Composites Science and Technology 53 (1995) 41 l-421

0 1995 Elsevier Science Limited

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ELSEVIER 0266-3538(95)00030-S 0266-3538/95/$09.50

ANALYSIS OF THE SINGLE-FIBRE PULL-OUT TEST BY

MEANS OF RAMAN SPECTROSCOPY: PART II.
MICROMECHANICS OF DEFORMATION FOR AN
ARAMID/EPOXY SYSTEM

D. J. Bannister, M. C. Andrews, A. J. Cervenka* & R. J. Young$

Manchester Materials Science Centre, UMIST/University of Manchester, Grosvenor Street, Manchester, UK, Ml 7HS

(Received 23 September 1994; revised version received 6 January 1995; accepted 27 January 1995)

Ffrict
Abstract Original frictional pull-out force
,$,,
The single-fibre pull-out test has been analysed for Maximum pull-out force
Kevlar-49 fibres in a cold-cured epoxy resin by using L Fibre embedded length
both a conventional pull-out experiment and Raman Lf Free length of fibre outside the resin block
spectroscopy. The interfacial shear strength (ISS) has Lcrit Stable/unstable debonding transition point
max
been estimated from the pull-out force for fibres with a L Maximum embedded fibre length that can
range of embedded lengths. Raman spectroscopy has be ‘pulled-out’ of the resin
been used to analyse the distribution of ftbre strain in m Bonded/debonded transition point
the pull-out test by mapping the variation of strain Fibre radius
along an aramid fibre undergoing pull-out from the ‘R Effective radius of the interface
epoxy resin matrix. At low strains the behaviour S Fibre aspect ratio
follows elastic shear-lag analysis but, as the jibre strain Ef Fibre tensile strain
is increased, debonding takes place at the fibreimatrix 6 Ultimate fibre tensile strain
interface. It is found that this debond propagates along E
aPP
Strain applied to free end of fibre
bon
the interface until the entire fibre is debonded. The fibre Ef Contribution to fibre strain from bonded
is then pulled out of the resin matrix by a frictional region
deb
pull-out process. It is shown that the conventional Ef Contribution to fibre strain from debonded
pull-out experiment produces only an apparent value of region
max
ISS and that through a partial-debonding model it is Ef Maximum theoretical pull-out strain
tot
possible to use the interfacial parameters obtained from Ef Total theoretical strain due to both bonded
the Raman analysis to predict the data from the and debonded regions
conventional test. yrn Matrix Poisson’s ratio
Uf Fibre tensile stress
tot
Keywords: composites, Raman spectroscopy, pull-out Uf Total theoretical stress owing to both
test, interfacial properties, interfacial debonding, in- bonded and debonded regions
terfacial friction Interfacial shear stress
Mean apparent interfacial shear strength
Interfacial debonding shear stress
Interfacial frictional shear stress
NOMENCLATURE
Maximum interfacial shear stress
Interfacial shear strength
Ef Fibre tensile modulus Shear yield stress of the matrix
& Matrix tensile modulus
Fp Tensile force on free end of fibre
Fdrb
Debonding force 1 INTRODUCTION
P

