Mechanical and morphological properties of y ash/epoxy

composites using conventional thermal and microwave curing methods

T. Chaowasakoo, N. Sombatsompop
*
Polymer Processing and Flow (P-PROF) Group, School of Energy, Environment and Materials, King Mongkuts University of Technology
Thonburi (KMUTT), Bangmod, Thungkru, Bangkok 10140, Thailand
Received 3 March 2006; received in revised form 20 December 2006; accepted 19 January 2007
Available online 31 January 2007
Abstract
Conventional thermal and microwave curing methods were utilized to cure y ash/epoxy composites, and the mechanical and mor-
phological properties of the composites were evaluated. The conventional thermal curing was performed at 70 C for 80 min while micro-
wave curing was carried out at 240 W for 18 min in order to achieve the optimum cure of the composites, determined using Dierential
Scanning Calorimeter. The results suggested that the tensile and exural moduli of the composites increased with increasing y ash con-
tent while the eect became opposite for tensile, exural and impact strengths, and tensile strain at break. Improved mechanical prop-
erties of the composite could be obtained by addition of N-2(aminoethyl)-3-aminopropyltrimethoxysilane coupling agent, the contents of
0.5 wt% being recommended for the optimum mechanical properties. Beyond these recommended contents, the mechanical properties
greatly reduced, except for the exural modulus. The comparative results indicated that the composites by the microwave cure consumed
shorter cure time and had higher ultimate strengths (especially impact strength), and strain at break than those by the conventional ther-
mal cure. The composites with higher tensile and exural moduli could be obtained by the conventional thermal cure.
2007 Elsevier Ltd. All rights reserved.
Keywords: A. Coupling agents; B. Mechanical properties; B. Curing; Fly ash; A. Polymermatrix composites
1. Introduction
Ash residues are wastes of coal-red power plants and
they are produced at the boiler outlet of the plants, these
including y ashes and bottom ashes [1]. The demand for
lightweight materials, such as for concrete construction
applications, with high strength and stiness has led to
the development of y ash based thermosetting resins.
There have been a small number of material technologists
having interests in using of the y ash (FA) as ller in poly-
mer materials [26]. Chand [2] studied the eect of volume
fraction of y ash on the mechanical properties of unsatu-
rated polyester composites, and found that increasing the
volume fraction of y ash reduced the tensile and impact
strengths of the composites, this corresponding to the work
by Kishore et al. [3] for epoxy composite system. In bre-
epoxy composites, the addition of y ash led to a reduction
of the density and an increase in modulus of the compos-
ites, the latter eect being caused by an improved disper-
sion of the ber in the matrix [4]. The use of y ash
particles as ller in rubber materials has expanded the use-
fulness of the y ash particles. Garde et al. [5] indicated
that the mechanical properties of polyisoprene rubber
loaded with ash particles were still inferior to that lled
with silica. Sombatsompop et al. [6] suggested that y ash
(FA) particles contained 3040% of silica which could be
used as reinforcing or extending ller in natural rubber
(NR) compound. Further work by Thongsang and Som-
batsompop [7] suggested that the y ash particles could
become a reinforcing ller to improve the mechanical prop-
erties of FA/NR composites, after surface treatment by bis-
(3-triethoxysilylpropyl) tetrasulfane (Si69) at 2.04.0% wt.
At present, epoxy resins are widely used in various
engineering and structural applications such as electrical
0266-3538/$ - see front matter 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2007.01.016
*
Corresponding author. Tel.: +66 2 470 8645; fax: +66 2 470 8647.
E-mail address: narongrit.som@kmutt.ac.th (N. Sombatsompop).
www.elsevier.com/locate/compscitech
Composites Science and Technology 67 (2007) 22822291
COMPOSITES
SCIENCE AND
TECHNOLOGY
industries, and commercial and military aircrafts indus-
tries. In order to improve their processing and product per-
formances, and to reduce cost, various llers are
introduced into the resins during processing [8]. Most llers
used in the epoxy resins include inorganic [9,10], organic
[11,12] and ceramic materials [13,14]. It is accepted that
the properties of epoxy composites can be altered by the
characteristics of the llers including shape, size, volume
fraction in the resin, as well as the modication of the ller
surfaces. It can be expected that composites between
hydrophobic thermosetting materials and hydrophilic y
ash particles are incompatible and led to poor interfacial
bonding and inferior mechanical properties [1519].
Hydroxyl groups on the y ash surfaces usually cause clus-
ter or agglomerate between themselves and lead to strong
llerller interaction in the polymer matrices [20]. There-
fore, many silane coupling agents are applied to promote
adhesions between the thermosetting matrices and the y
