Polymer International Polym Int 51:12681276 (2002)

DOI: 10.1002/pi.940

Characterization of an ABS-modified epoxy

system
J Cano, A Torres, MJ Abad, L Barral,* FJ Dez, J Lopez
and C Ramrez
Departamento de Fsica, EUP Ferrol, Universidad de A Coruna. Avda 19 de Febrero s/n, 15405 Ferrol, Spain

Abstract: In this work an epoxy system containing a diglycidyl ether of bisphenol A (DGEBA) and
1,3-bis(aminomethyl)cyclohexane (1,3-BAC) is modied with poly(acrylonitrile-co-butadiene-co-
styrene) (ABS). Using dynamic mechanical analysis the glass transition temperatures and the
associated activation energies are determined in the neat epoxy and some blends. The presence of ABS
produces a constant diminution of the glass transition temperatures and increases the activation
energies. The brittle character of the neat epoxy and the blends, compared with the ductile character of
ABS, is studied using an instrumented impact pendulum. The shape of forcetime curves and energies
and data dispersion of each composition are analyzed. By using scanning electron microscopy it is
possible to see various zones of different roughness and to distinguish the regions of tension and
compression of Charpy impact fractured surfaces. The presence of a two phase-morphology in the
epoxy-ABS blends is also shown.
# 2002 Society of Chemical Industry

Keywords: ABS: DMA characterization; epoxy resins; fractography; instrumented impact

INTRODUCTION the state of molecular motion as temperature is

Crosslinked epoxy resins, obtained by the cure of
precursors (ie epoxy resins monomers and hardeners),
are among the most important thermosets for struc-
tural applications. One major drawback of thermosets
is their poor resistance to impact and to crack initiation
and propagation. Consequently, the improvement of
the fracture toughness of thermosets, while maintain-
ing other desirable properties, such as modulus and
glass transition temperature, Tg, is the aim of many
researches in the eld.1
One frequently used approach to toughening
thermosets is the addition of second-phase polymeric
material, such as liquid rubbers or thermoplastics. In
this work the aim is to characterize an epoxy system
obtained by reaction of a diglycidyl ether of bisphenol
A and a diamine hardener modied by addition of
different amounts of poly(acrylonitrile-co-butadiene-
co-styrene) (ABS). The brittle character of the un-
modied system is well known.2
Three techniques are used in this work to charac-
terize the modied epoxy system: dynamic mechanical
analysis (DMA), instrumented impact pendulum and
scanning electron microscopy (SEM).
Dynamic mechanical properties are the mechanical
properties of materials as they are deformed under
periodic forces. The dynamic mechanical technique
can provide valuable information about all changes in
scanned. This technique is, therefore, considered to
be one of the most effective for studying the inuence
either of molecular structure or of phase morphology
on the physical properties of natural and synthetic
polymers.3 DMA usually indicates the presence of
different transitions, such as the a and b transitions, by
the peaks in the tan d curve. It is well known that the a
and b transition peak positions appear shifted toward
higher temperatures when the frequency of scan
increases, and the activation energy of every transition
can be obtained.4
The energy to break a specimen in a conventional
(non-instrumented) impact pendulum is measured by
the difference of the heights of a pendulum hammer
before and after the impact. This energy is indicated by
an analogue display with idle pointer. In an instru-
mented impact pendulum a load sensor at the tup of
the striking hammer measures the force F that the
striker applies to the specimen during loading and
breaking of the specimen. The load F(t) measured in
time t is used to calculate, following Newton's law of
forces, the velocity v(t) of the pendulum hammer and
the displacement s(t) of the pendulum. Consequently,
it is possible to plot the force versus time or the force
versus displacement and the work or energy W to break
a specimen is obtained by integration. If the integra-
tion is not carried out over the entire impact process,

* Correspondence to: L Barral, Departamento de Fsica, EUP Ferrol, Universidad de A Coruna. Avda 19 de Febrero s/n, 15405 Ferrol, Spain
E-mail: labpolim@udc.es

Poster presentation Session D: Paper presented at the Polymers in the Third Millennium Conference, 26 September, 2001, Montpellier,
France
(Received 15 October 2001; revised version received 14 January 2002; accepted 6 February 2002)