It is widely acknowledged that the fibre/matrix

* Also at Koninklijke/Shell-Laboratorium, Amsterdam, interface influences the properties of fibre-reinforced
The Netherlands. polymer composites. In general, fibre-reinforced
$ To whom correspondence should be addressed. composites should possess a good interfacial shear
411
412 D. J. Bannister et al.
strength, z,, that is dependent upon the fibre surface
properties and the mechanical properties of the fibre
and matrix. Several test methods have been developed
for the evaluation of z, including fibre
fragmentation,le3 push-out or indentation,4 and the
single-fibre pull-out test.5.6 The different techniques
yield different results and correlations between them
are often poor.7,8 The single-fibre pull-out test is,
however, a method commonly employed for the
determination of the interfacial parameters because of
its simplicity and versatility.
In part I of this study’ Raman spectroscopy was
used to analyse the distribution of fibre strain in the
single-fibre pull-out test by mapping the variation of
strain along aramid fibres undergoing pull-out from an
epoxy resin matrix. Both sized and de-sized aramid
fibres were used with room-temperature and high-
temperature cured resins. In all cases specimens were
investigated that contained embedded fibres that
spanned the width of the resin block (at least 3 mm).
At low strains, the behaviour followed conventional
shear-lag analysis, but as the fibre strain was
increased, yielding was also thought to have taken
place in the resin at the fibre/matrix interface. It was
found that failure eventually took place by either
fibre/matrix debonding or fibre fracture outside the
resin matrix.
This study uses Raman spectroscopy to quantify the
strain distribution along a Kevlar fibre, of embedded
length -1000 pm, undergoing pull-out from an epoxy
resin matrix. The process is also analysed theoretically
by using a modified theory that combines conventional
shear-lag analysis’” and debonding theories.” This
theory is used to model both the partially debonded
single fibre undergoing pull-out and the data from a
number of mechanical pull-out experiments on
specimens with a variety of embedded fibre lengths
(cl500 pm).
2 EXPERIMENTAL PROCEDURE
2.1 Materials
The fibre used in this study was a commercial grade of
aramid fibre, Kevlar-49, supplied by E. I. Du Pont de
Nemours, Central Research, Wilmington, USA. The
fibres had been sized during processing to improve
both the handling characteristics and matrix adhesion
in composites. The same type of fibre was used in the
previous study,’ with a diameter of -12 pm, a tensile
modulus of about 120 GPa, a tensile strength of
-2.6 GPa and a strain-to-failure of about 2.2%
The matrix material was a two-part, cold-curing
epoxy resin consisting of 100 parts by weight of
butane-1,4-diol diglycidyl ether resin (LY5052) and 38
parts by weight of isophorone diamine hardener
(HY5052), both obtained from Ciba Geigy. This was
again the same type of resin as was used before.’ It
has a Young’s modulus of about 3 GPa and a shear
yield stress of -43 MPa.
2.2 Preparation of single-fibre pull-out specimens
(SFPO)
The SFPO specimens were prepared in silicone rubber
moulds approximately 10 mm X 10 mm X 3 mm, as
described elsewhere.’ A segment of the rubber,
approximately 5 mm X 5 mm, was removed from the
centre of the mould with an adapted razor blade. A
2 mm deep razor cut was made in one side of the
mould wall. The mould was flexed to open the cut to
allow the introduction of a fibre and then released to
grip the fibre. The desired embedded length was
obtained by drawing the fibre through the cut. The
cavity was filled with epoxy resin that was cured at
room temperature (22 f 2’C) for 7 days. After curing,
the sample was carefully removed by manipulation of
the mould.
Optically flat smooth surfaces of the specimens were
obtained by placing the individual mould on release
paper on glass slides. A smooth top surface combined
with a sharp 90” corner between the top and the side
surfaces were essential in the production of good
Raman spectroscopy specimens. The optically sub-
standard specimens were adequate for the mechanical
pull-out tests. Specimens were prepared with a range
of embedded lengths from 100 pm to 1500 pm and a
free-fibre length of approximately 40 mm.
2.3 Raman spectroscopy
The SFPO specimens were fixed individually to small
glass slides with the free-fibre length cemented
between two small pieces of card.” The specimens
were mounted on a ‘Minimat’ miniature materials
straining rig (Polymer Laboratories, UK), which was
subsequently placed on the stage of an Olympus BH-2
optical microscope connected via a spatial filter
assembly to a Spex 1OOOM single monochromator.
Raman spectra were obtained from the aramid fibres,
both in air and within the epoxy resin, using the
632.8 nm red line of a 15 mW helium-neon laser
focused to a 5 pm spot on the surface of the fibre. A
highly sensitive Wright Instruments charge-coupled
device (CDD) camera was used to collect Raman
spectra using an exposure time of 7 s. The peak
position of the strain-sensitive 1610 cm-’ Raman
band’ was used to map the fibre strain profiles at
various levels of applied strain.
2.4 Mechanical pull-out tests
Specimens unsuitable for Raman spectroscopy were
examined by optical microscopy to determine the
embedded length of the fibre to *lo pm. The
specimens were subsequently tested to failure in ah
 Analysis of the single-fibre pull-out test 413

