Mode I interfacial toughening through discontinuous interleaves for damage

suppression and control

M. Yasaee
a
, I.P. Bond
a,
, R.S. Trask
a
, E.S. Greenhalgh
b
a
Advanced Composites Centre for Innovation and Science (ACCIS), University of Bristol, Queens Building, University Walk, Bristol BS8 1TR, UK
b
Composites Centre, Imperial College London, London SW7 2AZ, UK
a r t i c l e i n f o
Article history:
Received 14 April 2011
Received in revised form 30 August 2011
Accepted 6 October 2011
Available online 22 October 2011
Keywords:
D. Fractography
B. Delamination
B. Fracture toughness
Crack arrest
a b s t r a c t
An investigation is described concerning the interaction of propagating interlaminar cracks with embed-
ded strips of interleaved materials in E-glass bre reinforced epoxy composites. The approach deploys
interlayer strips of a thermoplastic lm, thermoplastic particles, chopped bres, glass/epoxy prepreg,
thermoset adhesive lm and thermoset adhesive particles ahead of the crack path on mid-plane of Dou-
ble Cantilever Beam (DCB) specimens. During these mode I tests, the interlayers were observed to confer
an apparent increase in the toughness of the host material. The crack arrest performance of individual
inclusion types are discussed and the underlying mechanisms for energy absorption and the behaviour
of the crack at the interaction point of the interleave edge were analysed using scanning electron
microscopy.
2011 Elsevier Ltd. All rights reserved.
1. Introduction
Arresting crack propagation in materials is achieved by intro-
ducing a feature that is capable of absorbing energy which would
have otherwise initiated and propagated cracks [13]. To achieve
crack arrest during delamination of Fibre Reinforced Polymer
(FRP) composites, any feature must be capable of increasing the
critical strain energy release rate, G
C
, of the material. There is lim-
ited research in the subject of crack arrest in FRP composite mate-
rials. The most common crack arrest features implemented at a
structural level are stringers [4], rivets [5], holes [6], and buffer
strips [7], which all aid in the redirection and arrest of unstable
cracks. Some of these techniques, although successful in homoge-
neous materials such as steel or aluminium, are not as effective
in FRP composites. This is because the additions of structural dis-
continuities are likely to have a signicant detrimental effect on
the global mechanical performance of the FRP. This study will focus
on the problem and behaviour of delaminations in FRP at a mate-
rial level, whereby a crack arrest feature is incorporated during the
fabrication process using additional materials.
Delamination is a common failure mechanism associated with
laminated FRPs and is a manifestation of their poor through thick-
ness strength. Comprehensive research has been undertaken into
the understanding of delamination in laminated FRPs, with a re-
cent report by Brunner et al. [8] providing a good indication of
overall progress. Delamination can be partitioned into three pure
modes of loading; mode I (opening), mode II (shear) and mode III
(tearing/twisting) [9], although the latter is usually neglected and
is not considered in this study. Combinations of loading modes
usually occur to give mixed mode I/II loading. Experimental meth-
ods developed to measure the interlaminar fracture toughness of
FRP composites under different mode mixities have been standard-
ised for composite materials [1012].
One method of increasing interlaminar toughness of a compos-
ite is by modifying the resin-rich layer in between the plies. This
method is called interleaving and has shown to provide consider-
able improvements in both impact resistance and inter-laminar
toughness of an FRP [1215]. Similarly, crack arrest of delamina-
tions has been achieved by the use of periodically spaced ductile
adhesive strips placed in between the plies [7,1618]. Such strips
were successful in arresting delamination; however, testing was
only performed under tensile loading.
Interleaving will have noticeable effects on other composite
properties depending on the extent of implementation within a
laminate. Introducing interleaves will result in lower global stiff-
ness, strength and changes to the global bre volume fraction, V
f
,
of the composite. Therefore, to mitigate this situation, additional
plies must be introduced which in turn will result in a weight pen-
alty [20]. However, within this investigation instead of applying
continuous layers of toughening materials, different material types
are interleaved as a discrete single strip. To the best of the authors
knowledge there has been no reported work on the effect of crack
propagation from an unmodied interlaminar region of a compos-
1359-835X/$ - see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2011.10.009

Corresponding author. Tel.: +44 (0) 1173315321.

E-mail addresses: m.yasaee@bristol.ac.uk (M. Yasaee), i.p.bond@bristol.ac.uk
(I.P. Bond), r.s.trask@bristol.ac.uk (R.S. Trask), e.greenhalgh@imperial.ac.uk (E.S.
Greenhalgh).
Composites: Part A 43 (2012) 198207
Contents lists available at SciVerse ScienceDirect
Composites: Part A
j our nal homepage: www. el sevi er . com/ l ocat e/ composi t esa
ite into a series of interleaved features. Understanding the mecha-
nisms that cause an apparent increase in the interlaminar tough-
ness of a composite due to the inclusion of discrete pieces of
interleaved materials will aid in the development of improved
damage tolerant composite materials.
This investigation undertakes an experimental assessment of
mode I fracture toughness in E-glass reinforced epoxy FRP follow-
ing the inclusion of various interleaved material inserts. The ability
of an individual insert material to increase the strain energy re-
lease rate G
C
, is assessed from the mechanical response and using
detailed fractography between the interaction region of the propa-
gating crack and the interleaved feature.
2. Interleaved composites
The implementation of interleaved layers does not necessarily
add signicant cost to the fabrication of a composite, although
some interleaves layers, such as those incorporating carbon nano-
tubes (CNTs), are bespoke and expensive to manufacture.
Interleaved materials used for FRP composite fracture tough-
ness enhancements in this study are classied into ve different
types; additional matrix resin, thermoset adhesive lms, random
short bres, micro-sized polymer particulates, and thermoplastic
polymer lms.
