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www.elsevier.com/locate/compositesa

J.-L. Bailleul*, V. Sobotka, D. Delaunay, Y. Jarny

UMR CNRS 6607, Laboratoire de Thermocinetique, La Chantrerie-Rue Christian Pauc, 44306 Nantes Cedex 03, France

Received 3 July 2002; revised 23 January 2003; accepted 2 April 2003

Abstract

During thermoset composite materials processing, the chemical reaction is highly exothermic and because of the low thermal conductivity

of the material, significant temperature and state of cure gradients can be generated in thick parts. This creates non-uniform stresses that

provoke defects. We propose to control the transformation by monitoring the temperature of the mold walls. A general inverse analysis based

on the conjugate gradient method of minimization associated to the adjoint equations is used. After having detailed the method, we propose

two examples. The first one presents an optimal cycle to obtain uniform conversion at the end of the curing of an epoxy/glass-fiber composite.

The second example is concerned with the control of the temperature variations during the curing of a polyester/glass-fiber composite. The

method is experimentally validated and proves to be very powerful and flexible.

q 2003 Elsevier Ltd. All rights reserved.

Keywords: A. Thermosetting resin; E. Cure; E. Heat treatment

1. Introduction

Composites are more and more used in structural

applications and often reach thickness of the order of one

centimeter and this even for large series applications where

for productivity reasons the duration of the cycles becomes

relatively short. The composite materials are insulating,

and since the heat released during the chemical reaction of

curing is in the heart of the piece, the evacuation of the

heat generated is difficult. This provokes large temperature

and degree of conversion gradients. The quality of the part

is altered by the internal stresses that can provoke warpage

and in some cases cracks. The shrinkage of organic resins

reaches 7% during curing, even if thermoplastic additives

compensate partially at the end of curing [1,2]. If the

surfaces of the piece come unstuck from the mold wall

during gelation, the aspect of the surface is damaged. If

one has imperatives of surface aspect, it is therefore

necessary to control the development of shrinkage during

curing. In any case, one may try to master either the space

and time distribution of the temperature, either of the

conversion distribution, or the distribution of the shrinkage

* Corresponding author. Tel.: 33-2-4068-3137; fax: 33-2-4068-3141.

E-mail address: jean-luc.bailleul@polytech.univ-nantes.fr (J.-L.

Bailleul).

1359-835X/03/$ - see front matter q 2003 Elsevier Ltd. All rights reserved.

doi:10.1016/S1359-835X(03)00141-6

time. These distributions are not independent, they are

coupled, and the control of one can prove to be sufficient or

on the contrary it is impossible to control them simultaneously. The parameters on which one can act are the

cycles of pressure or the applied temperature profiles on

the walls of the mold.

In a recent article, Antonucci et al. [3] proposed a

methodology to act on the temperature profile of the mold

walls, in order to reduce the temperature gradients

connected with the exothermal reaction. The authors

show that the cycle limits also the gradients of conversion. Ruiz and Trochu [4] established a cycle of curing

permitting to reduce the residual stresses in the piece. In

these two examples, the authors follow an empirical

approach, based on intuitive physical considerations.

Although this approach gave excellent results, it cannot

take into account multiple constraints and couplings, for

example the impossibility to get very fast time variations

of the mold wall temperature or the complexity of the

thermo-mechanical coupling. An alternative consists then

of using a method of optimization in which one is

searching for an optimal cycle allowing to minimize a

criterion chosen according to a specific objective. It is

what we chose to illustrate in this article. The choice of

the criterion is delicate, but in this exploratory study, we

696

Nomenclature

a

ad

b

dH

DH

f

g

l

m

r

Cp

d

F

G

J

K

L

state of cure

desired state of cure

conjugate factor

residual energy

total enthalpy of the transformation (J/g)

value of the criterion

penalization factor

thermal conductivity (W/(m2 K))

distance of descent

density (kg/m3)

specific heat (J/(g K))

descent direction

function product of KG

kinetic function of a

deviation criterion

kinetic function of T

thickness of the piece (m)

conversion remains uniform in all points of the part

during a time between a time t1 and the time final tf : Two

examples will be presented to test the capability of the

algorithm. The first one consists of obtaining a uniform

partial conversion at the end of cure. This choice is linked

to a strategy of determining the thermal conductivity

according to the degree of conversion, that requires

obtaining a uniformly transformed sample. The second

consists of taking one of the cases treated in Ref. [3] and

applying the optimization method. We will search therefore a cycle that allows a conversion distribution in which

the state of cure gradients are limited during part of the

curing cycle. We will consequently limit the temperature

gradients and then the stresses.

2. Cure modeling

We consider a mold filled of raw composite, after the

filling phase. The piece is of uniform thickness and its size is

such that it can be considered as a plate. The walls of the

mold are heated and cooled, but the performance of the

temperature control system is such that the heating and

cooling rates are lower than a given limit. This will be

integrated like a constraint in the optimization process. The

temperature of the mold walls will be supposed uniform on

all their surface. We will consider that the variations of

temperature along the length and the width are negligible in

comparison to the thickness. As a consequence, the problem

will be considered as unidirectional across the thickness x:

The temperature and conversion field obey the energy and

kinetic equations coupled through the heat source due to the

curing reaction, and the thermal properties that depend on

the temperature and the state of cure.

