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**mechanical responses of the ®bre/matrix interface
**

Mondher Zidi

a,c

, Luc Carpentier

a

, Antoine Chateauminois

b,

*,

Ph. Kapsa

a

, FrancË ois Sidoro

a

a

Laboratoire de Tribologie et Dynamique des SysteÁ mes, UMR CNRS 5513, Ecole Centrale de Lyon, BP 163, 69131 Ecully Cedex, France

b

Laboratoire d'IngeÂ nierie et Fonctionnalisation des SysteÁ mes, UMR CNRS 5621, Ecole Centrale de Lyon, BP 163, 69131 Ecully Cedex, France

c

Laboratoire de MeÂ canique des Solides, Ecole Nationale d'IngeÂ nieurs de Monastir, Avenue Ibn Eljazzar, 5019 Monastir, Tunisia

Received 16 July 1999; received in revised form 22 November 1999; accepted 16 May 2000

Abstract

An analytical shear-lag model has been developed for quantifying the interfacial shear strength of glass-reinforced composites

from micro-indentation experiments. The model takes into account the local ®bre environment, together with the occurrence of

debonding and ®bre sliding. In order to simulate the experimental indentation curves, various interfacial laws have been imple-

mented. In a ®rst approach, it was assumed that the shear stress in the debonded part of the interface was constant and propor-

tional to the debonding stress. A more re®ned generalised interface law relating the shear stress to the ®bre displacement was

subsequently introduced to describe a progressive transition from an adhesive to a sliding state. The model has been successfully

applied to the analysis of experimental reduced indentation curves giving the displacement of the ®bre surface as a function of the

applied load. #2001 Elsevier Science Ltd. All rights reserved.

Keywords: Micro-indentation; Shear lag; Glass/epoxy composites; Interface law; Fibre/matrix debonding

1. Introduction

The durability of polymer-matrix composites under

mechanical and environmental loading is known to be

strongly dependent upon the strength of the ®bre/matrix

interface. As a result, many methods based on both

macro- or micro-mechanical tests have been developed for

measuring the level of adhesion at the interface [1]. Among

the many micro-techniques for interfacial property char-

acterisation, the micro-indentation test is very attractive

because it is an in-situ testing method conducted on real

composites, thus allowing for evaluation of the proces-

sing or environmental conditions encountered either

during manufacturing or service. Initially introduced by

Mandell et al. [2,3], this test consists in indenting a sin-

gle ®bre in the polished cross-section of a composite

specimen until the occurrence of interfacial debonding.

The corresponding debonding load is generally identi®ed

either from the force/displacement curves or from speci®c

procedures involving microscopic observations after

testing at increasing indentation loads [4±7].

The derivation of the interfacial shear strength from

the measured debonding load is, however, complicated

by the highly heterogeneous stress ®eld induced by the

indenter. From parametric ®nite-element studies, Ho et

al. [8] and Mandell et al. [3] have also demonstrated that

the local ®bre arrangement can strongly aect the per-

turbed stress ®eld around the indented ®bres. As a

result, the scatter in the local ®bre packing can result in

very dierent debonding loads. In order to overcome

these diculties, Mandell and co-workers proposed a

data reduction scheme based on a linear axi-symmetric

®nite-element analysis. In a ®rst step, the experimental

debonding loads need to be shifted to an adjusted value

for a given ratio t

m

,d

f

, where t

m

is the average matrix

thickness between the tested ®bre and its nearest neigh-

bours and d

f

is the ®bre diameter. The interfacial shear

strength is subsequently calculated from this adjusted

debonding load using a maximum shear stress criterion

0266-3538/01/$ - see front matter # 2001 Elsevier Science Ltd. All rights reserved.

PI I : S0266- 3538( 00) 00123- 8

Composites Science and Technology 61 (2001) 369±375

www.elsevier.com/locate/compscitech

* Corresponding author. Tel.: +33-4-72-18-6453; fax: +33-4-78-

33-1140.

E-mail address: antoine.chateauminois@ec- lyon.fr (A. Chateaumi-

nois).

and the results of the ®nite-element analysis. The use of

this procedure is, however, complicated by the ambi-

guities surrounding the experimental determination of

t

m

in the real non axi-symetric con®guration.