The most straightforward method is the use of additional ma-
trix resin on the delamination interface, effectively increasing the
interface thickness. This method has been shown to give a substan-
tial improvement in the interlaminar toughness of the composite
with G
IC
and G
IIC
values increasing by 70% and 200%, respectively,
with an interleave thickness of 0.2 mm [15,19]. It was proposed
that the G
IC
increase of such interleaved resin rich interfaces in-
creases with thickness until it reaches a plateau equivalent to the
mode I fracture toughness of the matrix material [16]. The plastic
yield zone ahead of the crack tip is the essential mechanism that
determines the location of the crack propagation through thickness
of the interface, as illustrated in Fig. 1.
When the interleave thickness is smaller than the diameter of
the plastic yield zone the crack will migrate towards the weakest
region i.e. the boundary of the bre resin, resulting in an adhesive
failure of the interleave. However, as the interleave thickness in-
creases beyond the plastic yield zone diameter, the crack will no
longer propagate along the interface between the interleave and
host matrix but will remain within the resin resulting in cohesive
failure of the interleave [21] (see Section 5.1). The saturation of the
plastic yield zone has been shown to occur for insert thicknesses of
>0.1 mm for thermoset resins [22].
Sela et al. [22] looked at the effect on fracture toughness of dif-
ferent thicknesses of interleaved thermosetting adhesive lms.
They used various lm adhesives to show that the inclusion of
the interleaves signicantly increased both mode I and mode II
fracture toughness, a result also conrmed by Gibson et al. [23]
and Ozdil and Carlsson [24]. Jiang et al. [25] investigated loading
rate effects on the mode II interleave fracture toughness of Redux
319 adhesive (Hexcel, UK). They found that at lower loading rates,
delamination cracking tended to propagate along the boundary be-
tween the interleaved layer and the parent composite. However, as
loading rate is increased, crack growth remained within the inter-
leaved material which effectively increased toughness.
It is clear that the fracture toughness for cohesive failure of the
insert or parent resin is generally greater than that of adhesive fail-
ure at the bre/matrix interfaces. Therefore, for thin interface re-
gions, the fracture toughness reects the bond strength between
the matrix and bres whereas for thicker interface regions, crack
jumping is constrained and propagation is in the form of cohesive
failure of the resin, hence exhibiting an increase in G
IC
.
The use of additives such as short bres, nano bres or polymer
particles is another popular method of effectively providing an
interleaved layer. Lee et al. [26,27] investigated mode I and mode
II fracture toughness improvement using Non-Woven Carbon Tis-
sue (NWCT) as an interleave material. NWCT is ideal for this appli-
cation due to its good formability and relatively low cost. NWCT
contains unaligned short bres ranging from 3 to 25 mm randomly
distributed across the layer. They typically nd application in pro-
tective layers on exterior surfaces of composite structures. The
investigation by Lee et al. [26,27] showed the variation in mode I
and mode II fracture toughness (G
IC
and G
IIC
) and crack growth
location through the thickness of the interleave. Cohesive failure
of the interleave led to a signicant increase in composite tough-
ness of G
IC
by 28% and G
IIC
by up to 260%. They also carried tensile
strength analysis of Carbon FRPs (CFRPs) composites interleaved
with other types of Non-Woven Tissues (NWTs); these were
Non-Woven Polyester Tissue (NWPT), Non-Woven Glass Tissue
(NWGT) and Non-Woven Aramid Tissue (NWAT) [28].
Chopped aramid bres (1220 mm) were used as an interleave
layer with the intention of exploiting the high tensile strain to fail-
ure properties of the aramid bres [29,30]. Improvements in both
mode I and mode II fracture toughness were stated as being the re-
sult of additional aramid bre bridging during delamination.
Recent advances in the development of nanoscale bres have
led to several investigations for their implementation as inter-
leaved materials. Carbon Nanotubes (CNTs) [3135], PolyEtherKe-
tone Cardo (PEK-C) nanobres [36], Nylon-66 nanobres [37,38],
electro spun polysulfone (PSF) nanobres [39] and b-SiC whiskers
[40] have all been evaluated via fracture toughness testing and in
all cases signicant improvements in G
IC
and G
IIC
were reported.
The techniques used to manufacture such nanobre layers were
varied and the resulting interleaved layers are always unaligned.
However, Wardle et al. [31,32] have developed a novel technique
to align CNTs through the thickness and used these as interleaved
layers. Subsequent mode I and mode II composite fracture tough-
ness testing exhibited a 300% increase.
Spherical nylon particles of varying diameters (10180 lm)
were used as an interlayer material, however, it was reported that
the particles capability to sustain thicker interlayer regions helped
to increase energy absorption and hence exhibit improvements in
mode II fracture toughness [41,42]. In mode I, the fracture tough-
ness was reported to have been reduced as a result of the nylon
particle inclusions [43]. Crosslinked carboxyl functionalised elasto-
mer particles based on butadiene acrylonitrile (DuoMod DP 5045,
Zeon Chemicals Inc.) are micro particulates which have been devel-
oped to improve the fracture toughness of laminates. It was found
that interleaving of these particulates in CFRP laminates resulted in
G
IC
and G
IIC
increases of more than 70% and 350% respectively [44].
Other popular interleave materials include thermoplastic poly-
mer lms such as Carboxyl-Terminated Butadiene acryloNitrile
(CTBN), PolyUrethane (PU) [45], PolyEthylene Terepthalate (PET)
[4648], Ethylene base ionomer [49,50], Poly Ether Ether Ketone
(PEEK) [51] and PolyEtherImide (PEI) [23]. Each material confers
FRP Resin interface
Plastic yield zone
(b) (a)
Fig. 1. Illustration of plastic yield zone interaction with interleaf boundaries for
different thicknesses (a) adhesive failure of the resin and bre and (b) cohesive
failure of the resin. (For interpretation of the references to colour in this gure
legend, the reader is referred to the web version of this article.)