L

Q

R

t

T

U

U

x

X

Lagrange multiplier

contact resistance (m2 K/W)

time (s)

mold temperature (8C or K)

mold process control temperature (K)

mean initial control (K)

space coordinate

mass ratio of resin in the composite

Subscript

normal

0

space coordinate equal to zero

f

fiber or final state

i

lower

n

iteration index

r

resin

s

upper

in Fig. 1, the conversion and temperature fields verify the

system of Eq.(1):

8

T

T

a

>

>

rCp a;T

l a;T

rXr DH

>

>

t

x

x

t

>

>

>

>

>

a

>

>

FT;a

>

>

t

>

>

<

initialcondition:

>

>

>

Tx;0T0 tandax;0a0 t

>

>

>

>

>

boundaryconditions:

>

>

>

>

>

T T0;t2Ut

T TL;t2Ut

>

>

x02

xL2

l

:

Rs t

Ri t

x 0

x L

1

The signification of the parameters is given in the

nomenclature. On the boundaries x0 and xL; we

suppose the existence of thermal contact resistances Rs t

and Ri t: The boundary conditions at x0 and xL are

completed by the mold temperature Ut which is imposed

in time. The goal of our optimization method is the

determination of the mold wall temperature during the

whole process.

degree of conversion by the rule of mixture, the validity

being demonstrated in Ref. [5]. The FT; a function

appearing in the kinetic equation describes the chemical

reaction with a phenomenological relation of Kamal and

Sourour [6] or a Bailleul type [7], for example. The

generality of the algorithm allows the integration of all these

types of expressions.

The control algorithm of such a strongly coupled nonlinear system of equations, under the constraint of

maximum rate of evolution for the boundaries requires

relatively complex methods of optimization. The objective

of this article is to test the feasibility of their usage on real

cases, in order to solve practical problems of composite

processing: with a press of a given performance, how can

we achieve a thick piece with a uniform conversion degree?

How can we minimize the temperature gradients

during curing? Two examples are proposed to reach this

objective.

3. Optimization method

The inverse Lagrangian method [8] is based on the

elaboration of a criterion. We try to determine a state of cure

as uniform as possible at the end of the cycle for which the

temperature does not exceed the boundary limit beyond

which degradation starts. We use an optimization method

which is detailed in Appendixes A and B. We thus define the

following criterion to be minimized:

22

JU kaU 2 ad k21 gkU 2 Uk

with

tf L

kf k21

f 2 dxdt

kf k22

tf

f dt

In the above expression, aU verifies the set of Eq.

(1) where U is imposed, ad is the required state of

cure and U is a curing cycle introduced a priori to

avoid unrealistic controls. In actual practice, the value

of U is selected in the practical range of curing

temperatures.

The optimum solution Up(t), which minimizes JU; is

determined by a conjugate gradient iterative method. The

principles of this method may be found in Ref. [8]. The

iterated values U n are determined by the following

algorithm (Eq. (4)):

Repeat:

U n1 U n mdn

with :

dn t 27J n t bn dn21 t

697

and:

8

tf L

>

>

7J n 7J n dxdt

>

>

>

0

0

n

< b t L

f

7J n21 7J n21 dxdt

>

>

0

0

>

>

>

: 1

b 0

descent, m is the length of descent and bn designates the

conjugate state (See Appendix A for more details. Eq. (4) is

identical to Eq. (A37) in this appendix).

Both the descent direction d n and the descent depth m are

determined by introducing the Lagrangian of the problem as:

La; T; Q1 ; Q2 JU:

L tf a

2 KTGa Q2 dtdx

t

0 0

L tf

T

a

T

2 rXm DH

2

rC p

l

Q1 dtdx

x

t

t

x

0 0

5

where Q1 and Q2 are Lagrange multipliers associated to T

and a; respectively. The increment of the Lagrangian is

defined by:

dLa; T; U; Q1 ; Q2

L

L

L

dT

dU

da

a

T

U

(see Appendix A):

8

L

>

>

< T dT 0 ;dT

7

>

>

: L da 0 ;da

a

We then obtain two equations defining the adjoint system

(Eq. (8)). The details on how to derive these equations and

how to compute Q1 and Q2 may be found in Appendix A.

8

C p Q 1

Q 1

F

>

>

Q

r

l

W

>

>

t

x

x

T 2

>

>

>

>

>

>

>

Cp T

l T

>

>

Q1

8

r

>

<

T t

T x

>

>

Cp T

>

Q 1 Q 2

F

Q

>

>

W

Q1 rXDH 1

Q2 r

>

>

t

t

>

>

>

>

>

>

l T Q 1

>

:

2a 2 ad

a x x

with the boundaries conditions:

Q

Q 0; t

Q

Q L; t

2 l 1 xL 1

2l : 1 x0 1

Rs t

Ri t

x

x

Moreover, when T and a satisfy the direct system, i.e. the

integral terms equal to zero in the Lagrangian expression

698

(5), we have:

dLa; T; U; Q1 ; Q2

L

dU 7JUdU

U

so

L

7JU

U

The derivative of the Lagrangian versus U provides the

gradient of the criterion, which is used to calculate dn t

from Eq. (4).