Alternative methods based on mono-dimensional

shear lag models have also been used to analyse micro-

indentation data. Although these approaches imply very

crude assumptions [9,10], the resulting analytical rela-

tionships are very appropriate for the systematic identi®-

cation of parameters from experimental data. This latter

point is especially relevant in the ®eld of micro-inden-

tation tests, where the large data scatter requires the

statistical analysis of many experiments. In a previous

study [11,12], the present authors have derived and

validated by ®nite-element modelling (FEM) simula-

tions such a model for polymer matrix composites. This

model incorporates to main features:

1. the local environment around the tested ®bre is

taken into account through a single parameter,

which is calculated directly from the experimental

elastic stiness of the indented system.

2. the identi®cation of the debonding load is based

on a ®tting of the entire loading curve, instead of

the identi®cation of an always dubious threshold

for debonding.

In order to ful®l this last requirement, it was neces-

sary to incorporate into the model the possibility of

®bre sliding in the debonded part of the interface. In a

®rst approach, this was done by considering that the

interface obeyed a very simple Tresca criterion. The

interfacial shear stress in the debonded area was thus

assumed to be constant and equal to the debonding

stress. This model provided a satisfactory description of

the micro-indentation curves obtained using unidirec-

tional glass/epoxy composites [12]. Some limitations in

the application of the model were, however, encoun-

tered with other systems such as glass/polyester compo-

sites [11]. From scanning electron microscopy (SEM)

observations of the indented ®bres, the latter were rela-

ted to changes in the debonding mechanisms. This indi-

cated the need of further re®nements of the interface

law, in order to take into account the dierent debond-

ing behaviour observed experimentally.

The objective of this paper is therefore to present

some theoretical developments of the micro-indentation

model, which include more re®ned interface laws. The

ability of various interface laws to describe dierent kinds

of micro-indentation curves is especially considered.

Experimental results are provided in order to demon-

strate the potential of the theoretical model for the

simulation of dierent experimental indentation responses.

The systematic analysis of micro-indentation data using

these models will, however, be considered in a further

companion paper.

2. Background

2.1. Extraction of reduced indentation curves

The micro-indentation experiments provide raw

indentation curves giving the applied load as a function

of the overall displacement of the indenter. As a con-

sequence of the compliance of the polymer matrix, it is,

however, very dicult to accurately detect the debonding

load from such a curve. To overcome this problem, a

data reduction scheme has been proposed, which is

based on the removal of the displacement component

u

ep

caused by the elasto-plastic indentation of the ®bre

surface by the indenter. This later contribution was

assessed from micro-indentation tests carried out using

bulk-glass specimens whose chemical composition is the

same as for the ®bres. Full details regarding the develop-

ment of this procedure and its validation by means of

FEM simulations can be found in Refs. [5,11]. The sub-

traction of u

ep

from the overall displacement results in a

so-called reduced indentation curve giving the applied

load as a function of the displacement of the ®bre surface

only. These reduced curves contain all the useful infor-

mation regarding the analysis of the interfacial behaviour.

Depending on the magnitude of the applied load, the

reduced indentation curves can exhibit either a linear

elastic behaviour (at low loads) or a non-linear response

(at high loads) during loading (Fig. 1). By systematic SEM

and optical microscope observation of the ®bres after

indentation, it was established that the non-linear beha-

viour is associated to ®bre/matrix debonding (Fig. 2).

Some limitations were encountered in the ®ltering of

the experimental indentation behaviour of bulk glass at

low loads (P< 50 mN) during the unloading step. As a

result, the corresponding part of the reduced indentation

curve was not reliable and is not represented in Fig. 1 and

in all the subsequent ®gures showing reduced curves.

2.2. Basic equations used to model the reduced

indentation curves

In order to analyse the reduced indentation curves, a

mono-dimensional shear-lag model has been developed.

This model is able to simulate the loading and unloading

steps of the indentation experiments, while taking into

account interfacial debonding. The occurrence of

debonding is predicted by means of a maximum shear-

stress criterion. The model in its basic con®guration has

been fully detailed elsewhere [11,12] and only the basic

assumptions and equations will be recalled here.