ash [1618]. The mechanism of the polymer-ash interaction
involves formation of siloxane bonding [15,21].
Curing of thermosetting resins is usually carried out by
conventional heating oven which involves a direct applica-
tion of thermal energy from heaters to the resins. It has
been evidenced that this thermal curing introduces a num-
ber of processing related problems such as long curing
times and large temperature gradients [2224]. A micro-
wave curing has been referred to as ecient alternative
energy source for curing thermosetting resins and their
composites because curing by the microwave can reduce
the cure time and increase the crosslink rate [2530]. In
addition, the microwave irradiation allows more ecient
curing, more uniform cure and improved physical/mechan-
ical properties of the materials [3134].
According to literature, there have been a number of
published papers on using the microwave irradiation for
curing the epoxy composites [2630,3538], but none of
these have published on the microwave curing of y ash
lled epoxy composites. In this work, y ash particles were
chemically treated and introduced in epoxy resin, and the
composites were cured by conventional thermal and micro-
wave cures. The eect of y ash contents, chemical surface
treatment and curing systems were discussed based on the
changes in mechanical and morphological properties of
the composites.
2. Experimental
2.1. Raw materials
The epoxy prepolymer used was a diglycidyl ether of
bisphenol-A-(DGEBA) and the hardener was 3-amino-
methyl-3,5,5-trimethylcyclohexyl-amine (isophorone dia-
mine). The epoxy prepolymer and the hardener were
supplied by I-Chem Co., Ltd. (Bangkok, Thailand). Table
1 shows the chemical structures and descriptions of both
prepolymers. The resin and the hardener were mixed in a
ratio of 100:60 by weight as recommended by the supplier.
The y ash (FA) particles were suppiled by Mae Moh
Power Station of KNR Group Co., Ltd. (Lampang,
Thailand). The dimensions and shape of the FA particles
were examined using a JEOL JSM-6301F SEM machine
(Tokyo, Japan), and found that FA was made of round-
shaped particles with relatively smooth surfaces. The aver-
age particle size and pH of the FA used were 50100 lm
and 9.5, respectively. An X-Ray Fluorescence Spectrome-
ter (XRF Model MESA-500 W, Horiba Ltd., Japan) was
used for analyzing the chemical compositions of the FA.
It was found that the major component of FA was SiO
2
,
this being about 46%. In this work, the FA content was
varied from 0 to 80 phr.
2.2. Surface treatment of the y ash particles by silane
coupling agent
N-2(Aminoethyl)-3-aminopropyltrimethoxysilane (KBM-
603), supplied by Shin-Etsu Co., Ltd. (Japan), was used as
a chemical coupling agent for FA surface treatment. The
FA particles were carefully dried before use in an oven
Table 1
The chemical structures and descriptions of the epoxy, isophorone diamine and KBM603
Chemical description Chemical structure
DGEBA
Isophorone diamine
KBM603
T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291 2283
for 24 h at 80 C. Deionized water was prepared, and the
silane coupling agent was slowly dropped into the mixture
until the required concentration was met. In this work,
KBM603 content was varied from 0 to 1.5 wt% of the
FA content. The FA particles were then added into the
solution with a further 15 min stirring in order to ensure
a uniform distribution of the coupling agent on the FA sur-
face before dried at 100 C for 24 h in an oven.
2.3. Sample preparation
The epoxy resin and hardener were mixed together in a
ratio of 100:60 by weight. This mixture was gently stirred
to avoid bubbles in the polymer. The y ash particles were
then slowly added at desired concentrations (from 20 to 80
phr) into the mixture and stirred for 20 min to ensure a
good mixing of the composite. After that, the composites
were de-gassed at room temperature for another 15 min.
In conventional (CV) cure, the FA/epoxy composite was
compression-moulded using two metal plates whose dimen-
sions were 200 200 mm
2
. A metal spacer of 3 mm thick
was used to control the thickness of the composite sheets
during the moulding. The prepared mixture was then
slowly poured in the mould and left to cure in a heating
oven. The optimal curing temperature and time were deter-
mined using a dierential scanning calorimeter (DSC).
In microwave (MW) cure, the FA/epoxy composite was
compression-moulded using two teon plates whose
dimensions were 180 50 mm
2
. A teon spacer of 3 mm
thick was used to control the thickness of the composite
sheets. The prepared mixture was then slowly poured in
the mould and left to cure in a multimode microwave oven
(Sharp Appliances Co., Ltd, Model: R-212 Bangkok, Thai-
land), operating at 2.45 GHz and using the on/o control
(times on and o were 12 and 20 s, respectively, at
240 W). All the y ash/epoxy composite samples were
placed at the same position throughout the work. In order
to give a good distribution pattern of the microwave eld,
all the composite samples were carefully placed near the
