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A study on mechanical, thermal, and electrical properties of glass fiber-reinforced epoxy hybrid
composites filled with plasma-synthesized AlN
Pravuram Panda, Gopa Mishra, Sisir Mantry, Saroj Kumar Singh and Swami Prasad Sinha
Journal of Composite Materials published online 15 October 2013
DOI: 10.1177/0021998313506242
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JOURNAL OF
COMPOSITE
Article M AT E R I A L S
Journal of Composite Materials
0(0) 1–10
! The Author(s) 2013
A study on mechanical, thermal, Reprints and permissions:
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and electrical properties of glass DOI: 10.1177/0021998313506242
jcm.sagepub.com
fiber-reinforced epoxy hybrid composites
filled with plasma-synthesized AlN
Abstract
Glass fiber-reinforced epoxy resin (GFRE) composites filled with aluminum nitride (AlN) powder were fabricated, and
their thermal and electrical properties were investigated. It is observed that with the increasing percentage of AlN
particles, there is a significant enhancement in thermal conductivity and micro-hardness, but there is a decline in tensile
strength. Experimental results demonstrate that the GFRE composites with 10 wt% of AlN loading show maximum
dielectric breakdown strength of 30.26 kV/mm with minimum volume resistivity of 7.5 1014
cm and thermal con-
ductivity value of 0.300 W/mK. Scanning electron microscopy studies were conducted to observe the voids and distri-
bution of filler in composites.
Keywords
Epoxy resin, plasma-synthesized AlN, glass fiber, hand-lay-up technique, GFRE composites
high dielectric breakdown strength, high electrical Table 1. Plasma operating parameters adopted in
resistivity (>1016 Vm), low dielectric constant (8.8 at extended arc thermal plasma reactor.
1 MHz), and low CTE which is close to that of silicon
Plasma operating parameters
and good corrosion resistance.14,15 Hence, the use of
AlN powder in glass fiber-reinforced epoxy resin DC load voltage (V) 50
(GFRE) composite enhances its thermal, electrical, Arc current (Ampere) 300
and mechanical properties to a large extent. NH3 gas flow rate (l/min) 2
Considerable work has been reported by many Ar gas flow rate (l/min) 1
researchers based on the study of thermal, mechanical, Reaction time (min) 25
and electrical properties of epoxy composites filled with Electrode spacing (cm) 5
nano- or micron-sized AlN filler.9,16–21 Rarely work
was explored on the same study about the glass fiber-
reinforced epoxy/AlN hybrid composite. The cost of
nano AlN powder in the international market is also atmosphere of ammonia (2 l/min) and argon (1 l/min)
too high, hence designing PMC using micron-sized cer- in an extended arc DC thermal plasma reactor (50 kW)
amic powder with good physical, mechanical, and elec- for a pre-optimized time of 25 min. The adopted plasma
trical properties is a challenge. operating condition was given in Table 1. The length of
In view of above, in our laboratory, we synthesized the arc was adjusted by moving the top electrode
fine AlN powders using thermal plasma technology via (anode) up and down by a rack and pinion arrange-
carbothermal reduction–nitridation process in an indi- ment. Ar gas helps in the formation and stabilization of
genously developed extended arc thermal plasma reac- plasma arc, and it also maintained in a protective
tor. Using the plasma-synthesized AlN powder, GFRE atmosphere inside the hearth. The gas flow was contin-
composite slabs were fabricated by conventional hand- ued even after the plasma treatment of the granules till
lay-up technique followed by light compression mould- the hearth was sufficiently cooled to prevent oxidation
ing technique. The main objective of the present study of the product. The solid–solid reaction between
is to develop the mechanical, thermal, and electrical a-Al2O3 and activated charcoal in NH3 plasma via car-
properties of GFRE resin composite using plasma- bothermal reduction process resulted fine AlN powder
derived fine AlN powder as filler material. with little unreacted carbon. After the synthesis of AlN
powder, unreacted free carbon was removed by heating
the plasma yield product in a muffle furnace at 700 C
Experimental procedures for 2 h in air. The detail of the powder synthesis method
and reaction mechanism involved was described in
Materials detail elsewhere.22
Low temperature curing epoxy resin (DGEBA, grade-
LY 556, density 1.15 gm/cc at 25 C), an aliphatic
Composite slab fabrication
amine-based hardener (HY951, Triethelene Tetra
Amine, density 0.98 gm/cc at 25 C, supplied by Ciba A weighed amount of epoxy resin and plasma-
Geigy Ltd., India), and bi-directional woven roving synthesized AlN powders were taken in a beaker and
E-glass fibers (having modulus 72.5 GPa, density mixed thoroughly with the help of a high speed stirrer
2.59 gm/cc at 25 C, Saint Gobain Ltd., India) were before the respective fiber mats were reinforced into the
used for the preparation of GFRP matrix composite matrix body. The mixture was kept in a vacuum oven at
system. Alumina (a-Al2O3, purity—99.5%, Median 30 C for 30 min to avoid air trapped into the mixture.
