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Effect of nano TiO2 particle size on mechanical properties of cured epoxy resin
Hamad A. Al-Turaif
Chemical and Materials Eng. Dept., King Abdulaziz University, P.O. Box 80204, 21589 Jeddah, Saudi Arabia
a r t i c l e
i n f o
Article history:
Received 14 May 2010
Accepted 20 May 2010
Keywords:
Epoxy resin
TiO2 nano particles
Tensile stress
Flexural stress
a b s t r a c t
Mechanical properties of toughened epoxy resin with two nano particles sizes of TiO2 (17 nm and 50 nm)
at different weight fractions (1%, 3%, 5% and 10%) were investigated and compared to that of submicron
particles at 220 nm. The composites were characterized by tensile, exural, pull-off and abrasion tests,
followed by X-ray photoelectron spectroscopy and scanning electron microscopy of the fracture surfaces.
The investigated epoxy depicted high performance epoxy systems formulated with low molecular weight
epoxy resin and diethyltoluenediamine as a curing agent.
Results indicate an enhancement in the epoxy composite mechanical properties due to the addition of
small fraction of TiO2 particles. Highest tensile stress values were found at 3 wt.% for 17 nm and 50 nm
particles and at 5 wt.% for 220 nm particles. The maximum exural properties were found at lower TiO2
fraction of 1 wt.% only. The exural behavior of the epoxy composite was not improved by further addition
of the ller. The enhancement of modied epoxy with the smaller nano particles size showed a better
resistance to weight loss. It is suggested that the amount of particles present and its size affect the matrix
deformation and as a result, the quality of interface in the composite. A relation between tensile and
exural stress as function of the toughened particle size was found.
2010 Elsevier B.V. All rights reserved.
1. Introduction
Since 1947 the epoxy resin has been extensively used in a variety
of wide industrial applications, such as surface coatings, adhesives,
painting materials as well as electronic devices. Like other thermosetting materials, epoxy resins are also extremely brittle, which
limits their application in products that require high impact and
fracture strength.
Various researchers attempt to overcome this problem by
introducing an intermediary phase through blending or chemical
reactions. Generally, the dispersed phase can be classied into four
types: reactive liquid rubbers, functionally terminated engineering thermoplastics, reactive ductile diluents, and inorganic/hybrid
particles. Their main objective is to enforce the crack resistance and
toughness without signicantly decreasing other inherent properties, such as thermo mechanical properties [1].
In recent years, nano particles are being used as advanced ller
to improve the mechanical properties of the epoxy resin. Different
types of nano particles like TiO2 [24], Al2 O3 [3], Silica [5], carbon
black [6], clay [6,7] and SiO2 [8] are used to improve the toughness
of the epoxy resins.
Several mechanisms leading to improve mechanical performance in nano lled epoxy have been introduced. The mechanisms
242
with Al2 O3 SiO2 . The other two grades, UV-TITAN L830 and UVTITAN L181, are ultra-ne with 50 nm and 17 nm crystal diameter,
respectively.
The matrix was selected as it is commercially known formulation which is used as a binder in oor coating industry [10]. The
epoxy resin chosen was DER 331TM . It is an undiluted DGEBA-based
liquid epoxy resin manufactured by DOW Chemical Company.
Low molecular weight grades of epoxy resin, such as these, have
become standard due to their versatility in various applications.
Typical properties for the resin include: epoxy equivalent weight
of 182192 g/mol, a viscosity of 110140 poise at 25 C and density
of 1160 kg/m3 at 25 C [11].
Isophorone diamine (IPDA) is also used as a curing agent in
conjunction with salicylic acid, to act as a catalyst. The IPDA is manufactured by Huntsman under the name of Aradur 42 with an amine
value of 645665 mg KOH/g, a viscosity of 6.2 cP at 25 C and a density of 920 kg/m3 at 25 C. ANTIFOAM C100 of Basildon Chemical
Company Limited was used in the mix as an air release agent with
the supplier recommended dose.
3PL
2bd2
where P is the load to break, b and d are the width and the thickness
of the specimen, respectively, L is the length between supports. Five
samples were used for each test.
2.5. Abrasion test
Abrasion test for all the samples investigated was performed
using the Taber Rotary Abraser 5135 according to (ASTM D 406007) [14]. The measurement of abrasion resistance was done by
weighing of the material sample before and after subjecting it to
a known abrasive stress throughout a known time period. The load
was 500 g on each side, the number of cycles was 75 rounds using
H-22 wear. The samples shape was square 20 cm 20 cm.
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improved, more than what could have been achieved by using submicron particles (220 nm) (Fig. 1). However, this is true for low TiO2
contents up to 3%. At 3% TiO2 content the improvement achieved in
UTS reached about 14%. Further increase in the TiO2 content above
3 wt.% leads to a gradual reduction in the values of UTS. On the
other hand, at submicron particles (220 nm), a maximum of 13%
increase in UTS is achieved but with higher TiO2 content of around
5%. Further, if we increase the TiO2 content above 5 wt.%, a gradual
reduction in the values of UTS is observed (Fig. 1).
The effects of the TiO2 fraction content on elongation at break,
toughness and the Youngs modulus of the epoxy resin composite
for the different particles sizes investigated are shown in Figs. 24,
respectively. A similar behavior as shown for UTS can be observed
here; at 17 nm and 50 nm the optimal values are at 3% while for
220 nm the optimal values are at 5%. This result corroborates with
the optimal fraction content of 4% found earlier for toughened
epoxy resin with 190 nm TiO2 particles size [16]. It seems that there
is a relation between the particle size and the fraction content producing the optimal values of the tensile properties, as one decreases
the particle size the optimum fraction content decreases. From an
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Fig. 5. Flexural stress of different TiO2 particles size at different weight fractions.
Fig. 6. Relation between the tensile and exural stresses as function of particle size.
Fig. 7. Weight loss % of different TiO2 particles size at different weight fractions.
a+b
c ln(tensile stress)
+
ln(particle size)
(tensile stress)2
Fig. 8. Pull-off strength of different TiO2 particles size at different weight fractions.
245
Fig. 9. SEM micrographs of the tensile fracture surfaces of epoxy resin modied with
17 nm TiO2 particles at different weight fraction: (a) 0 wt.%, (b) 3 wt.%, (c) 5 wt.%, and
(d) 10 wt.%.
246
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