# 2002 Society of Chemical Industry. Polym Int 09598103/2002/$30.00 1268


partial energy values can be obtained up to some
characteristic events of the load-time curve, by using
dedicated impact data analysis software.5 When the
instrumented pendulum has an incremental angle
encoder it is possible to calculate the energy absorbed
by a specimen from the maximum height of the
pendulum hammer after the impact.
The load signal measured in instrumented impact
tests shows characteristic oscillations that are inherent
to this measuring technique. These oscillations result
from the sudden loading to which the specimen is
subjected. Sometimes the amplitude of these oscilla-
tions is great and the amplied signal is accompanied
by electrical noise that complicates the detection of
characteristic events. It is possible to avoid this draw-
back and also improve the quality of the F(t) curve by
ltering the signal without signicatively altering the
energy quantities.6 Another consideration is that only
a certain part of the measured impact energy is used as
fracture energy for breaking the specimen, because
another part is converted into the translational and
rotational kinetic energies of the moving halves of the
broken specimen. These kinetic energy quantities are
more important for specimens that fail in a brittle
manner. For ductile specimens kinetic energies are
smaller or even negligible quantities.
SEM is very useful to examine the fracture surface of
a failed component and to determine the cause of
failure, initiation site, direction of crack propagation,
state of stress or loading conditions, effect of environ-
mental exposure, material defects or processing
deciencies. The topographic marks observed at the
fracture surface can help to identify the mechanism of
fracture of the epoxy systems analyzed.7,8
Another application of SEM frequently used in
blending is observation of the microstructure of
different compositions. The morphology of thermo-
plastic-modied epoxy resin is inuenced by the
amount of the modier and the cure conditions. With
lower thermoplastic modier contents, the thermo-
plastic domains are dispersed in epoxy-rich matrix and
are observed by SEM as a sea-island morphology.9
When the thermoplastic content is higher, a nodular
structure, with interconnected epoxy particles in the
thermoplastic is observed. At intermediate modier
contents, a dual-phase morphology having both sea-
island and nodular structures or cocontinuous mor-
phology can be observed in many systems.
In this study the impact fracture surfaces and
morphologies of the ABS-modied epoxy resin with
low contents of thermoplastic were analyzed by SEM.
EXPERIMENTAL
Materials
The epoxy resin used in this study was a commercial
diglycidyl ether of bisphenol A (DGEBA), Araldite
GY 260 from Ciba-Geigy, with weight per epoxy
equivalent of 205.1 g eq 1 as determined in our
laboratory by hydrochlorination.10 The neat epoxy
Polym Int 51:12681276 (2002)
Characterization of ABS-modied epoxy system
resin and its blends with poly(acrylonitrile-co-buta-
diene-co-styrene) (ABS), QI-300 with average mol-
ecular weight Mw = 163 500 and Mw /Mn = 2.59
manufactured by Polidux/Repsol, were cured with a
cycloaliphatic diamine hardener, 1,3-bis(amino-
methyl)cyclohexane (1,3-BAC), from Aldrich Chemi-
cals, having a molecular weight of 142.25 g mol 1 and
manufacturer purity value of >99% according to the
supplier. All components were commercial products
and were used without any further purication.
Blending and curing procedure
For neat epoxy and all mixtures the epoxy/amine ratio
was held constant and equal to 100/17 w/w. In order to
prepare epoxy resin/ABS mixtures with 5, 10 and 15
ABS per hundred parts of resin (phr) the correspond-
ing amount of dried ABS was dissolved in dichloro-
methane and mixed with the epoxy resin at room
temperature. The resulting solution was then heated at
8090 C and stirred in an oil bath to remove most of
solvent. When solvent was less than 0.1% w/w, the
binary mixture was cooled at room temperature and
the 1,3-BAC hardener was added and continuously
stirred during a few minutes. The mixture was poured
into a vertical U-shaped glass mould and cured in an
air circulating oven. The time and temperatures
scheduled in the cure were: 2 h at room temperature,
5 h at 40 C and 8 h at 60 C. Plates of 4 mm thick were
obtained at the end of cure process. These plates were
used to machine the samples for DMA and impact
tests.
Dynamic mechanical tests
The samples measuring 18  6  4 mm3 were analyzed
using a Perkin-Elmer DMA-7 with an intracooler
cooling accessory. All experiments were performed in
three-point bending measuring system and tempera-