We are now concerned with the determination of the

descent depth m (Appendix B). For U and d fixed, the

scalar m is determined by the solution of the optimization

problem:

minimize JU mdn fm

with m . 0

10

We have:

22

fm kax; t; U m dn 2 ad k21 gkU m dn 2 Uk

11

depth m; we can now modified the boundary conditions and

reiterate the process according to Eq. (4).

The calculation of the mold wall temperature U p t

should be achieved by making sure that the value found is

not physically impossible to obtain. Rates of heating and

cooling depend on the equipment available. They must be

attainable with the device used to produce the composite

piece. A set of constraints on the mold wall temperature

values is then defined as:

8

>

< Umin # Ut # Umax

dUt

>

: Vmin #

# Vmax

dt

15

U p t on the interval 0; tf has been calculated on a limited

number of points. The algorithm computes U p tj with j

1; ; n; n being defined by the user (of the order of 10 in

the realistic examples presented here).

22 m2 :kdak21 kdnk22

fm ka 2 ad k21 gkU 2 Uk

tf L

tf

dndt

2m

a 2 ad da dxdt g U 2 U

0

12

which can be written as:

fm A 2Bm Cm2

13

minimum of fm is defined as: m 2B=C: The increment

da is determined by the resolution of the sensitivity

equations which are obtained by writing first the direct

system (1) with T m dT and a m da: Then the same

equations for T and a are subtracted from the preceding

ones to yield the following system

Cp

Cp

dT

T

r

dT

rCp

da

t

a

T

t

dT

l

l

T

l

da dT

x

x

x

a

T

x

da

rDHX

14

t

da

F

F

dT

da

t

a

T

with the boundary conditions:

8

dT 2dn

dT

l

l

T

>

>

>

< Rs l x a da T dT x ;t;x 0

> dT 2dn

dT

l

l

T

>

>

;t;x L

l

da dT

:2

Ri

x

a

T

x

4. Demonstration examples

In order to check more surely the validity of the

calculations we have used an experimental method.

4.1. Example 1. Partial uniform curing at the end

of the processing cycle

The objective is to obtain a uniform predefined

distribution of curing at the end of the process. This is

necessary to measure the thermal conductivity la; T of a

sample as a function of the state of cure a: In order to use

classical methods to measure thermal conductivity such as a

guarded heat plate or a function estimation it is easier with a

uniform cure. For the guarded heat plate method, if a is not

uniform we can not know for what value of a the results

correspond. For function estimation, it is very difficult to

identify simultaneously the temperature and state of cure

dependence of the thermal conductivity. It would be an

estimation method for two functions what is very difficult.

The progression of the reaction must reach the required

value at the end of the partial curing process with a curing

rate equal to zero to prevent the continuation of the reaction

after the end of the cycles as illustrated by Fig. 2. The

measure of the thermal conductivity will correspond to a

fixed and not time dependant state of cure. The evolution

curves 1 and 2 illustrating the state of cure evolution at are

considered correct because they provide a degree of curing

with a plateau between t1 and tf ; unlike evolution curve 3

which keeps on rising beyond tf :

To reach a curing rate equal to zero at the end of the

cycle, the ultimate progression stage must remain constant

at the ad value on the interval t1 ; tf : In this example, we use

699

Table 1

Parameters of the kinetic function K for the epoxy resin

fiber glass reinforcement (Brochier M10).

As presented in Eq. (1), the thermal parameters depend

on temperature T and the state of cure a: So we have to

measure these parameters as a function of T and a: The

methods are described in Ref. [7] for the specific heat and

in Ref. [5] for the thermal conductivity. For the specific

heat we consider a simple model based on the rule of

mixtures:

16

where Cp0 is the specific heat of the raw resin and Cp1 is

the specific heat of the cured resin. By measurement, we

obtain the specific heat in J/g K, with T in Celsius:

Cp0 T 1:584 3:259 1023 T

^0:06 J=g K

17

before Tg 135 8C :

Cp1 T 1:213 4:338 1023 T

^0:1 J=g K

after Tg :

Cp1 T 1:944 1:378 1023 T

^0:05 J=g K

model for transverse conductivity found in Refs. [10,11] in

which the following equation was established:

l lr a; T

1 vf lf T 1 2 vf lr a; T

1 2 vf lf T 1 vf lr a; T

Value

Tref (K)

kref (s-1)

A

423

6.988 1023

17.631

(21)). The parameter values are shown in Tables 1 and 2.

