Synthesis and Characterization of Nanostructured Aluminum Borate by Sol-Gel Method

J Sol-Gel Sci Technol (2012) 64:100–103
DOI 10.1007/s10971-012-2833-4
ORIGINAL PAPER
Synthesis and characterization of nanostructured aluminum

borate by sol–gel method
R. K. Gupta • A. A. Al-Ghamdi • Omar A. Al-Hartomy •
Faten Al-Hazmi • F. El-Tantawy • F. Yakuphanoglu
Received: 23 April 2012 / Accepted: 29 June 2012 / Published online: 10 July 2012
Ó Springer Science+Business Media, LLC 2012
Abstract Nanostructured aluminum borate was synthe- 1 Introduction

sized using sol–gel technique. X-ray diffraction study
revealed that the synthesized aluminum borate was single The nanostructured materials such as nanotubes, nano-
crystal. These nanorods have very uniform diameter. High- wires, nanobelts, fibers and whiskers have been investi-
resolution transmission electron microscope images gated because of their interesting optical, electrical, and
indicate that aluminum borate is well crystallized. The mechanical properties [1, 2]. These materials with high
alternating current (AC) conductivity of the aluminum elastic modulus, tensile strength and low thermal expansion
borate was studied as a function of temperature and fre- properties could be used as reinforcements in composites to
quency. The AC conductivity mechanism of the aluminum increase the strength and wear resistance of metal or
borate was found to be proportional to xs. The exponent polymer matrix [1, 3, 4]. Among various nanostructured
s is almost independent with temperature. This suggests materials, aluminum borate shows high elastic modulus,
that AC conductivity mechanism of the aluminum borate tensile strength, resistance to corrosion, and chemical sta-
can be interpreted by localized hopping model. bility [5, 6].
Nanostructured aluminum borate has been synthesized
Keywords Aluminum borate Sol–gel AC conductivity via several methods such as thermal evaporation [7],
combustion synthesis [8], flux synthesis [9], chemical
vapor deposition [10], catalyst synthesis [6], solid state
R. K. Gupta (&) reaction [11], and sol–gel [12] methods. However, some of
Engineering Research Center, North Carolina A & T State these methods require high processing temperatures, high-
University, Greensboro, NC 27411, USA energy consumption, and need of catalysts. Among these
e-mail: ramguptamsu@gmail.com
techniques, sol–gel offers many advantages such as low
A. A. Al-Ghamdi O. A. Al-Hartomy F. Al-Hazmi temperature processing, low cost, easy technology, and
F. Yakuphanoglu wide range of accessible shapes [13, 14]. The product can
Department of Physics, Faculty of Science, King Abdulaziz be influenced by careful control of several reaction
University, Jeddah 21569, Saudi Arabia
variations.
O. A. Al-Hartomy Peng et al. [5] have synthesized aluminum borate
Department of Physics, Faculty of Science, University of Tabuk, whisker by firing a green powder compact of a mixture of
Tabuk, Saudi Arabia aluminum hydroxide, boric acid and an additive of nickel
oxide. They observed that the addition of nickel oxide
F. El-Tantawy
Department of Physics, Faculty of Science, Suez Canal accelerates the reaction between aluminum oxide and
University, Ismailia, Egypt boron oxide at high temperature and increases the aspect
ratio of the length to diameter of aluminum borate whis-
F. Yakuphanoglu (&)
kers. Single crystal aluminum borate nanowires were syn-
Department of Physics, Faculty of Science, Firat University,
23169 Elazig, Turkey thesized by directly heating a mixture of aluminum and
e-mail: fyhanoglu@firat.edu.tr boron oxide powder at 850 °C [6]. A self-catalytic growth
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J Sol-Gel Sci Technol (2012) 64:100–103 101
mechanism of the aluminum borate nanowires was pro-