Instron 1121 tensile testing machine at a cross-head types of curve are commonly observed (Fig. l(a)-(c)).
speed of 1 mmfmin-’ and with a full scale load of 1 N. In the first case (Fig. l(a)), for very strongly-bonded
All tests were performed in a temperature-controlled interfaces or weak interfaces where the embedded
room at 23 f 1°C and 50 f 2% relative humidity length is very small, the stored energy within the
(RH). For each individual specimen the system is high enough to extract the fibre immediately
load/displacement curves were recorded and conse- after the initiation of interfacial failure, and only the
quently the maximum pull-out force, Fy’, was maximum force during pull-out can be recorded. If the
obtained directly. testing guidelines outlined above are implemented,
the second type of curve (Fig. l(b)) may be
obtained,13 although it is more commonly observed
3 CONVENTIONAL ANALYSIS OF PULL-OUT
with weakly bonded interfaces. In this case, after
The shape of the force/displacement curves obtained interfacial failure, the fibre may be extracted
from the pull-out test depends ultimately on the progressively and frictional pull-out monitored until
intrinsic characteristics of the interface and on the final failure. Such data yield not only the maximum
dynamics of the test. It has been pointed out” that pull-out load but also the frictional load on the fibre.
there is a sudden release of strain energy stored in the The third type of curve (Fig. l(c)) has been observed
free part of the fibre under tension where the interface by Penn and LeeI for Kevlar/epoxy, and by Takaku
fails. The elastic contraction may result in the full and Arridge” with steel/epoxy single-filament model
extraction of the fibre from the resin. Pull-out tests are composites. Penn and Lee attributed the peaks in the
usually performed at a constant displacement rate and ascending region of the force/displacement curve to
therefore the stiffness of the mechanical load train damage caused by friction as the debonded region
should also be considered. As a result, it is develops along the fibre/matrix interface. Takaku and
suggested”.‘* that the free length of the fibre should Arridge, however, proposed a step-wise debonding
be kept to a minimum and the loading apparatus phenomenon.
should be as stiff as possible. The pull-out test is analysed conventionally from
In general, for brittle fibre/resin systems, three the relationship between the maximum pull-out load,
F r, and the embedded length, L,. Figure 2 shows
Force typical pull-out data, obtained using a tensile testing
machine, for our Kevlar-49/epoxy system with a
variety of embedded lengths. Early analysis of this
type of data16 assumed a yielding interface that would
allow the shear stress distribution along the
fibre/matrix interface to be approximated as a
constant, raa,which is defined through the simple force
balance equation
Displacement
Fr = 2mL, z, (1)
Force
I for a fibre of radius, r. The determination of r, from
the experimental data in this manner ignores stress

Displacement

Force
.. B

Embedded Length. L.(w)

Fig. 2. Experimental data for the dependence of the

Fig. 1. Schematic illustrations of possible force/ pull-out force, Fy, upon embedded length for the
displacement curves for the single-fibre pull-out test. Kevlar-49/epoxy system investigated.
414 D. J. Bannister et al.

concentrations and is therefore normally referred to as the fibre aspect ratio L,/r. The corresponding
a ‘mean apparent interfacial shear strength’.” interfacial shear stress is obtained from the considera-
Applying this approach to the data in Fig. 2 yields tion of the equilibrium of forces exerted on a
r, = 10 MPa. differential fibre element of length d_~:~”
The analysis of the pull-out test by Greszczuk’*
recognises the distribution of shear stress along the 2=E de,:
embedded region of the fibre as being non-uniform fdx2
and assumes the maximum force during pull-out is Differentiation of eqn (4) and substitution into eqn (5)
obtained at the initiation of debonding (Fr’ = ,F”) yields:
and that subsequent debonding will be unstable. The
theory therefore is applicable only to strongly bonded
interfaces and for a particular range of embedded
T = n
2
Ef eapp
cosh[n(L, - x)/r]
sinh[ns] (6)
lengths. I9
The strain and interfacial shear stress distributions for
Neither of these theories takes into consideration
a fibre exhibiting total adhesion to the matrix, with a
the effects of stable fibre debonding and the
typical embedded length L, = 4OOpm and at an
subsequent effects of interfacial friction. Hence, both
applied strain of ~~~~= 0.6% are illustrated in Figs 3
approaches produce unrealistic estimates of the
and 4 respectively.
interfacial shear strength for the single-fibre
composites.
4.2 Total debondmg model
The debonding model proposed by Piggott” assumes
a constant interfacial shear stress, r = Zi- For a
4 THEORETICAL CONSIDERATIONS OF pull-out specimen for which the interface fails by
PULL-OUT debonding the balance of forces2’ the following is
given