M. Yasaee et al. / Composites: Part A 43 (2012) 198207 199
a relative improvement in fracture toughness on the composite.
Some thermoplastic lms such as Kapton or PolyTetraFluoroEthyl-
ene (PTFE) do not bond to epoxy and are typically used for crack
starters in fracture toughness testing. However, Armstrong-Carroll
et al. [52] polymerised allylamine monomer in a plasma atmo-
sphere and condensed them onto Kapton and PTFE lms. This re-
sulted in a stronger bond to epoxy, subsequent mode II fracture
toughness showed a noticeable increase.
From the reported studies, interleaved layers offer a very prom-
ising technique for increasing interlaminar toughness. Using such
layers as strips in the form of a periodic crack arresting feature will
be investigated in this study and the propagation of a crack froman
unmodied region of the laminate into the interleaved zone will be
analysed.
3. Test procedure
For this investigation an ASTM-D5528 standard for Double Can-
tilever Beam (DCB) testing of unidirectional (UD) FRP composites
[10] was followed. Due to the low exural modulus of GFRP there
is a possibility of the specimen beam arms undergoing large deec-
tions. Hence, the specimen thickness, h, was chosen to satisfy the
following criteria:
h P8:28
G
Ic
a
2
0
E
11

1=3
1
with a maximum expected G
IC
of 1000 J/m
2
at an initial crack length
a
0
of 50 mm for an modulus E
11
of 42.2 GPa. A 24-ply composite
laminate of 0 plies of pre-impregnated E-glass bre/913 epoxy
(Hexcel, UK) was selected to give a total thickness of approximately
3.12 mm. A PTFE lm of 12 lm thickness was used as a crack starter
on the mid-plane of the laminate. An interleaved strip or crack ar-
rest feature of length 10 mm was placed 20 mm ahead of the initial
crack front, Fig. 2. Redux 810 epoxy adhesive (Hexcel, UK) was used
to adhere two piano hinges to the end of the specimen ready for
DCB testing.
Using a calibrated Instron test machine with a 18 kN load cell,
the load was applied to the specimen at a displacement rate of
4 mm/min. The resulting values of Load (P) and deection (d) were
recorded for every 1 mm increment in crack length a, for the 5 mm
prior to interaction with the interleave layer and 5 mm through the
interleave strip. Continued crack propagation was measured in
5 mm increments until the crack length reached a total length of
100 mm. The delamination growth was illuminated with a light
source placed under the translucent specimen and crack growth
was recorded using a digital camcorder placed above the specimen.
This allowed the crack growth to be recorded and any non-linearity
in the crack front monitored to distinguish specimens with asym-
metric loading. The basic modied version of the beam theory Eq.
(2) was used to calculate the G
IC
of each specimen [10,53].
G
Ic

3
2
pd
ba D
2
Five replicates were tested for each fracture toughness assess-
ment of the interleaved layers.
3.1. Interleave materials
Initial trials were undertaken using commercially available
materials for different interleave types. These trials allowed for
optimisation of the most efcient application method of each
material type into the GFRP laminates. The thermoset adhesive re-
sin, thermoplastic lm and the E-glass/epoxy prepreg strip were
cut to size and simply placed on the laminate with the prepreg
strip positioned 90 relative to mid-plane bre direction. The ther-
moset adhesive resin was found to diffuse along the bre direc-
tions which increased the interleave width from the intended
10 mm to approximately 15 mm. The chopped E-glass and aramid
bres were cut to approximately 10 mm lengths from bre tows
and evenly spread across the laminate with individual bres ran-
domly oriented. The particulates were weighed and spread onto
the laminate to cover the desired area through a ne sieve for even
distribution of 143 gsm.
Nylon particulates of different average diameters of 20 lm and
30 lm were chosen to distinguish if this had any signicant impact
on fracture toughness. Chopped glass and aramid bre allowed a
comparison of different bre strength and strain to failure and
the effect of randomness or order.
A novel thermoset polymer foam in spherical particulate form
of diameters in range of 60800 lm obtained from High Internal
Phase Emulsions (PolyHIPE) [54] was also investigated as such par-
ticles could potentially be used to add self-healing function to
FRPs.
Details of the interleave materials investigated, the thickness of
the interleave layers post-cure and the approximate areal density
are provided in Table 1.
4. Results
The typical DCB load vs. displacement curves of the baseline
and the specimens with the interleaved strips are shown in Figs. 3
and 4. Only one of the particulate interleaved samples is plotted.
Fig. 2. DCB test specimen geometry and interleaved strip location.
200 M. Yasaee et al. / Composites: Part A 43 (2012) 198207
The point at which the load curve deviates from the baseline sam-
ple is indicative of the crack propagation reaching the entry of the
interleaved strip. At this point propagation is momentarily arrested
until load increase generates enough strain energy to propagate
the crack through the interleaved strip. Almost all samples saw
an unstable propagation back into the parent material once the
crack had reached the end of the interleaved strip.
The average critical strain energy release rate, G
IC
, of each DCB
specimen with an interleaved strip was compared with that of
the baseline plain GFRP sample at the same crack length, Figs. 5
and 6. The effect of bre bridging is prominent for mode I delam-
ination in GFRP composites arising from the relatively weak inter-
face between the glass bres and the epoxy [55]. This effectively
increases the apparent fracture toughness of the GFRP samples at
longer crack lengths. Compston et al. [56] investigated the inu-
ence of bre volume fraction on the G
IC
value of GFRP laminates.
It was deduced that V
f
had little effect on the initiation G
IC
of the
composite, however, it was shown that increasing V
f
from 35% to-
wards 55% increased propagation G
IC
from 400to 780 J/m
2
due to
the increased amount of bre bridging. Once the crack had ex-
tended to roughly 80 mm, the effect of bre bridging tended to sta-
bilise and a constant G
IC
value for the GFRP composite was
observed. This value will be referred to as the propagation strain
energy release rate, G
ICProp
, which was measured as 684 J/m
2
.