posed. Single-crystal and uniform aluminum borate-coated
aluminum oxide nanowires have been synthesized in high
purity and in large yield via a reaction of metal aluminum
with boron oxide in the presence of carbon nanotubes [15].
The literature survey indicates that there is no detail study
on the alternative current (AC) conductivity of nanostruc-
tured aluminum borate.
In this work, we have reported a simple and effective low
temperature processed sol–gel method to synthesize alumi-
num borate nanorods. This method could be adopted for
large scale production of aluminum borate at low cost. The
synthesized nanostructured aluminum borate was charac-
terized using structural and AC conductivity measurements.
2 Experimental details
Fig. 1 XRD patterns of synthesized aluminum borate powder
The aluminum borate was synthesized using sol–gel
method. All the chemicals for the synthesis were purchased lattice parameters were in good agreement with the stan-
from the Alfa Aesar. Aluminum borate was synthesized dard powder diffraction parameters of aluminum borate
using Al(NO3)3 and H3BO3 precursors. For preparation of (JCPDS 032-0003). There was no other impurity peak in
aluminum borate, 1.0 M of Al(NO3)3 and 3.0 M of H3BO3 the diffraction patterns, indicating high purity of the sol–
were dissolved in deionized water and then 1.0 Mofcitric gel synthesized aluminum borate.
acid was added to this solution. The citric acid worked as a The morphology and nanostructure of the synthesized
chelating agent in the reaction. The resulting solution was aluminum borate were further analyzed by transmission
stirred at 150 °C for 5 h. At this temperature, the con- electron microscopy. TEM images of the aluminum borate
densation reaction between –COOH groups of citric acid are shown in Fig. 2. As seen in these figures, aluminum
occurred and led to the formation of water. The evapora- oxide was mainly composed of straight nanowires and
tion of water at this temperature made the sol to turn into a hardly any impurity was found. The nanowires have
gel. The obtained gel was heated 750 °C for 4 h under lengths of several nanometers and diameters ranging from
ambient atmosphere to decompose the chemical residuals 15–20 nm (Fig. 2a). From HR-TEM image (Fig. 2b), it can
such as citric acid and nitrate. The obtained powders were be seen clearly that the nanowires are well crystallized. The
pelleted in the form of disk under 5 ton pressures with the distance between the parallel fringes was about 0.44 nm,
diameter of 11 mm. corresponding to the (111) planes of Al18B4O33. Figure 2c
X-ray diffraction (XRD) patterns of the synthesized shows the selected area electron diffraction pattern (SAED)
material were recorded with BrukerAXS (D8 Discover) taken from a single nanowire. It is evaluated that the pat-
using 2h–h scan with CuKa (k = 1.5405 Å) radiation. The tern could be indexed as an orthorhombic Al18B4O33 phase
microstructure of the prepared material was observed using recorded from [-2 1 0] zoon axis [9].
a high-resolution transmission electron microscope The AC conductivity of the sol–gel synthesized alumi-
(HRTEM, Jeol). The electrical characterization of the num borate was studied to understand the conduction
material was performed using a semiconductor character- mechanism. The total measured conductivity r(x), is
ization system (Keithley 4200SCS). related to the DC conductivity rdc and the component
rac(x) according to the relation [16]
3 Results and discussion rac ðxÞ ¼ rtot ðxÞ rdc ð1Þ

The frequency dependence of the AC conductivity can
Figure 1 shows X-ray diffraction patterns of the synthe- be expressed by the power law
sized powder. As seen in XRD pattern, the sample showed
rac ðxÞ ¼ Axs ð2Þ
a polycrystalline nature. All the observed diffraction peaks
were indexed to the orthorhombic phase of Al18B4O33 with where A is a constant depending on temperature, x is the
the lattice parameters of a = 0.767 nm, b = 1.511 nm, angular frequency and s is an exponent less than or equal to
and c = 0.566 nm. The observed diffraction patterns and unity and represent the degree of interaction between
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102 J Sol-Gel Sci Technol (2012) 64:100–103
Fig. 2 Typical low magnification TEM image of the nanorods (a), HR-TEM image (b), and corresponding SAED pattern from part of a nanorod
of aluminum borate (c)
mobile ions and its surrounding lattices. The pre-factor A tunneling (OLPT) model [19], the exponent s should both
determines the strength of polarization [17]. Figure 3a shows temperature and frequency dependent. s decreases with
the relation between lograc(x) and logx for the aluminum increasing temperature from unity at room temperature to a
borate. It is observed that lograc(x) increases linearly with minimum value at a certain temperature then it increases
increasing logfrequency according to Eq. 2. The values of with increasing temperature. Therefore, OLPT model is also
exponent s were calculated from the slopes of the linear part not applicable for aluminum borate. For the correlated bar-
of Fig. 3a. It is clear from the Fig. 3b that the value of s is not rier hopping (CBH) model, values of the frequency exponent
almost changed as the temperature is increased. Based on the s is ranged from 0.7 to 1 at room temperature and is found to
values and temperature independent nature of s, we tried to decrease with increasing temperature. It is seen that s value
model the conduction mechanism of the aluminum borate. is almost independent temperature. Thus, the frequency
For the quantum mechanical tunneling (QMT) model [18], dependence of rac(x) can be not explained satisfactorily in
the exponent s should be almost equal to 0.8 and increase terms of the correlated barrier hopping model. Furthermore,
slightly with increasing temperature or independent of in the correlated barrier hopping (CBH) model, the power
temperature. Therefore, the QMT model is not applicable for law for the frequency dependence of rac is only an approx-
this system. According to the overlapping-large polaron imation, dependent on several parameters, one of them being
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J Sol-Gel Sci Technol (2012) 64:100–103 103
Fig. 3 Frequency dependence

of rac(x) for aluminum borate
at different temperature (a) and
temperature dependence of the
parameter s for aluminum
borate (b)
the activation energy of rdc. In order to determine activation References

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J Sol-Gel Sci Technol (2012) 64:100–103

Synthesis and characterization of nanostructured aluminum

Faten Al-Hazmi • F. El-Tantawy • F. Yakuphanoglu

Abstract Nanostructured aluminum borate was synthe- 1 Introduction

mechanism of the aluminum borate nanowires was pro-

3 Results and discussion rac ðxÞ ¼ rtot ðxÞ rdc ð1Þ

Fig. 3 Frequency dependence

the activation energy of rdc. In order to determine activation References

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