edge of the continuously rotating glass-plate in the micro-
wave oven. The cure times were xed at 18 min and the per-
centage cure of the composites was measured by the DSC.
In this work, the selected supplied power used in the micro-
wave was xed at 240 W, which was specied by the micro-
wave supplier (Sharp Model: R-212). The y ash/epoxy
samples produced at this microwave average power
(240 W) were reproducible in shape and had a least amount
of bubbles. It was aware that varying microwave powers
could aect the curing proles of the composite material
[39].
2.4. Characterizations
2.4.1. Cure characteristics
A dierential scanning calorimeter (Pyris1 DSC, Perkin
Elmer, NC, USA) was used to monitor the percentage cure
after the epoxy/amine resin was thermally or microwave
heated. The sample weight for such analysis was 3 mg.
The sample was scanned in a DSC pan at a heating rate
10 C/min with a temperature range from 25 to 200 C.
The optimal curing temperature in conventional oven were
selected from interval approximately 10 C below the onset
temperature of cure and a point midway to the maximum of
the exothermic DSC peak [38]. Based on this procedure, the
range of optimal curing temperatures were determined in
the DSC scans, and then fresh samples were analyzed iso-
thermally at the curing temperatures. The residual enthalpy
of curing for the partially cured resin for dierent times was
analyzed at the same heating rate and temperature range.
Samples that had been heated in a microwave oven for dif-
ferent times were also analyzed using the same technique.
This information was used to nd the cure time required
using the microwave (MW) and conventional (CV) curings,
and the percentage cure for the cured samples can be deter-
mined by considering the total enthalpy of a full crosslink-
ing reaction from the uncured epoxy sample under
exothermic condition (DH
Rxn
) and the total enthalpy of a
full crosslinking reaction from the partially cured sample
(DH
r
). The dierence in the DH
Rxn
and DH
r
values over
the DH
Rxn
simply indicates the percentage cure of the par-
tially cured sample, which is expressed shown as Eq. (1).
Percentage cure %
DH
Rxn
DH
r
DH
Rxn
100 1
2.4.2. Mechanical properties
Tensile properties of the composites were tested accord-
ing to ASTM D638 (1999) Type I (test speed of 50 mm/
min) using a universal testing machine (Autograph AG-I,
Shimadzu, Tokyo, Japan). Flexural properties of the com-
posites were performed according to ASTM D790 (1999) at
test speed of 1.3 mm/min) using a universal testing
machine. (Autograph AG-I, Shimadzu, Tokyo, Japan).
The un-notched izod impact test (Yasuda Impact Tester
Model 258, manufactured by Yasuda Seiki Seisakusho
LTD., Nishinomiya, Japan) was employed. The sample
dimension (50 mm 10 mm 3 mm) for the impact test
does not conform to ASTM specications, but relative
comparison of performance was envisaged in this study.
2.4.3. Scanning electron microscopy (SEM) studies
FA/epoxy composite samples subjected to impact were
examined with a JEOL (JSM-6301 F) (Tokyo, Japan)
SEM machine at 15 kV accelerating voltage. Fractured sur-
face of the composite samples from impact testing were
coated gold in an ion sputtering unit before failure mecha-
nisms were investigated.
3. Results and discussion
3.1. Eects of y ash content and curing techniques
Fig. 1 shows tensile curves for untreated-y ash/epoxy
composites cured by conventional thermal (CV) and
2284 T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291
microwave (MW) systems. It was found that the y ash/
epoxy composites cured from both systems exhibited a brit-
tle behavior, but the eect of y ash content on the tensile
curves was more pronounced for the MW cure. Fig. 2 com-
pares the tensile and the exural moduli with untreated y
ash content for the y ash/epoxy composites cured by CV
and MW ovens. For the both curing systems, it was found
that the increases in tensile and exural moduli of the com-
posites due to the addition of y ash can be considered in
two zones, one being 040 phr FA and the other being
4080 phr FA. The addition of y ash had more pro-
nounced eect on the tensile and exural moduli at below
40 phr. Beyond these concentrations, the eect became
minimized. The increased tensile and exural moduli were
associated with the higher modulus of y ash [10]. When
considering the eect of curing systems, it was observed
that the moduli of the MW cured composites were lower
than those of the CV cured composites. The dierence in
the properties of these two composites can be explained
by the dierence in percentage cures of these two compos-
ites curing systems whose results are shown in Table 2. It
was found that the percentage cure for the CV curing
was higher than that for the MW curing.
The tensile and exural strengths of untreated y ash/
epoxy composites cured by CV and MW systems are shown
in Fig. 3. It can be seen that the tensile and exural
strengths decreased slightly with increasing y ash content,
but these properties did not change much after 40 phr y
0
5
10
15
20
25
30
35
40
45
50
1 3 5 7 9
Tensile strain (%)
T
e
n
s
i
l
e