ture scan mode between 50 and 250 C under a
helium ow rate of 40 ml min 1, at a temperature scan
rate of 5 C min 1. Frequencies used in dynamic
experiments were 1 Hz for Tg determination and 0.01,
0.1, 1 and 10 Hz for activation energy.
Instrumented impact tests
All samples used in Charpy impact tests had dimen-
sions of 80  10  4 mm3 as in ISO 179.11 The speci-
mens of neat epoxy and epoxy/ABS blends were
machined by milling from rectangular plates and the
neat ABS specimens were obtained directly by injec-
tion moulding.
Some specimens of every composition were V-
notched in accordance with ISO 179 and ISO
2818.12 Machined notches were obtained in an ATS
FAAR Notching Machine. Dimensions of notches
were: notch base radius of 0.25 mm, remaining width
at notch base of 8 mm and V-notched angle of 45.
Unnotched and V-notched specimens were
fractured in an instrumented impact pendulum
INSTRON-WOLPERT PW5 of nominal energy of
7.5 J and velocity of impact of 3.85 m s 1. Instru-
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J Cano et al
Figure 1. Storage modulus and loss factor, tan d, of 5 ABS phr.
mented tup used has maximum nominal force of 2 kN.
The Charpy tests were conducted at room tempera-
ture and more than ve specimens of every composi-
tion were tested.
Scanning electron microscopy
Impact fractured surfaces of neat epoxy and phase
morphology of some blends were examined using a
JEOL JSM-6400 scanning electron microscope. SEM
observation was performed using secondary electron
imaging and acceleration voltage of the electron beam
ranging between 10 and 15 kV. The fractured surfaces
of some blends were etched with dichloromethane to
observe phase morphology. All samples were coated
with a thin layer (1525 nm) of gold, using a high
vacuum gold sputterer, before observation by SEM.
RESULTS AND DISCUSSION
DMA characterization
Figure 1 shows results of a typical DMA test of the 5
ABS phr modied epoxy samples. The prominent
tan d peak is characteristic of the glass transition (a
transition). In the region of a transition the rise in tan d
is accompanied by a steep drop in the storage modulus
E '. Here the glass transition temperature, Tg, charac-
terized by the peak in tan d at 1 Hz is 84 C. At 50 C,
approximately, we can see another broad peak of low
intensity corresponding a secondary transition (b
transition). In the region of b transition a little step
in E ' curve is observed.
Table 1 presents results of DMA tests of neat epoxy
(0 phr) and three ABSepoxy blends. Values of Tg and
tan d are obtained in tests as in Fig 1 to characterize
glass transition by peak of tan d at 1 Hz. Energies of
activation, Ea, of a transition of neat epoxy and blend
Table 1. Glass transition temperatures, Tg, and
tan d measured in the peak of DMA tan d curve.
ABS phr Tg ( C) tan d Ea (kJ mol 1)
0 90 1.40 281.50
5 84 1.23 390.35
10 84 0.97
15 85 0.90
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Figure 2. Activation energies, Ea, of neat epoxy (a) and 5 ABS phr (b).
of 5 ABS phr are obtained from the slope of the
Arrhenius plots as shown in Fig 2. A moderate drop of
Tg of the blends can be observed in Table I. Drops of
Tg approximately constant for different contents of
thermoplastic were also observed by others.13
It is well known that if the Tg of a material is
relatively low the material is limited in its structural
applications, due to the low modulus at temperatures
above the Tg. Here, the origin of a relatively low Tg of
neat epoxy (90 C) and blends (85 C) is in the cure
schedule, and implies a material with a low degree of
crosslinking, due to the absence of a postcure step at a
more elevated temperature.
The low Ea of neat epoxy in Table I can also be
attributed to a low degree of crosslinking obtained
during cure. This neat epoxy with other cure schedules
and other similar epoxy systems with postcure at
elevated temperatures can reach activation energies of
400 kJ mol 1 or more.2,4,14 It is necessary to consider
here that experimental values of Ea also are affected by
other effects, such as heating rate and test frequencies
used.15 The increase of Ea in 5 ABS phr with respect to
neat epoxy can be related to the difculty associated
with three-dimensional motion of chains between
crosslinking points during the glassrubber transition
process produced by the presence of ABS dispersed in
the epoxy-matrix. There is a monotonic decrease in
the maximum of tan d as the ABS content increases. A
decrease in the height of the damping peak was also
observed in other modied systems.13
Instrumented impact pendulum
Figure 3 displays two types of curves: force or load (F )
Polym Int 51:12681276 (2002)

