Development of a micro-indentation model simulating di€erent

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'Inge nierie et Fonctionnalisation des SysteÁ mes, UMR CNRS 5621, Ecole Centrale de Lyon, BP 163, 69131 Ecully Cedex, France
c
Laboratoire de Me canique des Solides, Ecole Nationale d'Inge 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 a€ect the per-
turbed stress ®eld around the indented ®bres. As a
result, the scatter in the local ®bre packing can result in
very di€erent debonding loads. In order to overcome
these diculties, 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 sti€ness 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 di€erent 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 di€erent 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 di€erent 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 dicult 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 e€ects 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 sti€ness 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
m—x
o
d
÷o
d
÷2 o
0
÷o
m—x
( )
_ _
(IP)
where o
m—x
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 coecient 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
sti€ness 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 di€erent
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
m—x
(0) ÷
o
m—x
÷o
0
nE
(IU)
. for o
0
4o
g
u
0
= u
m—x
(0) ÷
a
8Et
g
o
m—x
÷o
0
( )
2
÷
2t
g
an
2
E
_ _
(IV)
where o
m—x
and u
m—x
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
m—x
÷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 di€erent 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 di€erent glass-®bre-composite sys-
tems. In order to simulate various kinds of indentation
responses, di€erent 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
sti€ness 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 Re gion Rhoà ne-Alpes
and the CMCU (Comite Mixte de Coope 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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