s
t
r
e
s
s

(
M
P
a
)
FA0CV
FA20CV
FA40CV
FA60CV
FA80CV
0
5
10
15
20
25
30
35
40
45
50
0 2 4 6 8
Tensile strain (%)
T
e
n
s
i
l
e

s
t
r
e
s
s

(
M
P
a
)
FA0MW
FA20MW
FA40MW
FA60MW
FA80MW
Fig. 1. Tensile curves of untreated y ash/epoxy composites with varying y ash contents: (a) conventional curing and (b) microwave curing.
0.4
0.6
0.8
1
1.2
1.4
1.6
0 20 40 60 80
Fly ash content (phr)
0 20 40 60 80
Fly ash content (phr)
T
e
n
s
i
l
e


m
o
d
u
l
u
s


(
G
P
a
)
CV
MW
0.5
1
1.5
2
2.5
3
3.5
4
4.5
F
l
e
x
u
r
a
l


m
o
d
u
l
u
s


(
G
P
a
)
CV
MW
Fig. 2. Eect of y ash content on tensile and exural moduli for conventional (CV) and microwave (MW) cured y ash/epoxy composites: (a) tensile
modulus and (b) exural modulus.
Table 2
The percentage cures of the composites from the conventional and
microwave curing systems
Curing condition Percentage cure (%)
The conventional curing (70 C 80 min) 99.9
The microwave curing (240 W 18 min) 96.8
T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291 2285
ash. The decreases in these ultimate mechanical strengths
of the composites were probably caused by an incompati-
bility of the ash particles and the epoxy matrix, leading
to poor interfacial bonding. Specically, it was found that
the y ash particles formed a cluster or agglomerate among
themselves, resulting in a llerller interaction and a poor
interfacial bonding, due to strong polarity of hydroxyl
groups on the y ash surfaces [40]. For the eect of curing
system, it was observed that the tensile and exural
strengths for the MW cured composites were slightly
higher than those for the CV cured composites [41].
Fig. 4 illustrates the impact strength and tensile strain at
break for the y ash/epoxy composites with untreated y
ash content, cured by CV and MW ovens. It was found
that the eect of curing technique was much more pro-
nounced for the impact strength (Fig. 4a), as compared
with the tensile and exural strength. Therefore, the expla-
nations for the dierences in the mechanical properties of
the composites inuenced by the curing techniques were
focused on the impact strength. The greater impact
strength obtained from the MW cure could be reasoned
with regard to temperature-cure gradient eects and SEM
fracture surfaces as follows:
Temperature-cure gradient eects: The dierence in
impact strength of the composites may be related to
the dierence in temperature gradients across the speci-
men thickness under these two curing systems. The tem-
perature distribution during MW cure was more
uniform through specimen, due to the fact that the
microwave could interact with materials by a polariza-
tion process [29]. In contrast, the CV curing was more
dependent on heat conduction and convection eects;
as a result, the conventional cured composite had a large
temperature gradient across the specimen thickness.
Due to the large temperature gradient in the CV system
0
10
20
30
40
50
60
70
80
0 20 40 60 80
Fly ash content (phr)
0 20 40 60 80
Fly ash content (phr)
T
e
n
s
i
l
e


s
t
r
e
n
g
t
h


(
M
P
a
)
CV
MW
30
40
50
60
70
80
90
F
l
e
x
u
r
a
l


s
t
r
e
n
g
t
h


(
M
P
a
)
CV
MW
Fig. 3. Eect of y ash content on tensile and exural strengths for conventional (CV) and microwave (MW) cured y ash/epoxy composites: (a) tensile
strength and (b) exural strength.
0 20 40 60 80
Fly ash content (phr)
0 20 40 60 80
Fly ash content (phr)
2
4
6
8
10
12
14
16
18
I
m
p
a
c
t


