Composite Manufacturing

Atta ur Rehman Shah
PhD Student
Advanced Composite Materials Lab.
CHANGWON NATIONAL UNIVERSITY
Transport Phenomena in Composite
Materials

8.1: Introduction
Historically, materials were first produced by adding various
alloying elements and then tested to determine their
properties.

The composites field is unique in that composites are
designed to satisfy the performance requirements and then
manufactured.

In this chapter we concentrate on the design of processing
techniques to manufacture composites with the required
characteristics.
8.2: Resin Flow through Fiber Bed
The flow of resin in fiber bundles can be assumed to be a flow in a
porous medium, it has been generally analyzed based on Darcys
law.
Considering an infinitely small composite representative volume
element (RVE) as in figure, the resin flow in the fiber bed of the
composite material may be expressed by Darcys law:

8.2.1 Fiber Consolidation
u
i
is the resin flow velocity
k
ij
is the permeability of the fiber bed
p is the pressure in the resin
is the resin viscosity
(8.1)
The net resin flow rate in the x-direction; d
qx
can be expressed as

Considering the net resin flow rate in the x-, y-, and z-directions
simultaneously, the total net resin flow rate dq = d
qx
+ d
qy
+ d
qz
is
expressed by the following equation:

If the total volume of the composite RVE is v and the fiber volume is
v
f
, then the void ratio e, (volume not occupied by fibers)/(volume
occupied by fibers), becomes

(8.2)
(8.3)
(8.4)
where V
f
is the fiber volume fraction. The void volume v
v
=v-v
f
from the
RVE dxdydz is expressed as

Then the volume of resin v
r
is expressed as

where S is the degree of saturation, defined as the percentage of the
void volume that is filled with resin.
The rate of change of the resin volume in the volume of the RVE is
expressed by

(8.5)
(8.6)
(8.8)
Combining equations (8.3) and (8.8), the following resin flow
equation is obtained:

The above equation can be divided into four categories:
1. When both e and S are constant: steady flow.
2. When e varies, but S is constant: consolidation if e decreases, or expansion if
e increases.
3. When e is constant, but S varies: drainage if S decreases, or imbibition if S
increases.
4. When both e and S vary: compression or expansion.
(8.9)
During the processing (such as the curing operation) of the
composite material, the external applied pressure p
ext
(t) can be
divided into two components; , required for the fiber deformation,
and p(t), required for the resin flow:

The magnitude of stress was modeled by Gutowski and Dillon
(1997) by assuming elastic deformation of fiber bundles:
(8.10)
(8.12)
(8.13)
where V
a
is the maximum available fiber volume fraction, V
0
the initial fiber volume
fraction, and the material constant depending on the fiber bundle shape.
The above eqn is very complicated, Lee and Kim (1994) devised
another fiber deformation equation based on the method of soil
mechanics, such as:
where
0
is a constant determined by experiment.
(8.14)
Equation (8.14) has better fitting characteristics for the experimental results.
The permeability k
ij
in equation (8.1) has been modeled by several
researchers. One of the theoretical models is the KozenyCarman
equation:
where r
f
is the radius of the fiber and C
x
is the KozenyCarman constant determined by
experiment.
For flow transverse to the fiber bundle
where V
a
is the available fiber volume fraction at which the transverse flow stops.
The temperature inside composite structures is not always constant,
which affects the viscosity and degree of cure.
The energy equation is expressed as follows when the convective
heat transfer is neglected

8.2.2 Resin Curing Process
where T, , and c represent the temperature, density, and specific heat of
composite material, respectively.
K
T
xx
, K
T
yy
, and K
T
zz
represent the coefficient of thermal conductivity in the x-, y-, and
z-directions
Q/t in the last term represents the heat generated per unit mass
The heat generation term can be experimentally obtained by differential scanning
calorimetry (DSC).
The DSC is a cure monitoring technique that measures the degree of
cure by the heat generated during the cure of material.
The total heat generation H
U
can be expressed as:

(8.24)
(8.25)
where H
T
is isothermal heat of reaction.
(8.26)
The model for describing the isothermal cure of reactive resins is
given by (Lee, 1997):

where the constants k
1
, k
2
, m, and n are determined by nonlinear
least-squares curve fit to the d/dt versus data.