As anillustrationof howthe fracturetoughness of the interleaved
region varies, the average critical strainenergy release rate plot for a
GFRPsamplecontaininga polyimidelmis comparedwiththe base-
line plain GFRP, Fig. 5. An increase in critical strain energy release
rate, G
IC
, was observed between 70 mm < a < 80 mm. The average
G
IC
rose to a peak at a = 80 mm before unstable delamination
occurred, after whichthe G
IC
returns tothe G
ICProp
of the parent mate-
rial. Similar behaviour was observedfor all the interleavedmaterials
that gave anincreasedstrainenergyreleaserate, relativetothe base-
line G
ICProp
.
The peak G
IC
for all the different interleaved layers occurred at
around 80 mm of crack length. The G
IC
values of the interleaved
layers at 80 mm are presented in Fig. 7. The interleaved materials
Table 1
Interleaved strip material data.
Type Product name Company Interleaf cured thickness (mm) Approximate areal density (gsm)
Thermoset adhesive lm Redux 312 Hexcel, UK 0.24 159
Glass bre Advantex type 30 glass bre Owens corning 0.030.7 335
Aramid bre Kevlar 49 Dupond 0.090.27 67
Prepreg strip (base material) E-glass/913 epoxy Hexcel, UK 0.133 160
Nylon particles (20 lm) Polyamide nylon 6 (PA6) Goodfellow, UK 0.1 143
Nylon particles (30 lm) Polyamide nylon 12 (PA12) Goodfellow, UK 0.07 143
Thermoset polymer PolyHIPE particles PolyHIPES 0.125 143
Polyimide thermoplastic lm Surface treated upilex-50RN UBE industries, Ltd. 0.05 79
0
10
20
30
40
0 10 20 30 40 50
L
o
a
d

[
N
]
Displacement [mm]
Base
Chopped Aramid Fibres
Chopped Glass Fibres
90 Prepreg Strip
Fig. 3. Load vs. displacement curves for baseline and chopped aramid, glass and 90
prepreg interleaved strip DCB specimens. (For interpretation of the references to
colour in this gure legend, the reader is referred to the web version of this article.)
0
10
20
30
40
0 10 20 30 40 50
L
o
a
d

[
N
]
Displacement [mm]
Base
Polyimide Thermoplastic Film
Thermoset Adhesive Film
Nylon Particles 20m
Fig. 4. Load vs. displacement curves for baseline and thermoplastic lm, thermoset
adhesive, and the 20 lm nylon particulate interleaved strip DCB specimens. (For
interpretation of the references to colour in this gure legend, the reader is referred
to the web version of this article.)
0
500
1000
1500
50 55 60 65 70 75 80 85 90 95 100
G
I
C

[
J
/
m
2
]
Crack Length [mm]
Base
Polyimide Thermoplastic Film
Unstable Delamination Interleaved
Region
Fig. 5. Mode I Averaged Strain Energy Release Rate (G
IC
) for baseline plain parent
and polyimide thermoplastic lm interleaved strip samples (error bars equal one
standard deviation, minimum of ve samples per data point). (For interpretation of
the references to colour in this gure legend, the reader is referred to the web
version of this article.)
M. Yasaee et al. / Composites: Part A 43 (2012) 198207 201
that offer improved fracture toughness relative to the baseline G
IC-
Prop
are:
polyimide thermoplastic lm (79% increase in G
ICProp
)
chopped aramid bres (46% increase in G
ICProp
)
90 E-glass/epoxy prepreg strip (46% increase in G
ICProp
)
thermoset adhesive lm (43% increase in G
ICProp
)
chopped glass bres (16% increase in G
ICProp
).
Thermoplastic particles (20 lm and 30 lm Nylon) and thermo-
set polymer foams (PolyHIPES) reduced the G
ICProp
value by 33%,
27% and 28%, respectively. However, the actual G
ICProp
value was
still larger than the initiation G
IC
of the baseline GFRP laminate,
measured as 279 J/m
2
. This reduction in G
ICProp
is attributed to
the inhibition of bre bridging effect due to the presence of the
particles, which is also evident from the slow return to the G
ICProp
value once outside the interleaved region, Fig. 6. Conversely, the
greater thickness of the ply interface that these particles confer,
possibly contributes to the marginal increase in the initiation value
of G
IC
for the composite.
5. Fractography
The most promising interleaved materials were chosen for frac-
tographic analysis. A fully fractured half beam of each DCB speci-
men was cut using a diamond cutter 10 mm either side of the
interleave edge. Both top and bottom fracture surfaces were then
Au sputter coated and examined using a Hitachi S-3400N VP Scan-
ning Electron Microscope (SEM) at magnications of 50
1200 times and voltage accelerations of 1520 kV, with the sur-
faces titled by 15 along the longitudinal bre axis. A schematic
of the different areas of interest are shown in Fig. 8. Regions 1
and 5 have similar fracture surface characteristics to the baseline
laminate. As the crack moved to region 2, there have been various
interactions of the crack with the edge of the interleaved layer and
the change in local geometry, hence generating distinct fracture
morphologies. Region 3 illustrates how the interleaved material
was able to absorb a signicant amount of fracture energy whilst
the change from the toughened zone to the baseline, region 4, pro-
vides some insight into the unstable crack front behaviour as the
crack leaves the interleaved region. The fractographic analysis fol-
lows established methods of sample preparation and analysis
according to the guidelines given in Ref. [57]. The key to the mean-
ings of the annotations used on the SEM images are provided in
Fig. 8.