s
t
r
e
n
g
t
h


(
k
J
/
m
2
)
CV
MW
0
2
4
6
8
10
12
14
16
T
e
n
s
i
l
e


s
t
r
a
i
n


a
t


b
r
e
a
k


(
%
)
CV
MW
Fig. 4. Eect of y ash content on impact and tensile strengths for conventional (CV) and microwave (MW) cured y ash/epoxy composites: (a) impact
strength and (b) tensile strain at break.
2286 T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291
some internal stresses were expected to develop, causing
the lower impact strength [42]. The crosslink (closely
associated with % cure) distribution for the MW cured
composites was also expected to be more uniform than
that for the CV cured composites. This view was also
supported by Thostenson and Chou [23] who studied
the eect of MW and CV curing systems on the temper-
ature distribution and % cure of glass/epoxy composites,
and found a signicant lag of 60 C between the centre
and surface of the composite thickness during the CV
cure, and the composite at the centre had gelled faster
and thus a higher degree of cure as compared to the sur-
face part, this temperature lag being not the case for the
microwave-cure sample. They also observed a higher
resistance to visible cracks in the composites cured by
MW method.
SEM fracture surfaces: SEM micrographs of the frac-
ture surfaces for epoxy resin cured by MW and CV sys-
tems are shown in Fig. 5. It was observed that the
fracture surfaces from the CV cure (Fig. 5a and b) were
smooth and at-clean whereas those from the MW cure
(Fig. 5c and d) were rough and more ductile.
Fig. 4b compares the tensile strain at break with varying
untreated y ash contents for the composites cured by CV
and MW methods. It was found that the tensile strain at
Fig. 5. SEM micrographs of the conventional and microwave cured epoxy resin (50 and 500 magnication): (a) conventional curing (50),
(b) conventional curing (500), (c) microwave curing (50), and (d) microwave curing (500).
0.4
0.6
0.8
1
1.2
1.4
1.6
T
e
n
s
i
l
e

m
o
d
u
l
u
s

(
G
P
a
)
0.0 0.5 1.0 1.5
FA20 FA80
KBM603 content
CV
MW
CV
MW
10
20
30
40
50
60
70
T
e
n
s
i
l
e

s
t
r
e
n
g
t
h

(
M
P
a
)
0.0 0.5 1.0 1.5
FA20 FA80
KBM603 content
CV
MW
CV
MW
Fig. 6. Tensile modulus and tensile strength of the y ash/epoxy composites with 20 and 80 phr for conventional (CV) and microwave (MW) cures at
dierent KBM603 contents: (a) tensile modulus and (b) tensile strength.
T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291 2287
break of composites slowly decreased with addition of ash
particles. The explanation for this was a decrease in the
matrix homogeneity and the incompatibility of the matrix
and the ller as discussed earlier on. It was noticeable that
the tensile strain at break for the MW cured composites
was slightly higher than that for the CV cured composites,
the explanation being the same as given for the impact
strength result.
3.2. Eects of silane coupling agent content and curing
techniques
The eect of surface treatment on y ash particles by
silane coupling agent (KBM603) was discussed through
the results shown in Figs. 610. In this part, two selected
contents of y ash particles were used, i.e., 20 phr for
low FA loading and 80 phr for high FA loading.
Fig. 6 shows the eect of KBM603 content on the tensile
modulus and tensile strength of the y ash/epoxy com-
posites. The tensile modulus was found to increase to a
maximum value at KBM603 content of 0.5 wt% ash par-
ticles, and then slightly decreased with higher KBM603
loadings. Similar behavior was found for the tensile
strength of the composites. The optimum KBM603 at
0.5 wt% y ash to be added in the composites agreed
with Abel et al. [43]. It also seemed that the changing
trends in the tensile modulus and tensile strength were
a function of KBM603 content. The composites with
the optimum KBM603 (0.5 wt%) content indicated rela-
tively high interfacial bonding between the y ash and
the epoxy in association with ether linkages formed by
the chemical reactions of the coupling agent and y ash
particles, and NC linkages between the amino groups
in the coupling agent and the epoxy resin, the schematic
mechanism being given in Fig. 7. The decrease in the ten-
sile properties at high KBM603 contents (above 0.5 wt%)
was related to a self-condensation reaction of the hydro-
lyzed or partially hydrolyzed coupling agents, resulting in
a formation of exible polysilanol molecules on the y
ash surfaces. These exible polysilanol molecules proba-
bly reduced the reactivity of the epoxy resin and the cou-
pling agent, and thus resulting in a decreased diusion of
the epoxy resin into the polysiloxane network. This was
supported by Culler et al. [44] who stated that the reac-
tivity of the c-aminopropyltriethyoxysilane (c-APS) and
epoxy resin was dependent on the extent of self-conden-
sation reaction. Similar reasons were given for the
changes in the exural and impact strengths of the com-
posites whose results are shown in Fig. 8. This explana-
tions for the changes in tensile properties of the
composites can be supported by SEM micrographs in
Fig. 9, showing the fracture surfaces of the y ash/epoxy
Fig. 7. A model of the treated y ash/epoxy composites using KBM603
concentration 0.5 wt% of the y ash.
20
30
40
50
60
70
80
90
100
F
l
e
x
u
r
a
l

