.13 Example of autoclave tooling (Borstell
and Turner, 1987).
etry. Figure 26.13 shows examples of autoclave
tooling setups with caul plates.
The three issues related to the tooling introducing a thermal strain. As the part and
design (Borstell and Turner, 1987) are thermal tool cool down from the gel temperature, the
expansion correction, coordinating the loca- tool usually shrinks more than the part. As an
tion of partial plies and use of caul plates. alternative, graphiteepoxy molds are used in
Because of the low coefficients of thermal some applications. Although some data has
expansion of composites when compared with been published, not all composite materials
metal tooling materials, thermal strain or have been measured. One empirical method is
stress must be considered for a curing process. to cure a representative panel on a plate of the
In the autoclave, the temperature at which the specified tooling material using the specified
resin solidifies is the gel temperature. At that cure cycle. Corrections can be estimated by
specific temperature, the part is the same size comparing the difference between the mold
as the thermally expanded mold. At a temper- and part dimensions. Another recommended
ature above the gel temperature, the tool empirical correction method is to correct steel
expands more than the partially cured part or nickel tools by making the tool 0.999 of the
 Effects of tooling and part shape 591

engineering dimension, and to correct alu- aluminum. During autoclave curing of com-
minum tools by 0.998. For example, a 2540 mm posite parts, the thermal uniformity is
(100 in) dimension is tooled to be 2537 mm excellent with rapid heat-up and cool-down
(99.9 in) for the steel tool. These corrections are
rates. It is easy to handle and transport
needed to ensure an acceptable fit of mating because of its light weight. It also offers out-
composite parts. standing durability because the mold surface
Most parts contain partial plies to accom- resists cutting or impact damage and is not
modate local areas of increased stress. Several thermally degraded. When damaged, it is easy
techniques are used to control the location of to repair by welding, soldering, silver-solder-
partial plies, including polyester film tem- ing, or selective plating. It can provide
plates, slotted templates, and rails and complex contours without expensive machin-
banking surfaces. These tools serve as supple- ing. With most resin systems, it shows good
mental guidance to position the partial plies inrelease properties.
the lay-up process. Figure 26.14 shows the procedures of mak-
Typical cases of applying a caul plate are toing an electroformed nickel tool. As in some
control the edge of a panel or the flanges of other types of tooling, constructing a model of
channels. The design of the metal caul plates the part surface is the first step in creating an
must take into account the fact that the matrix electroformed mold. The models are the same
resin melts in the autoclave to a very low vis- net dimensions as the required nickel mold.
cosity. The caul plate performs by pushing Compensation may be required when the coef-
excess resin sideways. Thus the rigid metal ficient of thermal expansion of the composite
caul plates must have high rigidity so that part differs greatly from that of the nickel
they do not deflect under autoclave pressure mold. Models are made from plaster, epoxy-
at curing temperature. The thickness of the faced plaster, fiberglass, fiberglass-epoxy,
caul plates can be calculated by use of the wood or other materials. From the model a
equations for unsupported bending beam reverse mandrel 'splash' is generally fabri-
analysis. The deflection of the caul plate can be
cated from epoxy-faced fiberglass or plaster.
estimated using the balance condition of resin The mandrel to be used in electroforming is
pressure and applied force (Gutowski and Cai, then copied from the 'splash', although the
1988).The caul plate deflections should be lim- model can be used as the mandrel if it is pre-
ited to half the tolerance permitted in the part.
pared correctly. The comers of the mandrel
should be designed to have radii in excess of
0.76 mm (0.030 in) to avoid thin spots in the
26.4.2 ELECTROFORMED NICKEL TOOLING
deposit. Draft and taper should be designed
An electroformed nickel tool consists of a into the mandrel to facilitate its removal from
4.6-6.4 mm (0.18-0.25 in) thick electrode- the electroform. Sharp corners or narrow, deep
posited mold surface that is supported by a grooves should be avoided if possible. The
simple steel substructure. The mold surface is mandrel can be fabricated from epoxy-faced
produced by the electroplating process fiberglass, rubber, or other materials. The sur-
(Sheldon, 1987). face of the mandrel is made conductive by
The electroformed tooling concept offers proper coatings. The back of the mandrel must
numerous advantages. The size of the mold is be reinforced to keep the mandrel from dis-
restricted only by the size of the electroform- torting during the electroforming process.
ing tank. The cost of producing duplicated Electroforming is the process of producing
tools is low. The mold surface is very smooth an article by electrodeposition of a metal onto
and scratch resistant. The coefficient of ther- a conductive mandrel surface. An anode sus-
mal expansion is approximately 40% less than pended in an aqueous electrolyte is connected
592 Consolidation techniques and cure control

---t -
Model Splash Fiberglass plating mandrel Mold electroformed
I
I
i

Plated mold and tool Mold and structure Plating mandrel

upport structure joined removed

Fig. 26.14 Example of electroformed nickel tooling (Sheldon, 1987).

