International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

Influence of Nickel Oxide Additive on the

Properties of Sol-Gel Prepared Aluminum
Borate Whsiker
D.Thenmuhil
Department of Ceramic Technology,
A.C.College of Technology,
Anna University, Chennai-25, India
thenmuhil@annauniv.edu

K.V.Vignaswaran
Department of Ceramic Technology,
A.C.College of Technology,
Anna University, Chennai-25, India
vikky06.kv@gmail.com

Abstract Whiskers usually have strength equal to that of a

perfect crystal. They have been found very useful as
reinforcement for metal matrix composites. They enhance
mechanical properties, thermal stability, wear resistance, and
also make them as light weighted ones. Aluminum borate
(9Al2O3.2B2O3) is an effective replacement to silicon carbide
whiskers in its use as reinforcement in aluminum metal owing to
its high tensile strength, oxidation resistance, chemical stability
and wear resistance. In this work, aluminum borate whisker
preparation is carried out by sol-gel process using aluminum
nitrate and boric acid. The prepared whiskers are then
characterized for its morphological and phase properties by
SEM and XRD respectively. The study shows that 3% NiO
added sample fired at 1100oC with 2 hours soaking had better
aspect ratio and productivity.
Keywords Aluminum Borate Whisker, Nickel Nitrate Additive,
Sol-Gel Process.

I. INTRODUCTION
Composites are composed of individual constituent materials
with significantly dissimilar physical or chemical properties.
The matrix phase is continuous phase while the distributed
phase is called as reinforcement phase. Different types of
composites are polymer matrix composites, metal matrix
composites, ceramic matrix composites. As far as metal
matrix composites are concerned the reinforcement may be
ceramic particles, whiskers, or fibers.
Metal
matrix
composite
(MMC)
with
discontinuously reinforcement find extensive application in
the automobile and aerospace industries due to their light
weight and superior mechanical properties even at elevated
temperatures, and hence are widely studied [1]. Such
composites are mostly prepared using ceramic whiskers, such
as silicon carbide, silicon nitride and aluminum borate.
Whiskers are elongated single crystals typically having 0.110m diameter and 10-1000m length. They are single
crystals which contains very few dislocations and the same
crystallographic orientation throughout. The strength and
Youngs modulus are very high. Due to their hardness and
strength, these whiskers are highly interesting as reinforcing
materials in ceramics as well as in metals.
Among whiskers, SiC whiskers were found to be
very effective with high hardness and strength [2]. But these
whiskers were costlier, carcinogenic and caused many health

S.ManishaVidyavathy
Department of Ceramic Technology,
A.C.College of Technology,
Anna University, Chennai-25, India
manisha @annauniv.edu

hazards. So identifying a cost-effective reinforcements and

fabrication techniques is important to promote development of
MMCs. Aluminum borate (9Al2O3.2B2O3) whisker is the
cheapest ceramic whiskers and its mechanical properties
matches SiC reinforced Al composites. Therefore aluminum
borate whiskers can be a better replacement for SiC to
reinforce aluminum matrix composites [3].
Aluminum borate (9Al2O3.2B2O3) has a melting
point of 1440C, density of 2.94g/cm3, Mohs hardness of 7,
tensile strength of 8GPa, high Youngs modulus of 400Pa and
low thermal expansion co-efficient. It tends to form a needle
shaped crystals which make them suitable for reinforcement in
metal [4]. These whiskers are of low cost, light weight and
increased strength. The properties of aluminum borate
whiskers are competitive with those of SiC whiskers and are
widely utilized for aluminum-based composite materials.
Aluminum borate whiskers were synthesized by
potassium sulphate flux method using aluminum sulphate and
boric oxide. The whiskers prepared had needle shaped
structure and could be used as an alternate for reinforcement in
metal. The main disadvantage of this method is that the
productivity was low [5].
The aluminum borate whiskers were prepared with
aluminum hydroxide, boric acid and nickel oxide additive by
vapour- liquid- solid method (VLS)[6]. The microstructure was
observed to have 54% to 56%porosity. The estimated aspect
ratio was reported to decrease with increase in sintering
temperature from 1150oC- 1350oC. In another work[4]the
aluminum borate whiskers were coated with NiO. Aluminum,
silicon and copper were used as starting materials. NiO was
coated on the whisker by chemical precipitation method. The
synthesized product had increased degree of reaction and high
tensile strength.
Glass ceramics containing aluminum borate
whiskers were synthesized to increase the fracture toughness
and hardness. The aluminum borosilicate glass was prepared
by using boric oxide, silica, alumina, barium oxide and
magnesia [4]. Aluminum borate hydrate was used as the
precursor. The synthesis was done in two different methods
namely crystallization of an aluminum boro silicate glass and
addition of an aluminum borate precursor powder to a glass
frit.

ISBN 978-93-80609-17-1
956

International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

Aluminum borate whiskers can also be synthesized

by various methods like thermal evaporation, combustion
synthesis, flux systems, solid state reaction, chemical vapor
synthesis, catalyst synthesis and sol- gel method. Among the
above methods, except sol- gel the other methods require high
processingtemperature, high energy consumption and catalyst.
The sol- gel method offers many advantages like
low temperature processing, low cost, easy technology, wide
range of accessible shapes and high purity of the synthesized
product [8].Aluminium borate whisker preparation by sol-gel
using aluminium nitrate nonahydrate and boric acid taken in
1:3, 1:4 and 1:6 ratio and firing at 750oC and 1050oC was
studied in an earlier work [1] and the effect of citric acid
addition was also analysed. It was reported that firing at
1050oC formed Al18B4O33 whisker irrespective of the raw
material proportion taken.
Works are continuously done to decrease the
processing temperature of whisker or to enhance the
characteristics of whisker by incorporating additives. Previous
work on porous ceramic preparation with a framework
structure of aluminum borate whiskers has shown that
addition of nickel oxide in the sol-gel prepared aluminum
borate whisker preparation enhances the aspect ratio of
prepared whisker. Hence the effect of nickel oxide in the solgel prepared aluminum borate whisker is analyzed in the
present work by addition of nickel nitrate during the sol
preparation. Nickel oxide was added to study its influence on
the reaction rate between the precursors and the aspect ratio of
the prepared whiskers.