T

20

KT kref exp 2A ref 2 1

T

Cp a; T Cp0 Ta Cp1 T1 2 a

Parameter

18

and lr is the resin conductivity. By measurement, we obtain

the orthogonal composite thermal conductivity in W/(m2 K)

with T in (8C):

G n a

kp

X

a k ak

21

k0

to 412.3 J/g.

The validation of the inverse algorithm was carried out as

follows: for a given thickness L 10 mm; a curing cycle

giving a spatially uniform ad 0:5 has been determined.

We started from an homogeneous temperature (40 8C)

and a state of cure equal to zero ax; 0 0: We will only

discuss the case with ad 0:5; but other cases can be found

in Ref. [12]. The results obtained with ad 0:5 are shown

in Figs. 3 5.

Fig. 3 shows the optimum mold wall temperature U p t

computed for 12 points. The cycle has been applied on a

press since it satisfies the constraints of Eq. (15). Fig. 4

shows the evolution of the deviation criterion JU to tend

towards a minimum.

We can note that 15 iterations are required to reach the

minimum value of JU: The convergence, here, was

achieved in two stages: a first stage up to iteration 7 and a

second stage between iterations 11 and 15. Fig. 5 shows the

evolution of the temperature and the state of cure in

the> heart of the sample versus time. We show also the

temperature evolution at the boundary x 0: The temperature gradient in the sample remains small.

The exothermic process in the heart of the sample is well

controlled. The cycle obtained U p t allows the reaction to

start doing a first heating plateau. It anticipates the start of

Table 2

Parameters of the kinetic function G of the epoxy resin

Parameter

Value

a0

a1

a2

a3

a4

a5

a6

a7

0.042

5.078

28.502

2265.238

727.932

2961.274

627.499

2162.547

raw composite :

19

cured composite :

For the kinetic reaction, we use a model which gives

a=t as the product of an Arrhenius law (function KT;

700

a first cooling stage.

A low temperature post-cure plateau allows to keep the

reaction velocity steady before stopping it definitively with

the final cooling stage. Fig. 6 shows the evolution of the

state of cure through the thickness of the part for several

times.

Two heating Plate (diameter 162 mm) placed inside a

press apply pressure on the sample ensuring 1D heat

transfer. Details on the press may be found in Ref. [9].

We checked the spatial distribution of residual heat in the

piece and compared it with the desired spatial distribution of

state of cure at the end of the curing ad 0:5:

The validation consists of measuring the spatial distribution of residual heat dH 1 2 aDHX: We cut out a

piece of material in the axial area of the partly cross-linked

sample (Fig. 7). We successively removed some thin layers

at position xi to prepare the samples on which the residual

energy measurement dHi will be carried out.

The measurement of the residual energy is carried out

with a DSC. Given that we are performing this analysis on

very small composite material samples, the resin Xi mass

ratio is unknown and must be determined by thermal

gravimetric analysis by decomposing the sample and

keeping the fibers only. We can then deduce the state of

cure at position xi by:

Fig. 5. Evolution of temperature in the heart of the sample at 50% curing for

a 10 mm part.

axi ; tf 1 2

dHi

Xi DH

22

repeating this procedure at several locations across the

thickness of the part. The experimental results shown in

Fig. 8 are very satisfying.

4.2. Example 2. Optimal curing of a polyester-glass fiber

composite

The second test is related to the curing of a highly

reactive polyester resin and random glass mat (fiber volume

fraction: 0.32) of 10 mm thickness treated in [3]. The

objective is to minimize temperature gradients in the

thickness of the part during curing.

The physical properties of the materials used are listed in

Table 3. The kinetic model of the resin given in Ref. [3]

verifies Eqs. (23) (27).

a_ Kp 1 2 aR

dR

2fKd I

dt

dI

2Kd I

dt

where,

23

24

25

701

Table 3

Physical properties of polyester-glass fiber composite

Properties

Resin

Fiber

Composite

Density (kg/m3)

Specific heat (J/kg K)

Thermal conductivity (W/m K)

1100

1680

0.168

2560

670

1

1567

1152

0.13

Table 4

Kinetic parameters of the polyester resin

Fig. 7. Descriptive diagram of the operating mode.

E

Kd Ad exp 2 d

RT

26

Ep

a m

Kp Ap0 exp 2 0 1 2

af

RT

27

of Eqs. (23) (27). Fig. 9 represents the reaction

velocity calculated with Eqs. (23) (27) for various

curing cycles.

The formulation of our optimization method uses a

specific description of the kinetics based on an assumption

of separation of variables, so that the thermal release rate

can be written as:

da

KTGa

dt

28

temperature in Arrhenius form by a function of the

conversion degree.

We are then obliged to adopt a strategy consisting of

rebuilding the resin kinetics in the form of Eq. (28) starting

from the mechanistic model (Eqs. ((23) (27))). Optimization is then performed from the phenomenological model

(Eq. (28)) and its validity will be checked for the

mechanistic model.

Function K is determined by simulating constant heating

rates from 15 to 40 K/min. For each heating rate the cycle is

cure.