4.1 Elastic stress transfer daf _ -22,

Piggott”’ has analysed elastic stress transfer for a dx r
pull-out specimen with one end of the fibre embedded Integration of eqn (7) with the boundary condition
in a resin block and the fibre gripped at the point uf = 0 at a distance x = L, yields:
where it leaves the resin, such that there is no free
length (Lf = 0). Application of a strain to the fibre, e,=?(L.-x)
&app, in order to extract the fibre from the polymer f

matrix creates a stress distribution within the The assumption of a constant shear stress gives
embedded region of the fibre, gf, that declines with a
distance x from the polymer surface, according to the T = ri (9)
following equation:” where ri is commonly known as the interfacial
frictional shear stress, related to the radial pressure, P,

-I I

where

n2=Ll__
E 1 1
(3)
Ef In(R/r) (I+ v,)

and ln(R/r) can be considered to be a volume fraction

parameter. If it is assumed that there is no bonding
across the fibre end, integration of eqn (2) with
boundary conditions: uf = gapp at x = 0, gf = 0 at
x = L, yields
Distance Along Fibre, x (WI)

E =E sinh[n(L, -x)/r] Fig. 3. Theoretical plots of strain during pull-out for the
f aPP (4) Kevlar-49/epoxy system, using L, = 400 pm. (a) Variation
sinh[ns]
of fibre strain with distance along the fibre for a totally
bonded interface at an applied strain of E,,,~=0.6%. (b)
where cf is the axial strain in the embedded region of Variation of strain for a completely debonded fibre with
the fibre at a distance x from the resin surface, and s is distance along the fibre.
416 D. .I. Bannister et al.

illustrated in Fig. .5(a) and (b) by using typical values
for the various parameters.
4.4 Instability of the debond process
A theory of partial debonding has been developed in a
series of recent papers by Hseuh,23*24 who assumed a
maximum shear stress criterion for the propagation of
debonding. This work has been critically assessed by
Kim et LZ~.,*~and a similar approach to partial
debonding is adopted in our analysis.
The total applied strain required to partially debond
a fibre, eapp, is given by the sum of the frictional
(debonded) and frictionless (bonded) components of
the partial debonding model, as shown in Fig. 5(a).
Assuming the frictional shear stress to be constant, the
axial strain component in the debonded region is
given by eqn (11) as:
deb _
Ef - Eapp - (14)
i.e.
&b
constant in the form of a critical length, LcritmIt is the
distance of a propagating debond from the fibre-
embedded end for which the debonding will become
unstable and lead to a substantial load drop (e.g. B-C
in Fig. l(c)). Thus, it controls the maximum strain,
e;lax, which is obtained during pull-out. For samples
with embedded lengths less than the critical length,
L, < L,-ity no stable debonding will be observed and,
furthermore, the strain required to initiate debonding
will decrease with decreasing embedded length. For
specimens with L, > Lcrit using the typical parameters
chosen (Fig. 6), debonding initiates at a strain of
approximately 0.62% for our system and the specimen
will exhibit both stable and unstable debonding. The
transition from stable to unstable debonding occurs
when the derivative of the total stress, u:Ot, with
respect to the bonded length, (1 - m)L,, is less than
or equal to zero.25 For our convenience we have used
2Ti[Z- (1 - m)L,]
the derivative of the strain with respect to the bonded
Efr
length, i.e.
de:”

Ef
_

-
27i(1 - m)L,
(15) d(1 - m)L,
10 (18)
Efr

The axial strain contribution from the bonded region The solution yields for the critical condition
is controlled primarily by the interfacial shear
strength, 7,, and the embedded length L,. At the
L

cnt
= mL

e
= rcosh’[~ (19)
n
initiation of debonding at x = mL, = 0 eqn (13) gives
the strain in the debonded region for m = 1 as: The critical bond length is a constant for a given
composite system being dependent on the ratio of
(16) E,/Ef, the fibrelmatrix volume fraction, the frictional
shear stress Zi and the interfacial shear strength 7,.
Therefore the total strain required to partially debond The critical bond length also defines the maximum
a fibre by a length of (1 - m)L, is strain, E;lax, obtained during a pull-out experiment for
a given embedded length. Hence for L, > L,,i,
Etot
f = ,cpb + $‘” = 2 tanh[nms] +
f
&Fax= 2 tanh
The plot of eqn (17) and its components are shown in f

Fig. 6 for three different embedded lengths. From the

For a single-fibre composite with L, < Lcrit the
partial debonding theory it is possible to define a
maximum strain during a pull-out experiment is
observed at the initiation of debonding (m = 1) and so
1.6
from eqn (16):