Hence Eqn (8.26) can be written as.
(8.29)
The viscosity of a fluid is a measure of its resistance to flow under
shear stresses.
In thermoplastic polymer, viscosity depends only on temperature and
shear rate; however, the viscosity of a thermosetting resin during the
curing process is a function of cure temperature T, shear rate , and
the isothermal degree of cure :
(Lee, 1997) recommends
For isothermal cure;
For non-isothermal cure;
Three parameter model;
where
and K
0
are the Arrhenius pre-exponential factors, and E
and E
are the activation

energies for the flow and the curing reaction, respectively.
The composite thermal conductivities of materials composed of
unidirectional fibers embedded in a matrix have been considered
(Springer and Tsai, 1967).
In the analysis, the following assumptions were made:
8.2.3 Composite Thermal Conductivity
1. The composites are macroscopically homogeneous.
2. Both the matrix and the fibers are locally homogeneous
and isotropic.
3. The problem is two-dimensional in the xy-plane, that
is, the temperature distribution is independent of z (as
shown in Fig).
4. The thermal contact resistance between the fiber and
the matrix is negligible.
The composite equivalent thermal conductivity K
11
in the fiber
direction may be predicted by assuming that the fibers and the matrix
are connected in parallel:

For the thermal conductivity K
22
in the transverse direction of fiber,
the representative volume element (RVE) whose dimensions are (2a
x 2b x 1), can be considered.
The heat flux q
T
i
per unit area per unit time in the x
i
-direction is
related to the temperature gradient T/x
j

where K
ii
(i=1, 2, 3) are thermal conductivities of composite in the x
i

(i=1, 2, 3) directions, respectively.

For new transformed axes x, y, z, as shown in figure

8.3: Cure Monitoring during Processing of Composite Materials
Cure monitoring is important for the quality control and improvement
of the mechanical properties of thermosetting resin matrix composite
materials.
Some cure monitoring methods are:

Differential Scanning Calorimetry (DSC), Dynamic Mechanical Analysis (DMA), Infrared
Spectroscopy (IRS), Optical Techniques, and Dielectrometry

Dielectrometry is considered the most promising in situ cure
monitoring technique, because it can monitor continuously the cure
chemistry of the resin throughout the process

The instrumentation includes two electrodes, which are embedded in composite
materials and are connected to an alternating electric field.
The amount of energy loss expended in aligning its dipoles and moving its ions in
accordance with the direction of alternating field is used for measuring the state of
cure.
Dissipation factor of the composite material is measured as:
V is applied voltage
V
m
is the voltage across composite
is the phase angle between V and V
m
Structure of a small interdigital
dielectrometry sensor
(dimensions in mm).
Isothermal degree of cure and the
derivative of the dissipation factor dD/dt
with respect to time when the holding
temperature was 120
o
C.
8.4: Heat Conduction and Moisture Diffusion in Composite Materials
The composite plates are usually thin compared with the in-plane
dimensions and frequently are subjected to temperature or moisture
differences through the thickness direction.
Therefore, the hygrothermal behavior in the thickness direction (z-
direction) is sometimes important.
The energy equation (8.23) becomes, without a heat generation
term,

The equation for moisture diffusion can be derived similarly as
or
where H is the moisture concentration (kg/m
3
) and K
H
zz
is the diffusion coefficient (m
2
/s).
(8.77)
(8.76)
In the study of hygrothermal behavior of composite materials, the
specific moisture concentration C (dimensionless) is frequently used