Parameter

Value

f

af

Ad

Ap0

Ed J=mol

Ep0 J=mol

It0

Rt0

Hr J=g

m

0.1

1.0

5.55 1016

0.38 1010

1.41 105

4.27 104

5.208 1023

0

244

4

temperature ramp between 25 and 220 8C and it is

completed by a last isotherm at 220 8C for 3 min. Then

for each scanning run, at a given time t; the temperature, the

conversion degree of the reaction, a; as well as the reaction

velocity da=dt are known. Fig. 10 represents the evolution of

the reaction rate, da=dt; according to the state of cure, a; for

several temperatures.

For each temperature, the curves pass by an extreme

which is approximately located at the same value a ap :

A reduced value of G is considered so that Gap 1: For

each level of temperature, one can determine the value of

the reaction velocity for a ap :

da

KT

29

dt aap

702

Table 5

Parameters of the kinetic function K for the polyester resin

Parameter

Value

Tref (K)

kref (s21)

A

361.5

6.192 1023

29.887

temperatures.

the function KT: This function is in the form of Eq. (20),

where Tref is a temperature chosen arbitrarily in the domain

of work at which a parameter Kref is associated. Thus, if we

draw the logarithm of KT for a ap as a function of

Tref =T 2 1 we obtain a straight line (Fig. 11). The slope is

2A and the line crosses the Y-axis at lnkref : This is

applied by taking a reference temperature of 361.5 K. The

parameters of function KT are given in Table 5.

The relationship between the reaction velocity and the

value of the function KT gives the value of function Ga

for a given conversion degree a: All the values obtained for

function G at several temperatures are presented in Fig. 12.

One thus can, with a good approximation, represent the

function Ga by a single curve, interpolated by

polynomials.

The interval [0,1] is divided into n subintervals

ai ; ai1 0#i,n in which

G is interpolated by a

P the function

k

polynomial Gn a kp

a

a

:

Table

6 gives the park

k0

ameter values of function G:

Fig. 13 shows that the phenomenological model is very

close to the mechanistic model for isotherms from 85 to

125 8C. We will thus use this model for optimization.

In order to approach realistic range of experimental

conditions, the maximum rate of the mold wall temperature

Ut is limited to 10 8C/min. It is a plausible maximum

heating rate for the Plate of a press.

equal to 20 8C and state of cure equal to zero ax; 0 0:

The initial cycle is a temperature ramp from 20 to 70 8C at

10 8C/min, then an isotherm at 70 8C for 30 min. Fig. 14 also

shows the cycle resulting from optimization, where four

points were examined in the cycle. One is composed of a

ramp from 20 to 68.5 8C, then a cooling to 24 8C and finally

of a second ramp to 75 8C. The rates of heating and cooling

Table 6

Parameters of the kinetic function G for polyester resin

State of cure interval

Parameter

Value

0 # a< 0:1

a0

a1

a2

a3

a4

a5

a6

0.0546

31.627

2431.148

3015.48

211,399.6

21,690.4

216,248.8

a0

a1

a2

a3

a4

a5

0.646

6.862

243.252

96.90

2104.198

45.373

a0

a1

a2

a3

2.116

26.107

5.777

21.782

0:8 # a

a0

a1

a2

a3

4.632

214.787

15.729

25.575

703

Fig. 13. Comparison of the curing rate given by the mechanistic model

(Eqs. (23)(27)) and by the phenomenological model (Eq. (28)) for a series

of constant temperatures presented in Ref. [3].

realistic in experiments.

We use the cycle of Fig. 14, determined by the inverse

algorithm and we add to this cycle a post-curing to 160 8C

for 30 min. The plateau at 160 8C is reached by a ramp at

10 8C/min. Then, one again calculates the changes of

temperature and conversion degree through the thickness of

the part (Fig. 15a and b). This direct calculation was carried

out by using the mechanistic formulation of the resin

kinetics.

We observe in Fig. 15a the very good homogeneity of

temperature during all the cycles. The most significant

variation, about 20 K, is for t 930 s at the beginning of the

cooling, the material not yet solid a , 0:6: The cooling

phase makes it possible to limit the heat released and as a

consequence, the temperature gradients.

Fig. 15b represents the state of cure in the part. The

reaction begins after 500 s. Then the conversion degree

increases quickly between 500 and 1000 s which corresponds to the heating ramp. During cooling, polymerization

is more rapid in the heart of the part, but the difference

decreases to lead to a quasi-uniform conversion degree a

0:64 at the end of the optimization, which was taken to

initiate the post-curing analysis.

If we focus more precisely on the beginning of the

reaction 500 s , t , 1000 s; we can see that it begins

through the thickness of the part.

degree equal to 0.24 an inversion occurs. The reaction

becomes faster in the middle of the piece. The cycle is

well optimized because it anticipates this inversion and

begins cooling before a 0:24: The edges being colder,

the heat released in the center of the piece can thus be

evacuated. This protocol prevents the trapping of residual

stresses in the part.