&;lax= 2 tanh[ns] (21)

f

For a given composite system there will be a

maximum embedded length of fibre, Ly”, that can be
debonded and ‘pulled-out’ from its matrix without the
fibre breaking at its failure strain (ET). The value of
Ly is obtained by equating the solution for the
maximum debond strain (eqn (20)) to the ultimate
0 1w 200 300 400 500 600 tensile strain of the fibre, E:, and it is given by
Degree of Debonding (I-m)L, (run)

Fig. 6. Dependence of the total strain required to partially L

max _
- 27,
‘E’ $ -%ttanh(!+!) +=$!I (22)
debond a fibre upon the degree of debonding predicted
using eqn (17). Three values of embedded length, L,, are
shown. Equations (20)-(22) allow the application of the partial
 Analysis of the single-jibre pull-out test
debonding model to the conventional mechanical
pull-out test.
5 RAMAN SPECTROSCOPY
Part I of this studyY was concerned with a
demonstration of the power of the Raman technique
in being able to map the distributions of fibre strain
for the pull-out of both sized and de-sized Kevlar-49
tibres fully embedded in both hot-cured and
room-temperature-cured epoxy resin blocks. Different
deformation processes were identified, but the present
study is concerned with a detailed investigation into
the behaviour of a single pull-out specimen consisting
of a sized Kevlar-49 fibre partially embedded in an
epoxy block, cured at room temperature to reduce the
effects of thermal stresses.
Figure 7 shows the distributions of strain along the
Kevlar-49 fibre of embedded length L, = 1080 ym, for
nominal applied strains, ranging from 0.6% to 1.6%.
This single Raman experiment provides a detailed
Insight into the three stages of pull-out, namely (i)
elastic deformation, (ii) partial debonding, and (iii)
frictional pull-out.
It should be pointed out that a nominal strain, E(),
will be employed to generate the theoretical curves for
the Raman data. The nominal strain is the estimated
maximum strain in the fibre at the surface of the resin
!x = 0). The value of E() may vary slightly from the
applied strain, E,~~, in the free-fibre, owing to the
stress concentration where the fibres enter the resin
block. It was found previously’ that there can
sometimes be discontinuities in fibre strain in this
region. The origin of this phenomenon is not yet
known, although recent finite element analyses of the
pull-out test26.27 have demonstrated that such discon-
tinuities may be a result of high radial and axial tensile
stresses in the fiber near to the fibre entrance that may
give rise to cracking of the fibre surface.
I ” “I
KEVLAR 49/ EPOXY PULL-OUT
Fig. 7. Variation of fibre strain with distance along the fibre
at different levels of applied strain, E,~,,, determined using
Raman spectroscopy for a Kevlar-49/epoxy specimen with
L, = 1080 Wm.
417
5.1 Elastic deformation
At low nominal strain, E,,50.60%, the fibre strain
decreases from a maximum where the fibre enters the
resin to approximately zero at the fibre embedded
end. Figure 8 reveals that this behaviour is
quantitatively similar to the distribution of fibre strain
predicted by shear-lag theory.“’ The slight discrepancy
between the theoretical curve given by eqn (5) and the
experimental data at x > 200 pm may be a result of
residual compressive stresses on the fibre induced
during curing of the resin matrix. The shear-lag
theory’” predicts that the strain will decrease to zero
over a stress transfer length and neglects residual
stresses in the matrix.
5.2 Partial debonding
At increased nominal strains, E,,2 0.60%, (Fig. 9) the
simple shear-lag theory becomes inadequate to model
the corresponding strain distributions. It is apparent
from Fig. 9 that debonding at the fibre/matrix
interface has occurred and the distribution of strain is
now defined by two distinct zones. The debonded and
bonded zones can be defined by the continuity of axial
strain at the point x = (1 - m)L., and the limits .Y= 0
and x = L,. Taking suitable values for rn and ; to tit
the experimental data, the theoretical strain distribu-
tions can be generated from eqns ( 11) and ( 12) for a
given nominal strain.
As the strain is increased there is stable propagation
of the debond along the fibre/matrix interface. The
correlation between the experimental data and the
theoretical strain distributions are very good for all
partially debonded data (Fig. 9).
5.3 Frictional pull-out
Once the fibre has been completely debonded from
the matrix the pull-out process is controlled by
interfacial friction and the strain profile in the fibre is
Fig. 8. Experimentally measured and theoretically predicted
variation of fibre strain with distance along the tibrc at a
nominal strain, F,,, of 0.6% for the Kevlar-G/epoxy
specimen with L, = 1080 ;tm.
41x D. J. Bannister et al.