An axi-symmetric con®guration with a single ®bre

(radius a) embedded in a polymer matrix is considered

(Fig. 3). The displacement, u x ( ), of the ®bre is supposed

to be uniform in a given cross-section. This assumption

allows treating the problem as mono-dimensional.

Radial and axial stresses as a result of residual curing

370 M. Zidi et al. / Composites Science and Technology 61 (2001) 369±375

stresses and Poisson's eects are not taken into account.

Boundary conditions are established by considering that:

i. the axial stress, o

0

, on the ®bre surface is uniform

and related to the applied load P through:

o

0

=

P

¬a

2

. (I)

ii. the displacement and the axial stress in the ®bre

decrease when the depth is increased (the specimen

thickness is much greater than the ®bre diameter), i.e.:

u ÷ 0Y o ÷ 0Y for x ÷ o (P)

Elastic equilibrium conditions in the ®bre are written

as follows:

do

dx

= ÷

2t

a

(Q)

where t is the interfacial shear stress. From Hooke's law

for the ®bre, the following equation can be written:

du

dx

= ÷

o

E

(R)

The interfacial shear stress, t x ( ), is assumed to be linearly

related to the displacement, w x ( ), of the matrix for r = a,

i.e.:

t = kw (S)

where k is a global stiness constant including the elastic

properties of the ®bre and the matrix, together with the

local ®bre environment.

By combining Eqs. (3) and (4), the following equili-

brium relationship can be written:

d

2

u

dx

2

÷

2t(x)

aE

= 0 (T)

when u = w, i.e. before local sliding, Eq. (6) reduces to:

d

2

u

dx

2

÷n

2

u = 0 (U)

with

n =

2k

aE

_

(V)

Fig. 2. SEM picture of an indented glass ®bre showing the occurrence of

debonding (glass/epoxy unidirectional composite, peak load 0.2 N).

Fig. 1. Typical reduced indentation curves showing either (a) a linear

behaviour (below the debonding load) or (b) a non-linear behaviour

(above the debonding load). Solid line in (b): theoretical curve using

Eqs. (10)±(12). (glass/epoxy system, indentation speed 0.2 mm s

÷1

).

Fig. 3. Geometry of the shear-lag model.

M. Zidi et al. / Composites Science and Technology 61 (2001) 369±375 371

After the onset of debonding, it becomes necessary to

take into account a debonded length, h, where t x ( ) is

de®ned by the interface law. In the basic version of the

model, an expression relating the stress t to the relative

displacement v x ( ) = u x ( ) ÷w x ( ) between the ®bre and

the matrix was considered. It was at ®rst assumed that

the shear stress was constant and equal to the shear

strength, t

d

, in the debonded area. The corresponding

interface law can thus be expressed as follows:

t = t

d

dv

dv [ [

(W)

From knowledge of the interface law, Eqs. (6) and (7)

can be solved using the appropriate set of boundary

conditions. Accordingly, the displacement, u

o

, of the

®bre surface can be expressed as a function of the

applied stress, o

0

:

a. during loading

u

o

=

o

0

nE

for o

0

- o

d

(IH)

where o

d

is the applied axial stress at the onset of

debonding.

u

0

=

1

2nE

o

2

0

o

d

÷o

d

_ _

for o

0

> o

d

(II)

b. during unloading

During unloading, the model can simulate the occur-

rence of sliding in the debonded part of the ®bre, when

the applied axial stress is less than a limiting value, o

g

.

For the studied glass/thermoset systems and the con-

sidered interface law, the calculation predicted that such

a sliding would require negative loads, i.e. a pull-out

con®guration[12]. As a result, only the purely elastic

response will be considered herein:

u

0

=

1

2nE

o

2

mx

o

d

÷o

d

÷2 o

0

÷o

mx

( )

_ _

(IP)

where o

mx

is the maximum load applied during loading.

The model requires the identi®cation of two para-

meters, namely n and the debonding load P

d

= o

d

¬a

2

.