and work or energy (W ) versus time (t) obtained during
instrumented impact tests. The amplitudes of super-
imposed oscillations in the curve F(t) are diminished
by damping the tup with a strip of rubber and the noise
in the signal is ltered using an electronic lter of
10 kHz. The peak-to-peak amplitude of ltered noise
is less than 10 N as can seen in the curves F(t). The
shape of the curve F(t) of unnotched specimens is very
Figure 3. Some typical loadtime curves of unnotched (a, c, e) and V-notched (b, d, f) specimens of neat epoxy (a, b), neat ABS (c, d) and 5 ABS phr (e, f).
Polym Int 51:12681276 (2002)
Characterization of ABS-modied epoxy system
different from that for neat epoxy (Fig 3(a)), in which
load grows linearly until a maximum where unstable
crack propagation starts and for ABS (Fig 3(c)), in
which unstable crack propagation starts after F has
passed the maximum. The curve of Fig 3(a) is typical
of a brittle material and the curve of Fig 3(c) of a
ductile material.
Two characteristic parameters of both types of F(t)
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J Cano et al

curves are total impact time (time from F = 0 at t = 0 to related with the energy delivered from the pendulum
F = 0 after impact), that generally is of the order of ms, and absorbed during the break of unnotched and
and maximum force. Figure 3 shows that total impact notched specimens, respectively. Wt is the energy
time is greater for the ABS than for neat epoxy (2.5 ms absorbed, calculated from curve load-displacement.
and 0.75 ms, respectively), and maximum force are the An is the energy absorbed, calculated from angle
same in both curves; consequently the area under the F encoder output. E is the energy absorbed, directly read
curve and the energy absorbed W are clearly greater for by the analogue display with the idle pointer. The
the ABS than for neat epoxy samples (2 J and 0.4 J, values shown are mean values obtained in impacts of
respectively). In the F(t) curves of notched specimens more than ve specimens of every material. Every
(Figs 3(b) and 3(d) for neat epoxy and ABS, respec- mean value is accompanied of the corresponding
tively) we can see less total impact time and maximum coefcient of variation, CV (ratio of standard deviation
force than in corresponding unnotched specimens and mean value, expressed as a percentage), that is a
and, consequently, the energy absorbed in the impact measure of data dispersion. The Table show that the
of notched specimens is less than in the impact of a values of E and An are comparable for every material as
corresponding unnotched specimen. The shape of F(t) expected, accounting for data dispersion, and values of
curve in Fig 3(d) for ABS, where the crack initiated Wt are less than the respective E and An.
after reaching maximum force, and the energy The value of Wt, is clearly greater in ABS than in
absorbed W, which is approximately three times that neat epoxy or in the compositions of 5 or 10 ABS phr,
of W in Fig 3(b) for epoxy, is related with the ductile both for unnotched and notched specimens. These
and brittle character, respectively of both materials. values are related to the ductile or brittle character of
Hence, some distinctive aspects of ductile and brittle the respective materials.
materials appear in both unnotched and notched Also it can seen that Wt values obtained for the