Physically, C represents the amount of moisture in the dry mass of
composite:
Eqn (8.77) can be written as:
where h is the thickness of laminate.
(8.81)
The solution of equation (8.81) with the boundary conditions is given
by (Holman, 1997)
As the time t increases, the specific moisture
concentration reaches C
throughout the
laminate, as shown in figure. Therefore, C

is
also called the equilibrium specific moisture
concentration.
8.5: Liquid Composite Molding (LCM) Processes
Liquid composite molding (LCM), includes several composite manufacturing
processes, such as resin transfer molding (RTM), vacuum-assisted RTM
(VARTM), and injection compression molding (ICM).

VARTM and ICM have been originated from resin transfer molding.

In RTM, liquid resin is introduced in a mold which already contains a dry
reinforcement called preform.

VARTM differs from RTM only in that a vacuum is drawn in the cavity before
the resin is introduced.

In the process of ICM, the mold is not fully closed at the beginning of resin
injection. The mold is compressed gradually after the resin is injected.
RTM VARTM
ICM
Darcys law for flow through porous media is used use to simulate
the mold filling process during RTM.
In a threedimensional flow in the preform with Cartesian coordinates,
the resin flow velocity components u
x
, u
y
, and u
z
in the x-, y-, and z-
directions, respectively, are expressed as

Then above equation can be written in a two-dimensional form with
p=p(x, y):
700 x 200 mm
rectangular cavity
Flow rate plot
Time plot
Flow Analysis in a
rectangular cavity
using LIMS
Flow Inlet port
8.6: Compression Molding
Compression molding has been used for molding thermosetting
materials such as phenolic powders and rubber compounds.

With the greater emphasis on the mass production of composite
materials, compression molding is now widely used to produce bath
tubs, dishwashers, refrigerators, air conditioners and automotive
components to replace porcelainized and painted steel.

In recent years, process developments such as in-mold coating is
used to mask the surface defects in a molded part, such as surface
waviness, porosity due to entrapment, and sink marks that appear on
the surface of a molded.
Compression Molding was used much, compared with the injection molding
process, until the development of highstrength sheet molding compound
(SMC).

SMC is a continuous sheet of ready-to-mold composite material containing
fibers and mineral fillers dispersed in a thermosetting resin.

The flow of SMC in the mold is a complex phenomenon which was
investigated with the following assumptions (Lee et al., 1984):

1. SMC is an incompressible, isotropic, Newtonian fluid under the molding conditions
used.
2. Nonslip conditions hold at the mold surfaces of z= h/2.
3. The dominant stresses are the transverse shear stresses across the narrow gap
between the mold surfaces and the in-plane stresses (in x,y-plane) are negligible.
Based on the above assumptions, the average velocities , and in
the x- and y-directions are expressed as
where p, , and h represent the pressure, viscosity, and charge thickness at time t, respectively.
where w
0
represents the mold closing speed (assumed to be constant)
(8.105)
(8.106)
(8.107)
The continuity equation in terms of the average velocity components
for an incompressible fluid is expressed as:

Substituting equations (8.105)(8.107) into equation (8.108), we
obtain the pressure distribution in the SMC:
(8.108)
The above method does not predict well for lower mold closing speeds according to
the experimental results performed by Barone and Caulk (1985).
At the faster mold closing speed, all
layers in a charge extend uniformly, with
slip occurring only at the mold surface.

At the slower mold closing speed, slip
also occurs between the surfaces of
interior layers.
Barone and Caulk (1986) analyzed the experimental results and advised the following
pressure distribution in the SMC
Where k
H
is the coefficient of
hydrodynamic friction, which considers
slip at the mold wall.
8.7: Continuous Molding Process
Filament winding is a technique used for the manufacturing revolved surfaces such
as pipes, tubes, cylinders, and spheres.