8 hrs. A total of 27 samples were prepared.

III. RESULTS AND DISCUSSION
A. SEM
The fired samples were characterized by Scanning
Electron Microscope (SEM) and X-Ray diffraction (XRD). All
the 27 samples with 3 firing temperature and each soaked for 3
different times were characterized by SEM. Of the various
firing temperatures and soaking times, the samples listed in
Table I were found to result in better whiskers as observed
from the SEM images.
TABLE I
ALUMINIUM BORATE WHISKER SAMPLES WITH BETTER MICROSTRUCTURE

Sample ID

% of NiO

AB1
AB2
AB3

1
2
3

Firing Temperature
(oC)
1000
1050
1100

Soaking
Time (Hrs)
5
2
2

The SEM images of AB1, AB2 and AB3 are given in

Fig.2, Fig.3 and Fig.4 respectively.

II. EXPERIMENTAL WORK

The sequence followed for the preparation of
aluminum borate whiskers is illustrated in the Fig.1
Fig 2 SEM image of AB1

Raw materials
Weighing
Mixing
Drying

Fig. 3 SEM image of AB2

Firing
Fig. 1 Flowsheet for the Preparation of Whiskers

The raw materials used in this work are Aluminum

nitrate nona hydrate (Al(NO3)3.9H2O), Boric acid (H3BO3),
Citric acid (C6H8O7), and Nickel nitrate (Ni(NO3)3).
Aluminum nitrate and boric acid were taken in the ratio of 1:3
which is twice the amount of citric acid taken. The various
proportions of nickel nitrate (1 wt %, 2wt%, 3wt % of l2O3)
were taken. The raw material mixture was dissolved in 50ml
deionized water and stirred vigorously. The clear,
homogenous sol obtained was dried at 120oC and fired at
various temperatures. The firing temperatures were varied as
1000oC, 1050oC and 1100oC and the soaking hours as 2, 5 and

ISBN 978-93-80609-17-1
957

Fig. 4 SEM image of AB3

International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

It can be observed from the figures that AB3 shows

that the perfect whiskers are formed with optimum aspect
ratio. The optimum aspect ratio is important in reinforcement
of whiskers as complication in reinforcement increases with
length of whiskers.

[6]

B. XRD

[8]

[7]

The XRD result of AB3 is shown in the Fig. 5.

Fig. 5 XRD result of AB3

The X-ray diffraction pattern confirms that the

diffraction peaks were aluminum borate phase and were in
good agreement with the standard diffraction parameters of
aluminum borate. There is no significant impurity peak in the
diffraction pattern showing high purity of aluminum borate
synthesized by sol-gel method.
IV. CONCLUSION
Aluminum borate whisker was prepared by sol-gel
method with nickel oxide additive and characterized by SEM
and XRD. Aluminum borate whisker of optimum aspect ratio
has been formed at the firing temperature of 1100oC and
soaking time of 2 hours.
The reinforcement of aluminum borate whisker gets
complicated since they cause health hazards. Since whiskers
of high aspect ratio with superior properties are difficult to be
reinforced a whisker preform is made and molten metal is
infiltrated [6]. Since this process consumes time and are not
cost effective an alternative method of reinforcing whiskers
uniformly to metal and form composite is under study.
REFERENCES
[1]
[2]
[3]
[4]
[5]

Jun Wang JianSha, Synthesis of Aluminium Borate Nano wires by

Sol-gel method, Material Research Bulletin vol.40, pp. 1551-1557,
2005.
Houyem Abderrazak and Emna Selmane BelHadj Hmaida, Silicon
carbide synthesis and properties, In book: Properties and Applications
of Silicon Carbide,; ISBN: 978-953-307-201-2 , Apr 2011.
J.D.Birchall, D.R.Stanley, M.J. Mockford, G.H.Pigott and P.J.Pinto,
Toxicity of silicon carbide whiskers, Journal of Materials Science
Letters, vol.7, pp. 350-352, 1998.
H.K.Lee, S.Zerbetto, P. Colombo and C.G.Pantano, Glass ceramics
and composites containing aluminum borate whiskers, Ceramics
International , vol. 36, pp. 1589-1596, 2009.
ErkinGonenli and A.GuneytTas, Synthesis of aluminum borate
whiskers for metal matrix composites, Powder Diffraction, vol. 15,
no.2, pp. 104-107, 2000.

ISBN 978-93-80609-17-1
958

L.M.Peng, X.K.Li, H.Li, J.H.Wang and M.Gong, Synthesis and

microstructural characteristics of aluminum borate whisker, Ceramic
International, vol. 32, pp. 365-368, 2006.
W.D.Fei and V.B.Li, Effect of nickel oxide coating of whisker on
tensile strength of aluminum borate whisker- reinforced aluminum
composite, Materials Science and Engineering: A, vol. 39 no.1-2, pp.
27-32, 2004.
R.K.Gupta, A.A.Al- Ghamdi and Omar A.Al-Hartomy, Synthesis and
characterization of nanostructured aluminum borate by sol- gel
method, Journal of Sol-Gel Science and Technology, vol. 64, no. 1, pp.
100-103, 2012.