specimens impact tests. unnotched specimens of all four materials studied are
Also in Fig 3(d), the area under the F(t) curve (and greater than respective value of notched specimen.
consequently the energy absorbed or work of fracture) This behaviour is general for polymeric and composite
can be partitioned into two parts as in the fracture of materials17 because notch facilitates the start of cracks
notched specimens of other ductile materials.16 The in the tip of notch that is a site of stress concentration.
`crack initiation work' is associated with the area of the The presence of ABS seems to improve the value of Wt
F(t) curve from the start of impact (F = 0, t = 0) until a of unnotched 5 ABS phr blend but not in 10 ABS phr
deep drop where the crack initiated after maximum of nor notched blends; this conclusion must be taken
F, and the `crack propagation work' is associated with with caution because data dispersion is relatively great
the residual area from crack initiation until the end of as indicated by the CV.
the impact. Table 2 also shows smaller CVs for ABS than for the
At a glance, F(t) curves of 5 ABS phr (Figs 3(e) and other three materials based on epoxy. This can be
3(f) for unnotched and notched specimens, respec- related with the process to obtain each material and to
tively) are more similar to curves of neat epoxy than of the manufacture of the specimens. Specimens of ABS
ABS. Nevertheless the F(t) curve of Fig 3(e) shows a were obtained directly by injection while specimens of
total time to impact and maximum force greater than neat epoxy and blends were machined (sowing and
that in Fig 3(a) of neat epoxy and, consequently, the milling) from plates as explained. It is well known that
energy absorbed in the impact of unnotched speci- the preparation of test specimens by machining
mens of 5 ABS is greater than the energy absorbed in inuences the nished surfaces and even the internal
the impact of neat epoxy. In the impact of notched 5 structure of the specimens.12 As a consequence it is
ABS phr the energy absorbed is practically the same as more probable to nd defects (trapped air bubbles,
that of the notched neat epoxy. scratches, dispersion in dimensions, etc) in machined
Table 2 shows the three parameters, Wt, An and E specimens than in those specimens obtained by
injection and so initiation of crack and fracture is less
random in ABS specimens. This could also explain the
Table 2. Mean values of fracture energies of unnotched specimens and of
V-notched specimens.
lower CV values for notched compared with un-
notched specimens because the presence of notches
ABS phr Wt (J) CV (%) Av (J) CV (%) E (J) CV (%) produces in all specimens an identical site of stress
Unnotched concentration which initiates the crack growth that
0 0.32 39 0.51 29 0.64 28 originates the fracture in less random conditions.
5 0.55 40 0.83 29 0.88 33
10 0.25 35 0.48 25 0.47 24 Scanning electron microscopy
Neat ABS 1.95 18 3.05 23 3.37 18 SEM was utilized in this work to observe the Charpy
V-notched impact fracture surfaces and to detect presence of
0 0.07 29 0.20 16 0.23 16 separated phases in the blends.
5 0.05 11 0.26 11 0.20 2
Figure 4 shows the impact fracture surface of un-
10 0.06 15 0.22 14 0.23 9
notched neat epoxy. Figure 4(a) displays the overall
Neat ABS 0.22 4 0.56 5 0.63 3
fracture surface (10  4 mm2). Fracture initiates in the