During the phase of post-curing t . 2300 s the edges

polymerize again more quickly than the heart. However, the

variations in the thickness are negligible because the largest

part of the heat released by the resin polymerization has

already been dissipated.

Optimization made it possible to obtain a realistic cycle.

It must be noted that this cycle would be very difficult to find

by an intuitive method and that it limits the temperature and

state of cure gradients in a part, avoiding the trapping of

residual stresses.

5. Conclusion

Fig. 14. Initial and optimized representation of the mold wall temperature.

of composite material based on an inverse method. It

consists of minimizing a criterion under constraints. In this

paper, this criterion is based on the state of cure, but the

generalization of the method allows to define any specific

criterion depending on the desired objective. The minimization method based on the adjoint state method is described.

704

method to handle realistic situations. The first case

corresponds to a partial uniform state of cure through the

thickness of the part. It was experimentally validated. The

second example is concerned with the control of curing for a

highly reactive polyester resin. A cycle achieving a quasiuniform temperature through the thickness of the part during

curing was found. This cycle is realistic because it is

possible to apply it on an industrial press for which heating

and cooling rates are limited.

Future perspectives of this work concern the use of such

an algorithm with a criterion based on the pressure evolution

in the mold cavity and secondly on the stress distribution

through the thickness of the part. This supposes complicating the model and as a consequence the adjoint equations,

but it seems accessible.

We detail in this appendix the method used to resolve the

inverse problem based on the 1D direct problem described

by the set of Eq. (A1):

T

T

a

A1

rCp a; T

la; T

rDH r

x

t

x

t

a

WhTFa; T

t

with

hT

tind

0

T

exp 2B ref 2 1 dt 2 tref

Tt

Wx 0

if x , 0

Wx 1

if x # 0

T0; x T0 x

dUt

# Vmax

dt

A3

Tx; t # Tmax

ax; tf ad

The Lagrangian L associated to the minimization

problem is introduced by:

La;T;U;Q1 ;Q2

L tf a

2WhTFa;T Q2 dtdx

JU

0 0 t

L t f

T

T

a

2 rDH r

Q1 dtdx

rCp a;T 2

la;T

t x

x

t

0 0

A4

associated to T and a: This Lagrangian may be expressed

by a sum of five integrals: L J A B C D E: In

this expression the function Ut; that we want to determine,

does not appear explicitly because it is a boundary

condition. It appears implicitly in the integral D :

L tf

T

la; T

Q1 dtdx

x

0 x

0

A5

D2

0 , t , tf

0 , t , tf

f 2 x; tdtdx

T

Q

la; T

x 1

dt

L tf

la; T

T Q 1

dtdx

x x

A6

with

tf

2

JU kaU 2 ad k2 gkU 2 Uk

Vmin #

D2

ad x; t and Ut

are given on the intervals 0; tf and

0; L; and g . 0: ad x; t is the state of cure that we want to

reach. We are searching a curing cycle Ut which

minimizes the criterion:

kf k2

Umin # Ut # Umax

0,x,L

a0; x a0 x 0 , x , L

T

Tt; 0 2 Ut

la; T

Rs

x x0

T

Tt; L 2 Ut

la; T

Ri

x xL

L tf

temperature, we impose the constraints given by Eq. (A3).

These constraints are due to the press capacities.

L tf

T Q1

dtdx

la; T

x x

tf T0; t 2 Ut

Q1 0; t

Rs

0

TL; t 2 Ut

Q1 L; t dt

Ri

0

A7

A2

Then, the Lagrangian expression in which Ut appears

explicitly becomes:

La; T; U; Q1 ; Q2

JU

L tf a

0

I1

da

a

2 WhTFa; T Q2 dtdx

L tf

0

la; T

T Q1

dtdx

x x

tf T0; t 2 Ut

Rs

Q1 0; t

TL; t 2 Ut

Q1 L; t dt

Ri

A8

Fa 1 da; T Fa; T 1

La; T; U; Q1 ; Q2 J I1 I2 I3 I4

1 L tf a 1 da

a

2

2 WFa 1 da; T

1!0 1 0

t

t

0

L tf da

WFa; T Q2 dtdx lim1!0

t

0

0

Fa 1 da; T 2 Fa; T

2W

Q2 dtdx

1

A15

lim

L tf

T

r a

2 rDH

rCp a; T

Q1 dtdx

t

t

0 0

A9

see that we have to calculate: L=ada; L=TdT and

L=UdU:

For the determination of the above terms, we have to

derive the Lagrangian (Eq. (A4)) versus a; T and U:

L

L

L

dT

dU

da

a

T

U

A10

L

da

a

J

I

I

I

I

1 2 3 4 da

a

a

a

a

a

I

daQ2 t0f dx 2

L t f Q

2

da dtdx

0

0 t

Q2 x; tf 0

; [ 0; L;