s
t
r
e
n
g
t
h

(
M
P
a
)
0.0 0.5 1.0 1.5
FA20 FA80
KBM603 content (%wt)
CV
MW
CV
MW
3
4
5
6
7
8
9
10
I
m
p
a
c
t

s
t
r
e
n
g
t
h

(
k
J
/
m
2
)
0.0 0.5 1.0 1.5
FA20
FA80
KBM603 content (%wt)
CV
MW
CV
MW
Fig. 8. Eect of KBM603 content on exural and impact strengths for conventional (CV) and microwave (MW) cured y ash/epoxy composites with 20
and 80 phr y ash: (a) exural strength and (b) impact strength.
2288 T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291
composites (20 phr) at high [Fig. 9a for 0.5 wt%
KBM603] and low [Fig. 9b and c for 1.0 and 1.5 wt%
KBM603, respectively] tensile strengths. From Fig. 9a,
it was found that the composite with 0.5 wt% KBM603
exhibited elongated ductile-fractured line around y ash
particles, indicating a good interfacial bonding between
the y ash and the epoxy matrix. This was not seen for
the composites with 1.01.5 wt% KBM603 concentrations
(Fig. 9b and c). When considering the eect of curing
system in Fig. 6, it was found that for all KBM603 con-
tents, the tensile modulus for the microwave cured com-
posites were slightly lower than that for the conventional
cured composites, but the opposite eect was observed
for the tensile strength.
Fig. 10 shows that the exural modulus increased with
increasing KBM603 content, this being an opposite eect
for the tensile modulus of the composites by varying
KBM603 contents. The dierence may be caused by the
exible polysilanol molecules formed by high KBM603
contents under tensile and exural deformations. Under
exural test, the polysilanols on the ash surfaces may have
a synergetic eect to resist the bending forces although they
had reduced a diusion of the epoxy resin into the poly-
siloxane network [44].
In summary, it was qualitatively observed that both
CV and MW curing systems had their individual eects
on the properties of the ash/epoxy composites. The CV
cure oered better modulus properties whereas the MW
cure gave better ultimate properties and used shorter cure
time [34]. In this work, the cure time used for the MW
cure was 18 min where that for the CV cure was
80 min. It should be noted that if the y ash/epoxy com-
posites were CV-cured at 18 min, the % cure obtained
was 60.8, and the mechanical properties of the compos-
ites, especially the moduli values, were expected to be
low.
4. Conclusion
The properties of the y ash/epoxy composites cured
by conventional thermal (CV) and microwave (MW)
Fig. 9. SEM micrographs of the y ash/epoxy composites with 20 phr y ash (2000 magnication): KBM603 contents at (a) 0.5 wt%, (b) 1.0 wt%, and (c)
1.5 wt%.
1
1.5
2
2.5
3
3.5
4
4.5
F
l
e
x
u
r
a
l