5.1. Thermosetting adhesive lm
The fracture surfaces of the sample with the Redux 312 adhe-
sive interleave strip are shown in Fig. 9. The inclusion of a thermo-
setting epoxy layer (Redux 312) generated the least disruption to
the ply architecture. As the crack moved towards the adhesive rich
region, (Fig. 9b), the riverlines that extend through the thickness,
changed direction, indicating local mode II loading was present.
Also, there was evidence of ductile failure in the adhesive (Fig. 9b).
Once in region 3 the uneven pockmarked morphology of the
surface of the adhesive, caused by the inclusion of rubber particles,
has resulted in highly ductile failure and consequently a more tor-
turous crack path (Fig. 9a). This would be the main contributor to
the energy absorption of the resin interleaf.
Observation of the fracture surfaces indicates that most energy
absorption could be attributed to the ductile nature of the epoxy.
The migration of the crack into the interleaved region was smooth
with no evidence of inter-ply cracking. The surfaces create similar
mode I features as found for the host epoxy resin but with a ductile
form of scarps, (Fig. 9c) thus an increase of 43% relative to the G
IC-
Prop
of the baseline laminate was measured.
5.2. Chopped aramid bre
The fracture surfaces of the sample with the chopped aramid -
bre interleave strip are shown in Fig. 10. By observing region 2 of
the fracture surface, (Fig. 10c and e), evidence of loose aramid -
bres indicates that there has been substantial bre bridging. Ten-
sile failures of glass bre and matrix gouges were also visible. As
0
500
1000
1500
50 55 60 65 70 75 80 85 90 95 100
G
I
C
[
J
/
m
2
]
Crack Length [mm]
Base
Nylon Particles 20m
Thermoset foam particles
Interleaved
Region
Fig. 6. Mode I Averaged Strain Energy Release Rate (G
IC
) for baseline plain parent
and particulate interleaved strip samples (error bars equal one standard deviation,
minimum of ve samples per data point). (For interpretation of the references to
colour in this gure legend, the reader is referred to the web version of this article.)
0
300
600
900
1200
1500
A B C D E F G H I J
G
I
C
[
J
/
m
2
]
A Base (Initiation)
B Base (Propagation)
C Thermoset Epoxy Film
D Chopped Glass Fibres
E Chopped Aramid Fibres
F 90 Prepreg Strip
G Nylon Particles 20m
H Nylon Paritcles 30m
I Thermoset foam particles
J Polyimide Thermoplastic Film
Fig. 7. Apparent average mode I propagation strain energy release rate (G
IC
) of the crack arrest features (error bars equal one standard deviation, minimum of ve samples per
data point). (For interpretation of the references to colour in this gure legend, the reader is referred to the web version of this article.)
202 M. Yasaee et al. / Composites: Part A 43 (2012) 198207
local cracks around the aramid bres are formed due to bridging,
these tended to migrate towards the global crack front. This phe-
nomenon manifested itself as gouges in the matrix resin. As the
crack continued into the interleave layer, region 3 (Fig. 10b), local
crack paths could be seen to have differed in direction from the
global crack path with many tensile failures of aramid bres visi-
ble. Once the global crack exited the interleave region, local crack
jumps, seen as smooth fracture surfaces (Fig. 10a) appear, before
converging to typical mode I scarps. From the extensive bridging
experienced in the region in the wake of the crack, some degree
of interlaminar shear has been introduced to the global mode I fail-
ure, this was seen as more pronounced riverlines (Fig. 10a and d).
Hence, the increased thickness region and the effective aramid -
bre bridging of the two interfaces contributed to the G
IC
increase
of 46% relative to the G
ICProp
of the baseline laminate.
5.3. Thermoplastic polyimide lm
The fracture surfaces of the sample with the thermoplastic
polyimide lm interleave strip are shown in Fig. 11. In regions 2
and 4 (i.e. before and after the interleaved regions), the fracture
surfaces appear similar. A step was generated as the crack travelled
from the parent composite through to the interleave region
(Fig. 11a, c and e). This was indicative of unstable crack jumps
hence the smooth surface with ne riverlines. Immediately under
the interleave edge the surface becomes rough. Regions where
the polyimide lm has been peeled off the matrix resin generates
either a smooth surface with shallow wave formation imprinted
on the resin (Fig. 11e) or interconnected shallow craters creating
a feature consistent with void coalescence (Fig. 11a and b) which
would indicate ductility of the lm during peel.
Evidence of adhesive failure i.e. matrix resin bonded to polyim-
ide lm, can be seen in Fig. 11b, which creates a rough surface indi-
cating resin damage, Fig. 11c. As the crack propagates from the
parent region into the interleave region, it will propagate either
to the top or bottominterface of the polyimide lm. This effectively
ties the two fracture surfaces with the lm material. During load-
ing, energy is required to effectively peel the lm from the two sur-
faces (Fig. 11b). This contributes to a substantial increase in energy
absorption as witnessed by the increase of 79% relative to the G
IC-
Prop
of the baseline laminate.
Once the crack has propagated fully through the interleave re-
gion, evidence of shearing can be seen as shallow cusps and more
pronounced step like river lines on the mode I scarps are formed
(Fig. 11d).
Crack Direction
4. Boundary Exit from the
Interleave Region
2. Boundary Entry to the
Interleave Region
5. Post Interleave Region
3. Interleave Region
1. Before Interleave Region
SEM Annotation Meaning
Global crack growth direction
Local crack growth direction
Shear direction
Fig. 8. Schematic illustration of the regions of interest for the delaminated fracture
surfaces of the DCB samples.
(b) Region 2, 1100x 15 Tilt (a) Region 3, 350x 15 Tilt
(c) Region 3, 1100x 15 Tilt
Scarps mixture of epoxy
film and parent resin
Ductile fracture of epoxy film
River line direction
Uneven surface of the
fractured epoxy film
Fig. 9. Fracture morphology of the mode I DCB sample with thermoset epoxy interleave strip.