5.4 Interfacial shear stresses

-0.2~. ’ ’ ’ . ’ ’ .
0
-200 200 400 600
Dostance Along Flbre. x @m)
Fig. 9. Experimentally measured and theoretically predicted
variations of fibre strain with distance along the fibre at
different nominal strain levels for the Kevlar-49/epoxy
specimen with L, = 1080 pm undergoing partial debonding.
given simply by eqn (8). From the experimental
results in Fig. 10, it was observed that the fibre was
pulled out in a ‘stick-slip’ manner and it was only
possible to obtain two strain profiles of the debonded
fibre. This ‘stick-slip’ motion is thought to be a
consequence of the difference between the dynamic
and static friction coefficients and the effect is
promoted by Poisson shrinkage of the fibres.‘* It was
also reported that below a given pull-out force the
‘stick-slip’ mechanism is replaced by ‘smooth sliding’,
which was not observed in this study. This could be
attributed to the stored elastic energy in the free-fibre
length, L,. Large free-fibre lengths will store enough
energy for a fibre to be completely pulled out without
further application of strain.17
It can be seen that the experimental data in Fig. 10
fit well to straight lines, except for x < 50 pm where
there is a slight discontinuity in fibre stress,’ as
discussed earlier. It would appear from the slopes of
the lines that, during frictional pull-out, z, increases
with decreasing embedded length.
I, I, I I
The interfacial shear stress distributions are shown in
Figs 11-13 for all levels of applied strain. They were
derived through eqn (5) from the theoretical curves
fitted to the fibre strain profiles in Figs S-10.
In the totally bonded condition, as the applied
strain is increased the maximum interfacial shear
stress increases until debonding is initiated. Figure 11
shows that, at a nominal strain of 0.60%, the
maximum interfacial shear stress is 41 MPa, and this
’ 1 . 1 appears to be below the level at which debonding
800 1000 ,200
occurs.
At nominal strains above O-60% it appears that
debonding is initiated and propagates along the
interface as the strain is increased. Figure 12 shows
the dependence of the interfacial shear stress with
distance along the fibre, upon nominal fibre strain in
the range 0.6% < E(,< 1.6%. The interfacial shear
stress builds up from the fibre end and then reaches a
peak value of between 32 and 42 MPa, at which point
debonding occurs. The interfacial shear stress in the
debonded region is of the order of 5 MPa and is
remarkably constant. It would appear, therefore, that
the interface has a maximum shear strength, z,,,, of
the order of 42 MPa, which is approximately equal to
the shear yield strength of the epoxy matrix
(zY = 43 MPa).2X It is important to note that a similar
value of rm5,,, was obtained for the identical
fibre/matrix system2’ from Raman measurements
upon fully embedded fibres in tensile bars subjected to
axial tension. Assuming that debonding of the
fibre/matrix interface occurs when the yield stress of
the matrix is reached, then for the composite system
investigated it follows that z,,, = fy = r&.h= 7,.
The frictional component of the partially debonded
fibre gives a frictional shear stress value of Ti of
approximately 4.5 MPa, and this does not vary
significantly throughout the debonding process
(Fig. 12). Following total debonding of the fibre and
the onset of frictional pull-out, the value of Zi
’ 8.

I ,
FRICTIONAL PULL-OUT I

ELASTIC SHEAR-LAG

0 200 400 600 800 ,000 1200

Distance Along Fibre, x (km) 50 100 150 200

Distance Along Fibre. x (em)
Fig. 10. Experimentally measured and theoretically pre-
dicted variations of fibre strain with distance along the fibre Fig. 11. Distribution of interfacial shear stress at a nominal
for different embedded lengths for the Kevlar-49/epoxy strain, E,,, of 0.6% for the Kevlar-49/epoxy specimen with
specimen undergoing frictional pull-out. L, = 1080 pm derived from the data in Fig. 8.
 Analysis of the single-jibre pull-out test 419