m
o
d
u
l
u
s

(
G
P
a
)
0.0 0.5 1.0 1.5
FA20 FA80
KBM603 content
CV
MW
CV
MW
Fig. 10. Eect of KBM603 content on exural modulus for conventional
(CV) and microwave (MW) cured y ash/epoxy composites with 20 and 80
phr y ash.
T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291 2289
curing techniques were studied through the eects of y
ash and silane coupling agent contents. The results sug-
gested that tensile and exural moduli of the y ash/
epoxy composites were observed to increase with increas-
ing y ash content whereas the mechanical (tensile, ex-
ural and impact) strengths, and tensile strain at break
of the composites progressively reduced with y ash con-
tent. It was recommended that 0.5 wt% coupling agent be
added into of the y ash/epoxy composites for optimiza-
tion of the mechanical properties. Beyond this recom-
mended content, the mechanical properties greatly
reduced, except for the exural modulus. Using the
microwave cure introduced the composites with shorter
cure time and higher ultimate strengths (especially impact
strength) and strain at break whereas the composites with
higher tensile and exural moduli were gained from the
conventional thermal cure.
Acknowledgement
The authors would like to thank Dr C. Thongpin and
Miss K. Chaochanchaikul for their constructive comments
and suggestions during the preparation of this article.
References
[1] National Report on Thailand Outstanding Technologist Award
By Foundation of the Promotion of Science and Technology
under the Patronage of H.M. the King, BKK, Thailand,
October, 2002.
[2] Chand N. SEM observations of fractured y-polyester composites. J
Mat Sci Lett 1988;7:368.
[3] Kishore, Kulkarni SM, Sharathchandra S, Sunil D. On the use of an
instrumented set-up to characterize the impact behavior of an epoxy
system containing varying y ash content. Polym Test 2002;21:
76371.
[4] Kulkarni SM, Kishore. Eect of llerber interactions on compres-
sive strength of y ash and short-ber epoxy composites. J Appl
Polym Sci 2003;87:83641.
[5] Garde K, McGill WJ, Woolard CD. Surface modication of y ash
characterization and evaluation as reinforcing ller in polyisoprene.
Plast Rubb Compos 1999;28:110.
[6] Sombatsompop N, Thongsang S, Markpin T, Wimolmala E. Fly Ash
Particles and Precipitated Silica as Fillers in Rubbers. I. Untreated
Fillers in Natural Rubber and StyreneButadiene Rubber Com-
pounds. J Appli Polym Sci 2004;93:211930.
[7] Thongsang S, Sombatsompop N. Eect of NaOH and Si69 Treat-
ments on the Properties of Fly Ash/Natural Rubber Composites.
Polym Compos 2006;27:3040.
[8] Sen S, Nugay N. Tunning of nal performances of unsaturated
polyester composites with inorganic microsphere/platelet hybrid
reinforcers. Eur Polym J 2001;37:204753.
[9] Evora VMF, Shukla A. Fabrication, characterization and dynamic
behaviour of polyester/TiO
2
nanocomposites. Mat Sci Eng
2003;A361:35866.
[10] Gupta NB. Eect of ller addition on the compressive and impact
properties of glass ber reinforced epoxy. Bull Mat Sci 2001;24:
21923.
[11] Kaynak C, Orgun O, Tincer T. Matrix and interface modication of
short carbon ber- reinforced epoxy. Polym Test 2005;24:45562.
[12] Pothan LA, Oommen Z, Thomas S. Dynamic mechanical analysis of
banana ber reinfoced polyester composites. Compos Sci Tech
2003;63:28393.
[13] Tilbrook MT, Moon RJ, Homan M. On the mechanical properties
of alumina-epoxy composites with an interpenetrating network
structure. Mat Sci Eng 2005;A393:1708.
[14] Hau Kuo D, Chih Chang C, Yue T, Wun S. Dielectric properties of
three ceramic/epoxy composites. Mat Chem Phys 2004;85:2016.
[15] Kishore, Kulkarni SM, Sunil D, Sharathchandra S. Eect of surface
treatment on the impact behaviour of y-ash lled polymer compos-
ites. Polym Intl 2002;51:137884.
[16] Sen S, Nuguy N. Uncured and cured state properties of y ash lled
unsaturated polyester composites. J Appli Polym Sci 2000;77:
112836.
[17] Guhanathan S, Saroja Devi M, Murugesan V. Eect of coupling
agents on the mechanical properties of y ash/polyester particulate
composites. J Appli Polym Sci 2001;82:17559.
[18] Guhanathan S, Devi MS. Eect of environmental stress on the
mechanical properties of surface treated y-ash/polyester particulate
composite. Polym Intl 2002;51:28996.