M. Yasaee et al. / Composites: Part A 43 (2012) 198207 203
(e) Region 2, 1100x, 15 Tilt
(b) Region 3, 500x, 15 Tilt
Fibre tensile fracture
Riverlines
(d) Region 5, 500x, 15 Tilt
Mode I scarps with shear
elements
(a) Region 4, 250x, 15 Tilt
e n o z h c i r n i s e R s e n i l r e v i R
(c) Region 2, 200x, 15 Tilt
Loose aramid fibres Gouges
Fig. 10. Fracture morphology of the mode I DCB sample with chopped aramid bre interleave strip.
(c) Region 2, 1000x, 15 Tilt
Possible void
coalescence
(a) Region 4, 300x, 15 Tilt
Unpeeled polyimide film
(d) Region 5, 550x 15 Tilt
Mode I with sheared
elements
Shallow cusps
Riverlines
Peeled polyimide film Resin rich zone
(e) Region 2, 300x, 15 Tilt
Fibre Sheared
Resin damage from
polyimide film peel
(b) Region 3, 300x, 15 Tilt
Shallow Craters
(cohesive failure)
Peeled edge of
polyimide film
Bonded resin
Fig. 11. Fracture morphology of the mode I DCB sample with polyimide lm interleave strip.
204 M. Yasaee et al. / Composites: Part A 43 (2012) 198207
5.4. 90 E-glass/epoxy prepreg strip
The fracture surfaces of the sample with the 90 E-glass/epoxy
prepreg interleaved strip are shown in Fig. 12. The features seen
here are identical to the mode I fractured surfaces for a 2D woven
bre composite [57], with evidence of conicting river lines and
scarps indicating many local crack propagation directional
changes. As the crack grows through the interleave region, evi-
dence of mode I/II mixity could be seen from the shallow cusps
(Fig. 12c) and local shearing of the matrix resin (Fig. 12a and b).
River lines can be seen to rotate from a perpendicular direction to-
wards the global crack direction (Fig. 12d). These conicting river
lines and scarps indicate the complex local crack path propagation
which aid in arresting propagating global cracks.
The effective energy absorption of this sample was similar to
that of the aramid samples which is the result of increased inter-
face thickness and bre bridging. Thus, a G
IC
increase of 46% rela-
tive to the G
ICProp
of the baseline laminates was observed.
6. Discussion
It is widely accepted that a composites performance can be sig-
nicantly reduced if minor aws or defects are present. This sensi-
tivity to defects inhibits the more widespread use of FRPs in safety
critical applications. Damage tolerance for composites has been a
target for many years, however, in order to realise such a charac-
teristic, the damage needs to be effectively managed.
Interleave materials have generally been implemented as
toughening mechanisms by introducing themas a continuous layer
within a laminated composite. This conguration, although capa-
ble of improving delamination resistance of a composite, has a
noticeable detrimental effect on other composite properties, such
as reduction in global stiffness, bre volume fraction reduction
which leads to subsequent weight penalty as a result [20]. An alter-
native, more benign approach is to apply interleaved materials as
periodic inserts. Using this technique it should be possible to con-
trol the distribution and direction of major damage propagation
and hence allow an element of damage tolerance to be designed
from the outset.
For example, during a low velocity impact on a typical FRP,
unstable crack propagation occurs from the impact site. This load-
ing condition is typically mode II dominated. If such an impact
damaged material is then exposed to axial compression, the del-
aminations will be seen to propagate in a manner dominated by
a mode I loading condition. Therefore, periodic interleaved inserts
can be used as means to compartmentalise the structure such that
delamination crack growth is arrested at multiple points thereby
providing control of subsequent damage. Understanding the pre-
cise mechanism by which a propagating crack front interacts with
an interleaved insert is an essential requirement to allow the
appropriate choice and location of such distributed inserts.
In this study, under mode I loading it has been shown that the
inclusion of the interleaved inserts markedly increases interlami-
nar fracture toughness of a GFRP.
The effect of these same inserts under mode II loading is re-
ported in an accompanying paper [58] where it is expected shear
loading will reduce the dominance of crack bridging effects from
the interleave materials; hence the different mechanisms that af-
fect G
IIC
will be of interest.
7. Conclusion
The experimental study described herein aims to determine
suitable materials for use as interleaved layers to act as delamina-
tion crack arrestors within GFRP composites. The crack arrestors
were deployed as 10 mm wide interleaved strips on the mid-plane
of 24 ply unidirectional E-glass/epoxy laminates. The different
interleave layers investigated included thermoplastic lm, thermo-
plastic particles, chopped E-glass and aramid bres, E-glass/epoxy
pre-preg orthogonally aligned, thermoset adhesive lm and
(c) Region 4, 1000x, 15 Tilt
(b) Region 2, 300x, 15 Tilt
Shearing direction Perpendicular
to global crack growth
(a) Region 3, 300x, 15 Tilt
Mode I scarps with shearing
(d) Region 3, 300x, 15 Tilt
Local perpendicular
crack growth direction
Shallow cusps
Fig. 12. Fracture morphology of the mode I DCB sample with 90 prepreg interleaved strip.
M. Yasaee et al. / Composites: Part A 43 (2012) 198207 205
thermoset adhesive particles. From mode I fracture toughness test-
ing, four interleave types were chosen for post-test fractographic
analysis due to the signicant improvement that was observed in
the measured mode I critical strain energy release rate, G
IC
, relative
to a baseline laminate.
This investigation indicates that increased interply thickness
from the use of an interleaved layer contributes only a small
amount to the energy absorption under mode I fracture. However,
the maintaining mechanical linkage between the two crack inter-
faces via the use of inserted bres or lms was seen to be the most
effective way of increasing the mode I fracture toughness for a lam-
inated GFRP.