diameter—4 mm, Grade-NSPL 20, NALCO, India) Then a hardener was added to the mixture at 1:10
and activated charcoal (Carbon content—81.3%, weight ratio of the resin, as recommended.23
MERCK, India) were used for the preparation of Composite slabs with particulate fillers (AlN) of three
AlN powder in our laboratory. different amounts (5, 10, and 15 wt%, respectively) with
fixed glass-fiber loading (50 wt%) were fabricated by
conventional hand-lay-up technique followed by light
Preparation of AlN from alumina compression moulding technique. A stainless steel
Alumina (a-Al2O3) and activated charcoal powders mould having dimension of 210 210 40 mm3 was
were mixed in the weight ratio of 5:3 with dextrin as used. The cast of each composite was cured under a
a binder and small granules (1–3 mm diameter) were load of 50 kg for 24 h before it was removed from the
prepared. The moisture present in granules was then mould. In order to achieve further better performance,
removed by heating at 100 C for 5 h on a hot plate. the composites were then post cured at 80 C for 2 h and
The dried granules were plasma-treated in the 100 C for 4 h in an oven and allowed to cool gradually
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Panda et al. 3
Figure 2. FESEM image and its corresponding EDAX spectrum of plasma synthesized hexagonal AlN powder.
Table 2. Density and void volume fraction of the PMCs filled with glass fiber and different wt% of
plasma-synthesized AlN powder.
Panda et al. 5
Density of composites
The density of a composite depends on the relative
proportion of matrix and reinforcing materials,
and this is one of the most important factors determin-
ing the properties of the composites. The theoretical
densities of samples were calculated based on the dens-
ity of AlN, epoxy, and glass fiber as 3.255, 1.15, and
2.590 g/cm3, respectively, according to the following
equation: Figure 3. Variation of density and void fraction in composites
with different wt% of plasma synthesized AlN powder.
1
ct ¼ w w wp ð3Þ
f m
þ þ
f m p
ct ce
Vv ¼ ct
ð4Þ
Panda et al. 7
Figure 6. TGA curves of neat epoxy and GFRE composites Figure 8. Variation of volume resistivity of PMC filled with glass
filled with different wt% of plasma synthesized AlN powder. fiber and plasma synthesized AlN powder with different wt%.
Figure 9. Microstructure of tensile fractured GFRE composites with (a) 0, (b) 5, (c) 10 and (d) 15 wt% of plasma synthesized AlN
powder.
polymer and glass fiber layers is high, which probably 15 wt% plasma-synthesized AlN powder, respectively.
allows the existence of free ions and also their unhin- It is evident from Figure 9(a) that the layers of polymer
dered transport through the bulk of the material result- and bidirectional glass fiber staked one over another
ing in an increase in the electrical conductivity through with good bonding. Lateral view of the tensile fractured
the volume of the material. However, with the increase glass fiber can be observed in Figure 9(a) and (b). It is
in AlN loading up to 10 wt%, immobilized polymer evident that glass fibers are well embedded in epoxy
chains act as ion traps, which inhibit the ion mobility which improves the mechanical properties of the com-
and the flow of electrons, thereby resulting in a decrease posites. There is no observation of AlN particles in the
in the overall conductivity values, i.e. an increase in micrograph of GFRE composite filled with 5 wt% of
volume resistivity.18 Furthermore, incorporation of AlN because of low filler concentration and well dis-
AlN (i.e. at 15 wt%) leads to the reduction in volume persion of the filler particles in epoxy. As the concen-
resistivity as filler makes partial interconnections tration of AlN increases up to 10 wt%, the formation of
between the particles lead to the margin decrease of voids started (Shown in Figure 9 (c)), which affects the
volume resistivity of GFRE composite system. Similar mechanical, electrical, and thermal properties of the
type of observation was observed in a previously composites. In 15 wt% of the AlN loading, agglomer-
reported paper related to the influence volume resistiv- ation/clusters of AlN particles were formed inside the
ity of epoxy/nano alumina composites on the filler composite which is shown in Figure 9(d). There is no
percentage.30 observation of particle-matrix debonding and micro-
cracks on the surface of the composites, which suggest
a relatively strong interfacial bonding and good com-
patibility of AlN particles with the epoxy matrix. This
Fracture surface morphology
further corroborates the enhancement of thermal con-
Figure 9(a) to (d) shows the morphology of the tensile ductivity, mechanical, and electrical property of GFRE
fractured GFRE matrix composite with 0, 5, 10, and matrix with AlN filler.
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