The winding angles and the placement of the reinforcements are controlled through
specially designed machines, traversing at speeds synchronized with the mandrel
rotation.
8.7.1 Filament Winding Process
The filament winding process can generally be classified as
helical and polar winding, as shown in figure.
The winding angle is specified by the ratio of the two relative
motions:

where N is the rotational speed (rpm), V is the speed of carriage
(m/min), and r is the radius of the current winding.

The two motions should be precisely synchronized for uniform
winding angle.
In racetrack polar winding, the fiber delivery system rotates in a
single plane or racetrack, as shown in figure.
The mandrel is incrementally rotated.
Stress in the direction of the fibers:
The circumferential component of the fiber tension:
The radial resin flow velocity u
f
through thickness:
Pultrusion (pull + extrusion) is a continuous manufacturing process
used to produce high-fiber-content plastic structural shapes.
Pultrusion can produce a variety of reinforced solid, tubular, or
structural profiles.
8.7.2 Pultrusion Process
Heat generated by the exothermic curing reaction raises the
temperature in the fiberresin stream.
The location of the exothermic peak depends on the speed of pulling
the fiberresin stream through the die, as shown in figure
Sumerak and Martin (1984) proposed five sources contributing to
total pulling force:
(1) hydraulic entrance effects, (2) thermal expansion of the liquid phase, (3) thermal expansion
and contraction of the gel and solid phase, (4) volumetric packing factors, and (5) die surface
and geometry factors.

The three phases contribute to the total pulling force, as expressed
by the following equation:
8.8: Autoclave Molding with Cooling and Reheating Cycles
During the cure of thick composite laminates, temperature overshoot may be
considerable, which degrades the properties of cured laminates.
Figure shows the effect of thickness on the midpoint temperature of carbon-fiber
epoxy composite laminates (T300/5208).
The laminates composed of more than 50 plies (1 ply thickness0.15 mm) would
be degraded because the maximum midpoint temperature exceeded the glass
transition temperature T
g
(140
o
C).
Kim and Lee (1997) introduced cooling and reheating steps into the
conventional cure cycle to prevent the temperature overshoot of thick
laminates.

Two important specific variables chosen to control the thermal
overshoot are the cure rate (d
m
/dt) and temperature (T
m
) of midpoint
of the laminate.

Using the variables, an autoclave cure cycle, which could maintain
the midpoint temperature within the temperature limit range (120
125C), was devised.
When the exothermic reaction of resin begins, the autoclave is
cooled by turning off the heater power to prevent temperature
overshoot.
To use this method, the cooling behavior must be determined by
experiment as shown in figure.
8.8.1 Cooling Step
The cooling curve of the autoclave
used for this experiment was fitted
to the following exponential form:
Where T
0
is the autoclave
temperature at the start of
cooling and t is the elapsed time.
(8.153)
The start point of cooling is set by a certain value of d
m
/dt, the rate
of degree of cure at the midpoint of the laminate.

In this case, the maximum temperature T
m
is limited to 125
o
C and a
value of d
m
/dt is chosen as the start point of cooling.

The value of d
m
/dt can be calculated from equations (8.26)(8.35)
and equation (8.153).

The cooling step ends as T
m
reaches the maximum value.
8.8.1 Cooling Step
When the midpoint temperature T
m
reaches the limit temperature
(125
o
C) and starts to decrease, moderate reheating is necessary to
maintain T
m
within a given temperature range.

The reheating rate of the autoclave was selected to maintain T
m

between the cure temperature (120
o
C) and the limit temperature
(125
o
C) in this example.

When the autoclave temperature T
a
reaches the cure temperature
(120
o
C) during the reheating operation, the reheating step ends and
most of the cure reaction of the laminate is almost accomplished.
8.8.2 Reheating Step
Figure 8.23 shows the modified autoclave cure cycle for the 100-ply
(15mm thick) laminate determined from the simulation with cooling
and reheating steps.
8.8.2 Reheating Step

Thank you

Composite Manufacturing

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