Acknowledgements
The authors would like to thank the ESPRC and DSTL for funding
of this work under CRASHCOMPS (EP/G003599), Airbus UK for
their additional nancial support, and Mr. Dan Cegla for supplying
the PolyHIPE particulates and for his assistance with the SEM
analysis.
References
[1] Farshad M, Flueler P. Arrest of rapid crack propagation in polymer pipes. Plast
Rubber Compos Process Appl 1996;25:2913.
[2] Kobayashi T, Dally JW. Crack arrest methodology and applications. ASTM STP
1979;711:189210.
[3] Roumaldi JP, Batson GB. Mechanics of crack arrest in concrete. Sel LDM Pap
Concr Mater Res 2008:247.
[4] Greenhalgh E, Hiley M. The assessment of novel materials and processes for
the impact tolerant design of stiffened composite aerospace structures.
Compos Part A 2003;34:15161.
[5] Mahfuz H, Majumdar P, Saha M, Shamery F, Jeelani S. Integral manufacturing of
composite skin-stringer assembly and their stability analyses. Appl Compos
Mater 2004;11:15571.
[6] Makabe C, Murdani A, Kuniyoshi K, Irei Y, Saimoto A. Crack-growth arrest by
redirecting crack growth by drilling stop holes and inserting pins into them.
Eng Fail Anal 2009;16:47583.
[7] Goree JG, A. National aeronautics and space, O. Scientic and technical
information, and S. United. Preliminary investigation of crack arrest in
composite laminates containing buffer strips; 1978.
[8] Brunner A, Blackman B, Davies P. A status report on delamination resistance
testing of polymermatrix composites. Eng Fract Mech 2008;75(June):
277994.
[9] Hodgkinson JM. Mechanical testing of advanced bre composites. Woodhead
Publishing; 2000.
[10] ASTM-D5528-01. Standard test method for mode i interlaminar fracture
toughness of unidirectional ber-reinforced polymer matrix composites.
ASTM International, vol. (2007)e2; 2007.
[11] ASTM-D6671-06. Standard test method for mixed mode I-mode II interlaminar
fracture toughness of unidirectional ber reinforced polymer matrix
composites. ASTM International; 2006.
[12] JIS-7086. Japanese industrial standard testing methods for interlaminar
fracture toughness ofcarbonbre reinforcedplastics; 1993.
[13] Carlsson LA, Aksoy A. Analysis of interleaved end-notched exure specimen for
measuring mode II fracture toughness. Int J Fract 1991;52:6777.
[14] Liao FS, Lu WH, Su AC, Kao PW, Hsu TJ. Effect of interleaving on the impact
response of a unidirectional carbon/epoxy composite. Composites
1995;26:21522.
[15] Masters JE. Improved impact and delamination resistance through interleang.
Key Eng Mater 1989;37:31748.
[16] Singh S, Partridge IK. Mixed-mode fracture in an interleaved carbon-bre/
epoxy composite. Compos Sci Technol 1995;55:31927.
[17] Bhatia NM, Verette RM. Crack arrestment of laminated composites. Fract Mech
Compos 1976:200.
[18] Sendeckyj G. Concepts for crack arrestment in composites. ASTM Spec Tech
Publ 1976;593:215.
[19] Chan WS. Delamination arrester-an adhesive inner layer in laminated
composites. Compos Mater 1986:176.
[20] Sela N, Ishai O. Interlaminar fracture toughness and toughening of laminated
composite materials: a review. Composites 1989;20(September):42335.
[21] Hojo M, Ando T, Tanaka M, Adachi T, Ochiai S, Endo Y. Modes I and II
interlaminar fracture toughness and fatigue delamination of CF/epoxy
laminates with self-same epoxy interleaf. Int J Fatigue 2006;28(October):
115465.
[22] Sela N, Ishai O, Bankssills L. The effect of adhesive thickness on interlaminar
fracture toughness of interleaved cfrp specimens. Composites 1989;20(May):
25764.
[23] Gibson RF, Chen Y, Zhao H. Improvement of vibration damping capacity and
fracture toughness in composite laminates by the use of polymeric interleaves.
J Eng Mater Technol, Trans ASME 2001;123:30914.
[24] Ozdil F, Carlsson LA. Mode I interlaminar fracture of interleaved graphite/
epoxy. J Compos Mater 1992;26(1):43259.
[25] Jiang WEI, Tsang FFY, Tjong SC, Li RKY. Loading rate dependence of mode II
fracture behavior in interleaved carbon bre/epoxy composite laminates. Appl
Compos Mater 2006:3619.
[26] Lee SH, Noguchi H, Kim YB, Cheong SK. Effect of interleaved non-woven carbon
tissue on interlaminar fracture toughness of laminated composites: Part I
mode II. J Compos Mater 2002;36:2153.
[27] Lee SH, Noguchi H, Kim YB, Cheong SK. Effect of interleaved non-woven carbon
tissue on interlaminar fracture toughness of laminated composites: Part II
mode I. J Compos Mater 2002;36:2169.
[28] Lee S, Lee J, Cheong S, Noguchi H. A toughening and strengthening technique of
hybrid composites with non-woven tissue. J Mater Process Technol
2008;207(October):219.
[29] Yadav SN, Kumar V, Verma SK. Fracture toughness behaviour of carbon bre
epoxy composite with Kevlar reinforced interleave. Mater Sci Eng B
2006;32:10812.
[30] Sohn MS, Hu XZ. Comparative study of dynamic and static delamination
behaviour of carbon bre/epoxy composite laminates. Composites 1995;26:
849.
[31] Wicks SS, de Villoria RG, Wardle BL. Interlaminar and intralaminar
reinforcement of composite laminates with aligned carbon nanotubes.
Compos Sci Technol 2010;70(January):208.