J

1

2

da lim ka 1da 2 ad k2 gkUa 2 Uk

1!0 1

a

L tf Q

I 1

F

da

2 2 2W

Q2 da dtdx

a

t

a

0

0

A13

2rCp

T

a

rDH r X

Q1 dtdx:

t

t

L tf C 2C T

pa

p

r da

lim

2 rDH X

r

Q1 dtdx

1!0 0 0

1

t

t

A20

L tf

J

da 2

a 2 ad da dtdx

a

td

0

A19

a: By definition:

I 2

1 L tf

T

a 1 da

da lim

rCpa 2 rDH r X

1!0 1 0 0

a

t

t

ka 1da 2 ad k2

ka 2 ad k2 21a 2 ad da 12 :kdak2

A18

chosen so that

it comes finally:

A12

A17

L t f da

Q2 dtdx:

0

0 t

by:

2

2 ka 2 ad k2 2 gkU 2 Uk

A16

pose:

A11

F

da Qda2

a

L tf da

I 1

F

2W

da

da Q2 dtdx

a

t

a

0

0

I

dL

705

A14

By definition:

By writing:

Cpa Cp 1

Cp

da Qda2

a

A21

706

We choose Q1 so that

Q1 x; tf 0

; [ 0; L

and we use a procedure similar to the one used for the case

of I1 :

L tf C T

I 2

Q

p

Q1 rDH r X 1 da dtdx

da

r

a

a t

t

0

0

A22

The fourth term of (A11) is the derivative of I3 versus a:

It is obtained by a procedure analogous to the one used for J:

We obtain:

L tf l T Q

I 3

1

da dtdx

da

A23

a

0 a x x

0

L tf

C p T

L

F

dT

Q2 r

Q

2W

T

T

T t 1

0

0

C p Q 1

l T Q 1

2r

t

T x x

Q1

l

2

dT dtdx

x

x

A28

boundary conditions on Q1 :

8

Q1

Q1

>

>

:

;t [ 0; tf

l

>

x0

<

x

Rs

A29

>

Q1

Q1

>

>

:

l

2

;t

[

0;

t

:

f

x xL

Ri

It is not a function of a; so:

have:

I 4

da 0

a

L

dT 0

T

A24

obtained by summing the terms of Eq. (A11):

tf

IL

da 2

a 2 ad dadt

a

td

L tf Q

C p T

F

Q

2 2 2W

Q r

t

a 2

a t 1

0

0

rDH r X

Q 1

l T Q 1

da dtdx

t

a x x

L

da 0

a

;da

A26

C p T

Q 2

F

Q

W

Q1 rDH r X 1

Q2 r

t

a

a t

t

l T Q 1

2a 2 ad

a x x

on td ; tf

Cp T

l T Q1

Q

T t 1 T x x

A31

with

2:l

Q1

Q1 0;t

Q1

Q1 L;t

;t[0;t

l

;t[0;tf

x0

f

xL

x

x

Rs

Ri

U appearing in Eq. (A10). Only two integrals J and I4

depend of U: By a procedure identical with the one used for

a; we obtain:

tf

J

dU 2g U 2 UdUdt

A32

U

0

and:

A27

tf

I4

dU 2

U

0

Q1 0; t

Q L; t

1

dUdt

Rs

Ri

A33

with

(

Cp Q1

F

Q

W

Q2

r

l 1

x

t

T

x

A25

A30

;dT

Q1 x; tf 0

;x [ 0; L

Q2 x; tf 0

;x [ 0; L

appearing in Eq. (A10). By a procedure identical to the one

used for a; we derive all the terms which constitute

the Lagrangian. We obtain the Lagrangian expression

versus T :

tf

L

Q1 0; t

Q1 L; t

dU

2gU 2 U 2

dUdt

Rs

Ri

U

0

A34

We can now express dL from Eq. (A10). Due to the

choice of the adjoint variables Q1 and Q2 which verify Eq.

(7), we have:

L

da 0

a

;da and

L

dT 0

T

;dT;

so:

dL

L

2 Q1 0; t Q1 L; t

dU 2gU 2 U

Rs

Ri

U

A35

direct problem, Eq. (9) gives:

2 Q1 0; t Q1 L; t

7JU 2gU 2 U

A36

Rs

Ri

707

a

WFa; T

t

By substituting Eq. (A41) into (A40), we obtain:

Tm

T

2 Cp

r Cpm

t

t

Tm

T

lm

l

2

x

x

x

x

a m

a

2

rDH r

A42

t

t

adjoint system, we can compute the gradient of the criterion.