[19] Kishore, Ravikumar NL, Sunil D. The eect of a starch envelope on
y ash particles on the impact properties of lled epoxy composites.
Adv Compos Lett 2003;12:4554.
[20] Ramos AD, da Costa HM, Soares VLP. Nascimento RSV, Hybrid
composites of epoxy resin modied with carboxyl terminated buta-
diene acrilonitrile copolymer and y ash microspheres. Polym Test
2005;24:21926.
[21] Halvorson RF, Erickson RL, Davidson CL. The eect of ller and
silane content on conversion of resin-based composite. Dent Mat
2003;19:32733.
[22] Marand E, Baker KR, Graybeal JD. Comparison of reaction
mechanisms of epoxy resins undergoing thermal and microwave
cure from in situ measurements of microwave dielectric prop-
erties and infrared spectroscopy. Macromolecules 1992;25:
224352.
[23] Thostenson ET, Chou TW. Microwave and conventional curing of
thick-section thermoset composite laminates: Experiment and simu-
lation. Polym Compos 2001;22:197212.
[24] Degamber B, Fernando GF. Microwave processing of thermosets:
non-contact cure monitoring and ber optic temperature sensors.
Plast Rubb Compos 2003;32:32733.
[25] Jacob J, Chia LHL, Boey FYC. Comparative study of methyl
methacrylate cure by microwave radiation versus thermal energy.
Polym Test 1995;14:34354.
[26] Nightingale C, Day RJ. Flexural and interlaminar shear strength
properties of carbon ber/epoxy composites cured thermally and with
microwave radiation. Composites 2002;A33:102130.
[27] Delmotte M, Jullien H, Ollivon M. Variation of the dielectric
properties of epoxy resins during microwave curing. Eur Polym J
1991;27:3716.
[28] Groombridge P, Oloyede A, Siores E. A control system for
microwave processing of materials. J Manuf Sci Eng 2000;122:
25361.
[29] Prasad Yarlagadda KDV, Hsu SH. Experimental studied on com-
parison of microwave curing and thermal curing of epoxy resins used
for alternative mould materials. J Mat Process Technol 2004;155
156:15328.
[30] Boey FYC. Microwave curing of an epoxy-amine system:eect of
curing agent on the glass-transition temperature. Polym Test
1995;14:83745.
[31] Rahmat AR, Heatley F, Day RJ. Comparison of microwave and
thermal cure of unsaturated polyester resin. Plast Rubb Compos
2003;32:25764.
[32] Zhou S, Hawley MC. A study of microwave reaction rate enhance-
ment eect in adhesive bonding of polymers and composites. Compos
Struct 2003;61:3039.
[33] Zhou J, Shi C, Mei B, Yuan R, Fu Z. Research on the technology and
the mechanical properties of the microwave processing of polymer. J
Mat Process Technol 2003;137:1568.
[34] Ku H. Curing vinyl ester particle-reinforced composites using
microwaves. J Compos Mat 2003;37:202742.
2290 T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291
[35] Boey FYC. Humidity and autoclave pressure eect on the interfacial
shear strength of a microwave cured epoxy-glass ber composite.
Polym Test 1995;14:4717.
[36] Yue CY, Looi HC. Inuence of thermal and microwave processing on
the mechanical and interfacial properties of a glass/epoxy composite.
Composites 1995;26:76773.
[37] Bai SL, Djafari V. Properties of microwave cured composites.
Composites 1995;26:64551.
[38] Boey FYC, Yap BH, Chia L. Microwave curing of epoxy-amine
system-eect of curing agent on the rate enhancement. Polym Test
1999;18:93109.
[39] Chia HL, Jacob J, Boey FYC. The microwave radiation eect on the
polymerization of styrene, J Polym Sci A. Polym Phys 1996;34:
208794.
[40] Choi SS, Nah C, Lee SG, Joo CW. Eect of llerller interaction on
rheological behaviour of natural rubber compounds lled with both
carbon black and silica. Polym Intl 2003;52:238.
[41] Boey FYC, Yue CY. Interfacial strength of a microwave-cured epoxy
glass composite. J Mat Sci Lett 1991;10:13334.
[42] Osswald TA, Menges G. Materials science of polymers for engineers.
New York: Hanser Publishers; 1995.
[43] Abel ML, Allington RD, Digby RP, Porritt N, Shaw SJ, Watts JF.
Understanding the relationship between silane application conditions,
bond durability and locus of failure. Intl J Adhesion Adhesives
2006;26:215.
[44] Culler SR, Ishida H, Koenig JL. FT-IR characterization of the
reaction at the silane/ matrix resin interphase of composite materials.
J Colloid Interf Sci 1986;109:110.
T. Chaowasakoo, N. Sombatsompop / Composites Science and Technology 67 (2007) 22822291 2291