7, = 7 max = 43 MPa and an average value of r, of

-4.5 MPa was obtained.
The partial debonding model has three distinct
regions defined by the instability criterion at L, = L,,,,
and the average ultimate tensile strain of the fibre at
L = LI,,. Figure 14 shows the experimental data
points from Fig. 2 and the theoretical curve (solid
squares) given by the model using the parameters
determined from the Raman measurements. Pull-out
data determined from the maximum applied strain in
a series of Raman pull-out experiments are also
0 200 400 600 800 ,000 1200 plotted. Most of the experimental data fall on or
Distance Along Fibre, x Cm)
above the theoretical curve. One source of the
Fig. 12. Distributions of interfacial shear stress at different discrepancy can be attributed to the different effective
nominal strain levels for the Kevlar-49/epoxy specimen with strain rates used in the Raman experiments and
L, = 1080 pm undergoing partial debonding, derived from
the data in Fig. 9.
mechanical pull-out testing. The Raman pull-out is a
quasi-static test with a displacement rate of approxim-
ately 0.2 mm/h compared to the dynamic strain rate of
increases to 5.3 MPa and then at L, = 600 pm to 60mm/h for the mechanical method. It can be seen
7.5 MPa (Fig. 13). This increase in ri as L, decreases that the Raman points tend to fall below the data
has been reported elsewhereZY for polyethylene/epoxy points for the conventional experiments. It should be
composites. One possible explanation is the resistance pointed out, however, that the majority of the Raman
to motion of kink bands and other regions of irregular data points also lie above the theoretical curve for
fibre diameter. The fibre can then behave as an elastic Si = 4.5 MPa. The pull-out specimen investigated in
string containing knots along its length. As pull-out detail in this present study had particularly well
proceeds, these knots cause an increase in debris defined behaviour showing distinct regimes of elastic
around the interface increasing roughness and deformation, partial debonding and controlled pull-
consequently increasing friction.2y out. The data point in Fig. 14 for this particular
specimen is indicated by an arrow and it can be seen
6 MODELLING OF THE MECHANICAL PULL- that it falls near to the theoretical line.
OUT TEST Other Raman pull-out specimens did not show such
well defined behaviour. In particular they did not
6.1 Dependence of pull-out force upon embedded undergo such controlled pull-out. owing probably to
fibre length the state of the debonded interface in individual
From the theoretical considerations of partial specimens. Hence. a theoretical curve has also been
debonding, eqns (20)-(22) can be applied to model
mechanical pull-out data. Val,ues of interfacial shear
strength, r,, and frictional shear stress, pi, were taken 040 ,.,,,,,,,,,,,,,,

from the results of the Raman experiments in Fig. 12. 035 - Flbre Fracture,

The interfacial shear strength was taken to be

I I I

FRICTIONAL PULL-OUT

000 *.““,“‘f,,, 1, ,.I.!

0 200 400 600 600 1000 1200 1400 1600 1600 2000

Embedded Lenglh. L, (,,m)