to the positive pole of a DC electric source, and parts. These include low coefficient of thermal
the mandrel (cathode) is connected to its neg- expansion, ease of preparation, low density,
ative pole. The flow of electricity or electrons and thermal stability (Harmon, 1987). Their
results in the oxidation of a nickel anode to disadvantage is that they are less durable than
nickel ions and the reduction of nickel ions to metal tools.
nickel metal at the cathode (mandrel). The Composite tool making starts with a master
typical rate of growth is approximately model, usually built with plaster or hard-
0.013-0.025 mm (0.0005-0.001 in) per hour. wood. The master models require proper
When the electroform is removed from the drying, sealing, and coating with mold release.
mandrel, its surface is a mirror image of the Then lay-up can be done directly on the plaster
surface of the mandrel. A natural physical or wood master. Liquid gel coats are required
characteristic of electrodeposition is that elec- to obtain a high fidelity surface on tools cured
tric current will tend to localize the deposit on by the vacuum bag process which does not
all edges and corners, causing an uneven generate enough pressure to ensure a void-free
thickness on the electroform. However, there surface, but may not be required on tools
are a variety of techniques to offset this effect. cured by the autoclave process which does
After the desired mold thickness is provide sufficient positive pressure. Prepregs
obtained, the mold is removed from the tank, with light weight fabrics are used directly
cleaned and the steel back-up structure is against the tool surface, while prepregs with
attached. The nickel mold is then polished to heavier fabrics are used to build up the thick-
the required finish, and ready for use. ness. During the lay-up, care should be taken
to work each ply into all radii and corners and
to remove all entrapped air. Debulking is
26.4.3 GRAPHITE-EPOXY TOOLING
applied after the lay-up, either with a vacuum
Composite tools have definite advantages bag setup or with -assistance of an autoclave
over metal molds for large or highly contoured for a pressure debulk, to consolidate the plies
 Eflects of tooling and part shape 593

and remove all entrapped air. The curing
process is done with a vacuum bagging sys-
tem or with an autoclave. With the tool still on
the model, the support structure, either a solid
laminate or an ’egg-crate’ panel is attached to
the tool by means of locally applied fabrics,
room-temperature curing, and high-tempera-
ture resistant resins. Once the support
structure is cured to the laminate shell, it is
removed from the master. Care should be
taken to avoid damaging either the tool or the
master. Figure 26.15 illustrates the
graphite-epoxy tooling making process.
Compositetools are being used successfully
throughout the aerospace industry to produce
parts that are structurally reliable, repro-
ducible, and dimensionally accurate.
Teflon separator film Breather cloth
In thermal expansion molding, two basic
methods are employed: the trapped or fixed-
volume rubber method and the
variable-volume rubber method. Figure 26.16
shows the setup for both methods. The fixed-
volume method exploits the large difference
between the coefficient of thermal expansion
of the elastomer and that of metals. The elas-
tomer is confined within a closed metal tool
Rubber tool sized to fill
the cavih, in the pan
,Pan

/ Vacuum bag

.--- Floating-plate
pressure control

’ Rubber tool projects above the

-
pan 30 excess pressure is vented
by forcing the floating plate
to the bag.

‘PFP master

Fig. 26.15 Example of graphite-epoxy tooling

(Harmon, 1987).

26.4.4 ELASTOMERIC TOOLING

M ,Outer box

Elastomeric tooling or rubber tooling can be

used to generate molding pressure or to act as
a pressure intensifier. In thermal expansion
molding, elastomeric tooling is constrained
within a rigid frame to generate consolidation
w
Fig. 26.16 Example of elastomeric tooling (Foston
pressure by thermal expansion during the cur- and Adams, 1987) (a) fixed volume method;
ing cycle (Foston and Adams, 1987). (b) variable volume method.
594 Consolidation techniques and cure control

cavity. When heated, it expands into the cavity, Impregnated Composites, Proc. 9th Int. Cod.
exerting the pressure required to compact a Composite Mater. (ICCM-9), 1993, 3,575-583.
composite laminate. The variable-volume Dave, R.S., Kardos, J.L. and Dudukovic, M.P., A
Model for Resin Flow During Composite
method offers more flexibility and control than Processing, Part 1: General Mathematical
the fixed-volume method because a precisely Development, Poly. Composites, 1987, 8(1),
calculated volume of rubber is not normally 29-38.
required. In most applications, the rubber is Dave, R.S., Kardos, J.L. and Dudukovic, M.P., A
simply 'set back' to allow for the bulk factor of Model for Resin Flow During Composite
the molding material during assembly of the Processing, Part 2: Numerical Analysis for
tooling details. A floating plate is used for the Unidirectional Graphite/Epoxy Laminates,
Poly. Composites, 1987,8(2), 123-132.
pressure control. Dave, R.S., Mallow, A., Kardos, J.L. and Dudukovic,
Thermal expansion molding with elas- M.P., Science-based Guidelines for the
tomeric tooling has been successfully used on Autoclave Process for Composites
commercial aircraft parts such as rudders and Manufacturing, SAMPE I., 1990,26(3),31-38.
spoilers (Schneider and Carroll, 1987). This Dusi, M.R., Lee, W.I., Ciriscioli, P.R., and Springer,
reduces the number of detail parts fabricated G.S., Cure Kinetics and Viscosity of Fiberite 976
and the need for bonding and mechanical fas- Resin, J. Composite Mater., 1987,21(3),243-261.
Foston, M. and Adams, R.C., Elastomeric Tooling,
tening on assembly, thereby effecting in Engineered Materials Handbook, Vol. 1:
significant reductions in production time and Composites, ASM International, 1987, pp.
cost. 590-594.
Gibson, R.E. and Hussey, M.J.L., The Theory of
One-Dimensional Consolidation of Saturated
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