1272 Polym Int 51:12681276 (2002)


Figure 4. Impact fractured surface of neat epoxy. Overall surface (a) and right to left zones (b, c, d, e).
right side, that is the opposite to the impact of the tup,
and crack advances right to left. In this SEM
micrograph, obtained with very low magnication
(14), various zones of different roughness are
observed and were denotated b, c, d, e and f, right to
left. Figures 4(b), 4(c), 4(d), 4(e) and 4(f) are the
1000 amplication of such zones (except Fig 4(e)
that is only 100 amplied, for clarity).
Roughness is at a minimum in zone b (near the edge
where crack initiated) and in zone f. In both of these
zones (Figs 4(b) and 4(f)) some parabolic marks can
be seen. Roughness is at a maximum in zone d, c and e
being transition zones of intermediate roughness.
It is known that this neat epoxy and other
materials,2,18 when broken in tension tests, present a
Polym Int 51:12681276 (2002)
Characterization of ABS-modied epoxy system
fracture surface with four characteristic zones corre-
sponding to the defect where failure is initiated and the
zones b, c and d. The presence of similar zones on the
right region of fracture surface of Charpy specimens of
Fig 4(a) can be explained by considering that the right
edge of specimens, where the crack is initiated, is
under tension and the opposite edge is under com-
pression in this three-point bending test. Figure 5
presents the different zones of fracture surface grouped
into the two regions (tension and compression) that
can be distinguished in Fig 4(a).
The complete fracture surfaces of the neat ABS and
5 ABS phr composition are shown in Figs 6(a) and
6(c), respectively, where cracks propagated also right
to left. Figures 6(b) and 6(d) are the 1000 magni-
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J Cano et al
Figure 5. Scheme of zones b, c and d in the tension region and zones e
and f in the compression region of Charpy impact fractured surface of neat
epoxy. Crack propagated right to left.
cation of the central region of the respective fracture
surfaces. Surface roughness is slightly different from
that of the neat epoxy, but it is also possible to
distinguish the regions of tension and compression.
The SEM micrographs of Fig 7 were obtained by
etching some specimens of ABS (Figs 7(a) and 7(c))
and 10 ABS phr (Figs 7(b) and 7(d)). The 10 000
magnication shows small domains (lesser than 1 mm)
of the dispersed phase ABS in the epoxy matrix. These
black domains in the photomicrograph are the holes
that remain after eliminating the ABS of the material
surface during the etching process. These ABS
domains are regularly distributed within the volume
of the specimen. Most of ABS domains seen in Fig
7(a) are uniform in shape with sizes below 0.5 mm. In
Figure 6. Impact fracture surface of ABS (a, b) and 5 ABS phr (c, d).
1274
Fig 7(b), corresponding to material with 10 ABS phr,
the shapes of the domains are more irregular and sizes
are greater than in the material with 5 ABS phr, as
expected since the epoxy-thermoplastic blend shows
sea-island morphology.
It is well known that the morphology of thermo-
plastic-epoxy depends on curing temperature and
thermoplastic content. It is also known that other
similar thermoplastic modied9,19 epoxies separate
into two phases during the cure process and that cured
thermoplastic blends show sea-island morphology
with the thermoplastic phase dispersed in the epoxy
matrix when the content of thermoplastic in the blend
is less than 10%. Other morphologies are possible
when the content of thermoplastic increases. Sea-
island morphology is not essentially affected by
addition of a postcured step in the cure schedule of
ABS-epoxy blends, as shown in Figs 7(c) and 7(d) for
5 ABS phr and 10 ABS phr, respectively, postcured
24 h at 150 C. This can be explained because phase
separation and morphology are essentially xed prior
to vitrication, which happens during the rst steps of
cure in this case.
CONCLUSIONS
The presence of ABS altered the values of glass
transition temperatures and associated activation
energies of different compositions compared with the
neat epoxy. The reductions in the glass transition
Polym Int 51:12681276 (2002)

Figure 7. Sea-island morphology in ABS modified epoxy of 5 ABS phr (a, c) and 10 ABS phr (b, d). Blends postcured at 150C (c, d).
temperatures of modied systems are practically the
same (5 C) in the three compositions studied. The
absence in the cure schedule of a postcure step at a
more elevated temperature is responsible of the low
activation energy value and relatively low Tg obtained
for neat epoxy and blends.
Energies absorbed, maximum force and total time
to fracture unnotched specimens are clearly greater
than for V-notched specimens of every composition.
Data dispersion is also greater in the unnotched
specimens. Data dispersion is less in neat ABS than
in neat epoxy and blends because ABS specimens
obtained by injection are more uniform in composition
and dimensions than machined neat epoxy and blend
specimens. Neat ABS absorbs much more energy than
neat epoxy in line with their ductile and brittle nature,
respectively, as evidenced in loaddisplacement or
loadtime curves obtained during instrumented im-
pact tests.
Using SEM it is possible to see various zones of
different roughness in the regions of tension and com-
pression of impact surfaces of the neat and the ABS
modied epoxies. Epoxy modied by 5 and 10 ABS
phr presents phase separation and shows a sea-island
morphology that is not altered by addition of a
postcure step. The size of dispersed ABS domains
increases with ABS content in the blends.
Polym Int 51:12681276 (2002)
Characterization of ABS-modied epoxy system
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