The former coecient is measured from the slope of the

initial elastic part of the loading curve [cf. Eq. (10)]. It

provides some information regarding the local environ-

ment of the tested ®bres: n is increased, i.e. the global

stiness of the system is increased, when the local ®bre

packing is enhanced. The value of the debonding load is

identi®ed by a least-square ®tting of the experimental

loading curve using expressions (10) and (11). The

interfacial shear strength is subsequently calculated

using the following expression:

t

d

=

nP

d

2¬a

(IQ)

Fig. 1(b) shows an example of the application of the

model to an experimental reduced indentation curve

obtained using an E-glass/epoxy system. It can be seen

that the linear response during unloading is consistent

with the assumption of a purely elastic response of the

system during this stage.

3. Improved interfacial laws

The model presented above is based on a very crude

assumption regarding the interfacial behaviour. It

proved, however, to give realistic values of the interfacial

shear strength (in the order of 70 MPa) for a wide range

of glass/epoxy systems [11]. With some other systems,

such as glass/polyester composites, it appeared, how-

ever, that the theoretical expressions were unable to ®t

the experimental indentation curves. This was observed

especially when a poor interfacial strength led to a pre-

mature and extensive debonding. These processes are

often associated with a `kink' in the reduced indentation

curve at the end of the linear stage, probably caused by

the debonding instability (Fig. 4). Above this critical

point, the displacement u

0

of the ®bre surface occurred

generally to a greater extent than for the glass/epoxy

systems. In addition, a non-linear behaviour, probably

associated with the occurrence of sliding, was also

observed during unloading. The theoretical curve

obtained using the initial version of the model with the

experimental data reported in Fig. 4 is also shown. This

result clearly demonstrates the inability of Eqs. (10)±

(12) to describe the experimental behaviour. Improved

interfacial laws were thus introduced to reproduce the

experimental response.

Fig. 4. Reduced indentation curve obtained using a glass/polyester

system (0.2 mm s

÷1

)., (*) experimental data; solid line, theoretical

curve using t

g

= ot

d

[Eqs. (16)±(18), o = 0.27, t

d

= 123 MPa, n = 0.04

mm

÷1

); dashed line, theoretical curve using t

g

= t

d

[Eqs. (10)±(12),

t

d

= 65 MPa, n = 0.04 mm

÷1

).

372 M. Zidi et al. / Composites Science and Technology 61 (2001) 369±375

3.1. Interface law including a sliding stress dierent

from the debonding stress

In the basic con®guration of the model, it was

assumed that the shear stress in the debonded area is

constant and equal to the debonding strength. It is

physically more realistic to consider that the transition

from an adhesive to a sliding state is associated with

a change in the interfacial stress. In a ®rst approach, it

was assumed that sliding occured at a constant stress,

t

g

, proportional to t

d

:

t

g

= ot

d

o - 1 (IR)

From Eq. (6), the equilibrium relationship in the

debonded area can be written as follows:

d

2

u

dx

2

÷

2t

g

aE

= 0 04x4h (IS)

Solving Eq. (15) together with Eq. (7) gives:

a. During loading

. for o

0

- o

d

, the elastic response of the system is

still given by Eq. (10),

. for o

0

5o

d

:

u

0

=

a

4Et

g

o

2

0

÷o

2

d

_ _

÷

o

d

nE

(IT)

b. During unloading

Two separate situations may be considered, depending

on whether the stress is greater or less than the stress,

o

g

, at the onset of sliding in the debonded part of the

interface:

. for o

0

5o

g

u

0

= u

mx

(0) ÷

o

mx

÷o

0

nE

(IU)

. for o

0

4o

g

u

0

= u

mx

(0) ÷

a

8Et

g

o

mx

÷o

0

( )

2

÷

2t

g

an

2

E

_ _

(IV)

where o

mx

and u

mx

0 ( ) are, respectively, the maximum

axial stress and the maximum displacement reached on

the ®bre surface (x = 0) during the loading step. The

stress, o

g

, at the onset of the sliding in the debonded

part of the ®bre is given by:

o

g

= o

mx

÷2oo

d

(IW)

It can be noted that the initial version of the micro-

indentation model [Eqs. (10)±(12)] is a limit case of this

model, when the value of o is set to 1.

As an example, the parameters of the model have

been identi®ed using the experimental data reported in

Fig. 4. The value of the parameter n was obtained from

the measurement of the slope of the initial linear part of

the loading curve. The values of o and P

d

were simul-

taneously obtained by an iterative least-square ®tting

technique using the data points of the entire reduced

indentation curve. The obtained value of the sliding

stress t

g

is signi®cantly lower that the debonding stress,

namely 0.21t

d

. It can also be noted that the modi®ed

interface law is able to simulate the non-linear behaviour

associated to the sliding of the ®bre during unloading,

which is not the case for the initial version of the shear-

lag model.