200 400 600 800 1000

Fig. 14. Experimental data for the dependence of the
I20(
pull-out force, Fr”“, upon embedded length for the
Distance Along Fibre, x (pm)
Kevlar-49/epoxy system investigated determined using both
Fig. 13. Distributions of interfacial shear stress at different conventional mechanical (0) and Raman (0) pull-out
nominal strain levels for the Kevlar-49/epoxy specimen experiments. The continuous curves are derived from the
undergoing frictional pull-out. derived from the data in partial debonding theory using r,= 31 MPa and the
Fig. 10. indicated values 01 r,.
420 D. J. Bannister et al.
plotted for t, = 15 MPa (using the same value of 5,). It
can be seen that now nearly all the data lay between
the two bounds, implying that all of the specimens
have a similar value of interfacial shear strength, r,,
but different frictional shear stress, Zi. This would
seem to be reasonable, since the strength of the
interface may not vary significantly from specimen to
specimen, but the frictional shear stress is likely to be
very sensitive to factors such as the local fibre
diameter, the presence of kink bands and the
geometry of the embedded fibre ends.
6.2 Modelling of the force/displacement curve
The partial debonding model can be utilized in the
explanation of the force/displacement curves in Fig. 1.
Takaku and ArridgeiS proposed that the peaks in the
ascending region of a force/displacement curve such
as that shown in Fig. l(c) were a consequence of a
step-wise debonding phenomenon. Their proposal
would appear to be confirmed by the application of
the partial debonding theory and the results from
Raman spectroscopy.
As the displacement is initially increased there is a
linear increase in force, concurrent with the elastic
shear-lag theory, until the shear strength of the
interface is reached at FFb (point A in Fig. l(c)).
After initiation of interfacial debonding the pull-out
force increases as debonding proceeds, until a
maximum force, F1p”“, is obtained (point B in Fig.
l(c)). This phenomenon of stepwise debonding was
apparent in nearly all the mechanical pull-out tests
and observed directly in the Raman tests. In terms of
the partial debonding model, FFb and Fr” are
defined by the interfacial shear strength, r,, and the
instability criterion for debonding, respectively. Upon
reaching FT”‘, unstable debonding occurs, accom-
panied by an instantaneous load drop in the
force/displacement curve. The pull-out process is then
controlled entirely by frictional stresses at the
interface and the initial frictional force, F:“, is given
simply by
Frc’ = 2mL, Ti (23)
Frictional pull-out then proceeds in a ‘stick-slip’
manner (point C in Fig. l(c)), as observed in both the
conventional analysis and the Raman spectroscopy
analysis. Eventually, this ‘stick-slip’ motion is
replaced by smooth sliding and this transition
probably depends upon the relationship between the
embedded length and the frictional shear stress.
In practice, however, the instantaneous load drop in
the force/displacement curve was either catastrophic,
resulting in complete fibre extraction, or minimal,
followed by the attainment of frictional data. The
partial debonding theory predicts a load drop equal to
Fl(eh during the process of unstable debonding, but the
drop may be magnified by energy released from the
free fibre, or minimized by frictional forces acting at
the interface. It would appear that to a certain extent
the ability to obtain frictional data depends upon the
embedded length of the fibre. For our particular
system, the force/displacement curves for short
embedded lengths (L, -=c800 pm) exhibited stepwise
debonding before catastrophic failure. Only em-
bedded lengths greater than 1000 pm consistently
produced frictional information.
The inability of short embedded fibres to pull out in
a controlled manner is dependent upon the frictional
shear stress, Zi. Upon initiation of unstable debonding,
the force required to debond the remaining fibre
rapidly decreases, but instead of producing a recoil the
applied force is balanced by the frictional forces at the
interface. It is clear from eqn (23) that the force
required to overcome the frictional shear stress
depends on the embedded length of the fibre.
Therefore, for short embedded lengths the values of Zi
required to prevent fibre pull-out are so high that in
practice they are unattainable. The situation in which
a large load drop is followed by frictional pull-out
(Fig. l(c)) could be attributed to partial extraction of
the fibre before a force equilibrium is achieved.” The
frictional shear stress may increase owing to Poisson
expansion, when the force is relieved by the slip
process, or to debris build up.
It is apparent that the shape of the
force/displacement curve depends on many interfacial
processes. The partial debonding theory goes some
way to explain, and predict, the peaks in the ascending
part of the curve. Equation (16) can be implemented
to predict the force required to initiate stepwise
debonding, whilst eqn (20) predicts the force for the
onset of unstable debonding. However, the theory
cannot predict the magnitude of the load drop on the
initiation of unstable debonding. The lack of
reproducibility in the preparation of specimens and
test dynamics could be largely responsible.
7 CONCLUSIONS
It has been shown that Raman spectroscopy is a
powerful tool for the investigation of interfacial
phenomena in composites. Application of the
technique to the single fibre pull-out test combined
with the development of a partial debonding theory
have led to the conclusion that the initiation of fibre
debonding is controlled primarily by the interfacial
shear strength, r,, for a given composite system.
Furthermore, propagation of fibre debonding and the
subsequent extraction of the fibre from the resin
matrix are controlled by the interfacial frictional shear
stress, ri, which is unique to a particular pull-out
specimen.
The partial debonding model for single-fibre
pull-out adequately describes the strain profiles
 Analysis of the single-fibre pull-out test 421

obtained from Raman spectroscopy at all levels of pull-out tests. Compos. Sci. Technol., 22 ( 198.5) 33-42.
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ACKNOWLEDGEMENTS interfacial radial and shear stress on the fibre pull-out in
composite materials. J. Phys. D: Appl. Ph_w, 6 (1973)
This work was supported by Research Grants from
2038-47.
the Engineering and Physical Sciences Research 16. Kelly, A. & Tyson, W. R., Tensile properties of
Council and the Ministry of Defence and from Shell fibre-reinforced metals: copper/tungsten and
Research. One of the authors (R. J. Y.) is grateful to copper/molybdenum. J. Mech. Phys. Solids. 13 (1965)
the Royal Society for support in the form of the 329.
17. Li, Z. F. & Grubb, T., Single fibre polymer composites.
Wolfson Professorship in Materials Science.
Part I: Interfacial shear strength and stress distribution
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