[32] Garcia EJ, Wardle BL, John Hart A. Joining prepreg composite interfaces with
aligned carbon nanotubes. Compos Part A 2008;39:106570.
[33] Sihn S, Kim RY, Huh W, Lee K-H, Roy AK. Improvement of damage resistance in
laminated composites with electrospun nano-interlayers. Compos Sci Technol
2008;68:67383.
[34] Arai M, Noro Y, Sugimoto K-Ichi, Endo M. Mode I and mode II interlaminar
fracture toughness of CFRP laminates toughened by carbon nanober
interlayer. Compos Sci Technol 2008;68:51625.
[35] Warren GL, Sun L, Hadjiev VG, Davis D, Lagoudas D, Sue HJ. B-staged epoxy/
single-walled carbon nanotube nanocomposite thin lms for composite
reinforcement. J Appl Polym Sci 2009;112:2908.
[36] Zhang J, Lin T, Wang X. Electrospun nanobre toughened carbon/epoxy
composites: effects of polyetherketone cardo (PEK-C) nanobre diameter and
interlayer thickness. Compos Sci Technol 2010;70(October):16606.
[37] Akangah P, Lingaiah S, Shivakumar K. Effect of nylon-66 nano-ber
interleaving on impact damage resistance of epoxy/carbon ber composite
laminates. Compos Struct 2010;92:14329.
[38] Shivakumar K, Lingaiah S, Chen H, Akangah P, Swaminathan G, Russell L.
Polymer nanofabric interleaved composite laminates. AIAA J 2009;47(July):
17239.
[39] Li G, Li P, Yu Y, Jia X, Zhang S, Yang X, et al. Novel carbon ber/epoxy composite
toughened by electrospun polysulfone nanobers. Mater Lett 2008;62:5114.
[40] Wang WX, Takao Y, Matsubara T, Kim HS. Improvement of the interlaminar
fracture toughness of composite laminates by whisker reinforced
interlamination. Compos Sci Technol 2002;62:76774.
[41] Gao F, Jiao G, Lu Z, Ning R. Mode II delamination and damage resistance of
carbon/epoxy composite laminates interleaved with thermoplastic particles. J
Compos Mater 2006;41(March):11123.
[42] Groleau MR, Shi YB, Yee AF, Bertram JL, Sue HJ, Yang PC. Mode II fracture of
composites interlayered with nylon particles. Compos Sci Technol 1996;56:
122340.
[43] Heness G, Stevens M, Dossett B. The effect of surface treatment on
delamination for a nylon interleaving material. Mater Forum 2007:905.
[44] Gilbert E, Hayes B, Seferis J. Interlayer toughened unidirectional carbon
prepreg systems: effect of preformed particle morphology. Compos Part A
2003;34(March):24552.
[45] Chen S, Jang B. Fracture behaviour of interleaved ber-resin composites.
Compos Sci Technol 1991;41:7797.
[46] Li L, Lee-Sullivan P, Liew K. The inuence of thermoplastic lm interleaving on
the interlaminar shear strength and mode I fracture of laminated composites. J
Eng Mater Technol 1996;118:302.
[47] Jiang W, Tjong S, Chu P, Li R. Interlaminar fracture properties of carbon bre/
epoxy matrix composites interleaved with polyethylene terephthalate (PET)
lms. Polym Polym Compos 2001;9:1416.
[48] Pegoretti A, Cristelli I, Migliaresi C. Experimental optimization of the impact
energy absorption of epoxycarbon laminates through controlled
delamination. Compos Sci Technol 2008;68(10):265362.
[49] Matsuda S, Hojo M, Ochiai S, Murakami A, Akimoto H, Ando M. Effect of
ionomer thickness on mode I interlaminar fracture toughness for ionomer
toughened CFRP. Mater Res 1999;30:13119.
[50] Akimoto A, Shonaike GO, Usui Y, Aoki Y, Murakami A, Matsuda S. Fracture and
damping of ionomer interleaved epoxy composites. J Thermoplast Compos
Mater 2000;13:314.
[51] Fracasso R, Rink M, Pavan A, Frassine R. The effects of strain-rate and
temperature on the interlaminar fracture toughness of interleaved PEEK/CF
composites. Compos Sci Technol 2001;61(1):5763.
206 M. Yasaee et al. / Composites: Part A 43 (2012) 198207
[52] Armstrong-Carroll E, Iskandarani B, Kamel I, Donnellan TM. The inuence of
interleaf deformation behavior and lm-resin adhesion on the fracture toughness
of interleaved composites. In: Composite materials: fatigue and fracture: a
symposium sponsored by ASTM committee D-30 on high modulus bers and
their composites, Dallas, TX, 2425 October 1984, ASTM; 1986. p. 299.
[53] Brown R. Handbook of polymer testing: physical methods. CRC Press; 1999.
[54] Haibach K, Menner A, Powell R, Bismarck A. Tailoring mechanical properties of
highly porous polymer foams: silica particle reinforced polymer foams via
emulsion templating. Polymer 2006;47(June):45139.
[55] Hwang W, Han KS. Interlaminar fracture behavior and ber bridging of glass-
epoxy composite under mode I static and cyclic loadings. J Compos Mater
1989;23:396430.
[56] Compston P, Jar PYB. The inuence of bre volume fraction on the mode I
interlaminar fracture toughness of a glass-bre/vinyl ester composite. Appl
Compos Mater 1999;6:35368.
[57] Greenhalgh ES. Failure analysis and fractography of polymer
composites. Woodhead Publishing Ltd.,; 2009.
[58] Yasaee M, Bond IP, Trask RS, Greenhalgh ES. Mode II interfacial toughening
through discontinuous interleaves for damage suppression and control.
ComposPart A: Appl Sci Manuf 2012;43:12128.
M. Yasaee et al. / Composites: Part A 43 (2012) 198207 207