The capability of the model to describe various

experimental indentation curves has thus been enhanced

by considering that t

g

= ot

d

. This interface law relies,

however, on the assumption that the transition from an

adhesive to a sliding state occurred in a discrete way at the

interface. In the reduced indentation curve, this feature

results in a sharp kink when the applied load P reaches

the debonding load (see Fig. 4). This is not very realistic

from a physical point of view, and an interface law simu-

lating a more progressive debonding will be considered in

the subsequent section.

3.2. Generalised interfacial law

In order to describe a progressive interfacial debonding,

Needleman [13], Tvergaard [14] and Raous et al. [15]

have introduced various interface models that relate non-

linearly the normal and tangential tractions to the

corresponding displacement discontinuities. These models

require heavy ®nite-element simulations and are there-

fore not suitable for the systematic analysis of experi-

mental data. In this study, a similar but simpli®ed

approach was proposed. Instead of relating the inter-

facial shear stress to the relative displacement, v x ( ), in

the debonded portion of the ®bre [cf. Eq. (9)], a gen-

eralised interface law considering the ®bre displacement

only was introduced. The following expression has been

proposed:

t = t

d

u

h

u

_ _

[

(PH)

where u

h

is the ®bre displacement at the end of the

debonded area (x = h) and [ is a parameter which

allows to describe dierent interfacial response (Fig. 5).

By varying the value of [ between 0 and o, it is possible

to simulate debonding processes occurring in an inter-

mediate way between a perfectly plastic and a brittle

behaviour. When [ = 0, the generalised interface model

is equivalent to the basic model [Eqs. (10)±(12)].

M. Zidi et al. / Composites Science and Technology 61 (2001) 369±375 373

By replacing (20) in Eq. (6), we obtain:

d

2

u

dy

2

÷

2t

d

aE

u

h

u

_ _

[

= 0 (PI)

with the following boundary conditions:

du

dy

(0) =

2t

d

anE

. u(0) = u

0

=

2t

d

aEn

2

(PP)

where y = x ÷h.

By considering the variable z = du,dy, the problem

can be solved from the following set of equations:

z

/

=

2t

d

aE

u

h

u

_ _

[

. u

/

= z (PQ)

z(0) =

2t

d

anE

. u(0) =

2t

d

aEn

2

(PR)

The problem can no longer be solved analytically, but

a numerical resolution is easily obtained. As an example,

a theoretical loading curve has been reported in Fig. 6,

together with the corresponding experimental data. The

®tting procedure provided a value of [ equal to 1.4 and

70 MPa for t

d

. The positive value of [ could indicate

that the elastic properties of the interface are progres-

sively lowered during the debonding process.

4. Conclusion

A mono-dimensional shear-lag model has been devel-

oped for the analysis of experimental micro-indentation

data obtained using dierent glass-®bre-composite sys-

tems. In order to simulate various kinds of indentation

responses, dierent interface laws have been imple-

mented in the model. A simple approach considering

that the shear stress in the debonded area is constant

and proportional to the debonding stress has proven to

be suitable to describe the experimental behaviour of

composite materials with poor interfacial properties. A

more physically realistic interface law taking into

account the progressive debonding of the interface was

also introduced. At the expense of some numerical

computations, this latter approach allowed us to

describe a wide range of indentation responses through

the identi®cation of two interface parameters.

Whatever the interface law considered, the key features

of the model were retained, namely:

1. the ®bre local environment is globally taken into

account through the measurement of the elastic

stiness of the system,

2. the debonding load is determined from the whole

loading curve and not from the identi®cation of a

decohesion threshold.

Acknowledgements

The authors wish to thank the ReÂ gion RhoÃ ne-Alpes

and the CMCU (ComiteÂ Mixte de CoopeÂ ration Uni-

versitaire Franco-Tunisien) for ®nancial support. Many

thanks are also due to IFREMER (Brest, France) for

providing materials and ®nancial support.

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