By using the conjugate gradient method, we have the

descent direction [8].

a m

a

2

Wm Fm 2 WF

t

t

dn t 27J n t bn d n21 t

da lim

A37

m!0

and

8 1

>

b 0

>

>

>

>

L tf

<

7J n 7J n dtdx

0

0

n

>

>

b L tf

>

>

>

:

7J n21 7J n21 dtdx

0

a 2 am

lim dam

m!0

m

A43

dT lim

m!0

T 2 Tm

lim dTm

m!0

m

;n . 1

Cpm Cp

determine the descent depth. The method is presented in

Appendix B.

lm l

Cp

Cp

dTm Q2 da2m ; dTm2

dam

a

T

A44

l

l

dT Q2 da2m ; dTm2

da

a m T m

Let us write:

Appendix B. Determination of the descent depth m

U n1 t U n t mn dn t

A40

a m

a

2

t

t

am

a

2

t

t

E Wm Fm 2 WF

T

T

a

l

rDH r

x

t

x

t

C rDH r

am

Wm Fm

t

rCp

Tm

T

lm

l

B

2

x

x

x

x

A39

problem, and to U m dU correspond the solutions Tm and

am So, Tm and am are solutions of:

Tm

Tm

am

rCpm

lm

rDH r

x

t

x

t

A45

A38

defined such as J is a minimum at the iteration n 1: For a

given iteration, J is a function of m :

2

Jm kaU m dU 2 ad k2 gkU m dU 2 Uk

Tm

T

2 Cp

A r Cpm

t

t

A41

We have:

Cp

Cp

A

dT

T

r

dT

lim

rCp

da

m!0 m

t

a

T

t

A46

dT

l

l

T

:

l

da dT

m!0 m

x

x a

x

T

x

A47

lim

708

lim

m!0 m

rDH r

da

t

A48

D da

m!0 m

t

A49

lim

E WF

WF

lim

dT

da

A50

m!0 m

T

a

To completely determine the sensitivity of the system,

we consider the initial and boundaries conditions.

for t 0 we have:

dax; 0 dTx; 0 0

;x [ 0; L

at x 0 we have:

dT

l

l

T

dT 2 dU

dT

l

da

Rs

x

a

T

x

at x L we have:

dT

l

l

T

dT 2 dU

dT

2

l

da

Ri

x

a

T

x

da

t

tf

U 2 Uddt

tf

0

dddt

tf L

td

tf

0

L

td

a 2 ad dam dxdt

A61

da da dxdt

References

A53

A54

A55

A56

2

JU md ka m da 2 ad k2 gkU md 2 Uk

2ma 2 ad da

ka 2 ad k2 gkU 2 Uk

A57

JU md f m a 2b:m c:m2

A60

positive, so c is also positive. Finally, the depth of descent is

given by:

m2

and:

2gmU 2 U:

b

c

A52

the system (A54). We have then:

am ax; t; U md ax; t; U m da

m2

da

WF

WF

dT

da

t

a

T

2

JU md kam 2 am k2 gkU md 2 Uk

A59

Then we have:

A51

C p

Cp

dT

T

r

dT

rC p

da

t

a

T

t

dT

l

l

T

dT

l

da

x

x a

x

T

x

rDH r X

df m

2b 2cm 0

dm

A58

of f(m) versus m:

residual stress development during cure. J Compos Mater 1992;26:16.

[2] Millischer A, Delaunay D, Jarny Y. Thermomechanical coupling in

B.M.C. injection process: characterization, modelization and experimental validation. Third Can Int Conf Compos (CANCOM Montreal

August 2001.

[3] Antonucci V, Giordano M, Hsiao KT, Advani SG. A methodology to

reduce thermal gradients due to the exothermic reactions in

composites processing. Int J Heat Mass Transfer 2002;45:1675 84.

[4] Ruiz E, Trochu F. Analysis of thermal residual stresses during the

curing of composites parts manufactured by Resin Transfer Molding.

Third Can Int Conf. Compos (CANCOM Montreal August 2001.

[5] Bailleul J-L, Delaunay D, Jarny Y, Jurkowski T. Thermal conductivity of unidirectional reinforced composite materials: experimental

measurement as a function of state of cure. J Reinforced Plast Compos

2001;20:5264.

[6] Kamal MR, Sourour S. Kinetics and thermal characterization of

thermoset cure.”. Polym Engng Sci 1973;13(1).

[7] Bailleul J-L, Delaunay D, Jarny Y. Determination of temperature

variable properties of composite materials: methodology and

experimental results. J Reinforced Plast Compos 1996;15:47996.

[8] Jarny Y. In: Woodbury KA, editor. The adjoint method to compute the

numerical solutions of inverse problems. Inverse engineering handbook, Boca Raton, FL: CRC Press; 2002.

[9] Bailleul J-L. Optimisation du cycle de cuisson de pie`ces epaisses en

materiau composite. Application a` un preimpregne resine epoxyde/

fibres de verre. The`se de Doctorat de lUniversite de Nantes

[10] Hasselman DPH, Donaldson KY, Thomas JR. Effective thermal

conductivity of uniaxial composite with cylindrically orthotropic

carbon fibers and interfacial thermal barrier. J Compos Mater 1993;

27(6):63744.

[11] Benveniste Y, Chen T, Dvorak GL. The effective conductivity of

composites reinforced by coated cylindrically orthotropic fibers.

J Appl Phys 1990;67:2878 84.

[12] Bailleul J-L, Delaunay D, Jarny Y. Optimal thermal processing of

composite materials: an inverse algorithm and its experimental

validation. Proceedings of 11th IHTC, vol. 5, Kyongju, Korea, August

23 28, 1998. p. 8792

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