Ultrasonics Sonochemistry 23 (2015) 185–191

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Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultson

Synthesis of titanium dioxide by ultrasound assisted sol–gel technique:

Effect of calcination and sonication time
D.V. Pinjari a,⇑, Krishnamurthy Prasad b, P.R. Gogate a, S.T. Mhaske b, A.B. Pandit a,⇑
a
Chemical Engineering Department, Institute of Chemical Technology, Matunga, Mumbai 400 019, India
b
Department of Polymer and Surface Engineering, Institute of Chemical Technology, Matunga, Mumbai 400 019, India

a r t i c l e i n f o a b s t r a c t

Article history: Nanostructured titanium dioxide has been synthesized using both conventional and ultrasound assisted
Received 8 July 2014 sol–gel technique with an objective of understanding the role of cavitational effects in the synthesis
Received in revised form 14 October 2014 process. The experiments were conducted at a constant calcination temperature of 750 °C and the calci-
Accepted 15 October 2014
nation time was varied from 30 min to 3 h to study the effect of calcination time on the properties of the
Available online 23 October 2014
synthesized TiO2. The TiO2 specimens were characterized using X-ray diffraction (XRD) and scanning
electron microscopy (SEM). The influence of the sonication time on the phase transformation process
Keywords:
from anatase to rutile and also on the crystallite size and percentage crystallinity of the synthesized
Sol–gel synthesis
Ultrasound
TiO2 has also been investigated. It was observed that 100% phase transformation occurred after 3 h of
Titanium dioxide calcination for the ultrasound assisted sol–gel synthesized TiO2. The study on the phase transformation
Calcination time via variation of sonication time yielded interesting results. It was observed that as the sonication time
Sonication time increased, an initial increase in the rutile content is obtained and beyond optimum sonication time,
Nanosynthesis the rutile content decreased. In general, the ultrasound assisted process results in synthesis of TiO2
material with higher rutile content as compared to the conventional sol–gel process.
Ó 2014 Elsevier B.V. All rights reserved.

1. Introduction
The physical methods of nanoparticle synthesis have a few
inherent disadvantages such as the inability to obtain nanoparti-
cles with controlled size distribution and also the sizes are often
around 100 nm or above which may not meet the requirements
of the specific applications where the properties are dictated by
the size distribution and mean size [1,2]. Precipitating clusters of
inorganic compounds from a solution of chemical compounds
has been an attractive way for synthesis of nanoparticles due to
the simplicity of the experimental methods, which is especially
valid if the goal is to just obtain a nanocrystalline powder, instead
of a ‘‘dispersible’’ nanoparticulate powder [1]. Among the different
approaches for solution based processing, sol–gel process com-
monly applied for making inorganic networks of nanomaterials
through the formation of a colloidal suspension (sol) and gelation
of the sol to form a network in a continuous liquid phase (gel)
[3]. The sol–gel process is widely used for manufacturing nanopar-
ticles of various metal oxide materials like TiO2 [4–6], ZnO [7,8],
SiO2 [9,10], WO3 [11], etc. The sol–gel route is very attractive
⇑ Corresponding author. Tel.: +91 22 33612012; fax: +91 22 33611020.
E-mail addresses: dv.pinjari@ictmumbai.edu.in (D.V. Pinjari),
ictmumbai.edu.in (A.B. Pandit).
because of the ease of operation and ability to tailor the morphol-
ogy of particles by controlling the relative rate of hydrolysis and
condensation reactions (both alcohol condensation and water con-
densation) [1,12]. The sol–gel technique requires annealing treat-
ment of the amorphous precipitates to induce crystallization. The
annealing process consists of two stages viz. dehydration and cal-
cination. Dehydration is typically carried out in an air-circulating
oven at a suitable temperature while the calcination is done in a
muffle furnace. The calcination procedure is used for conversion
of the hydroxide complex into the final metal oxide. The calcina-
tion temperature and the time of exposure to the high temperature
have a significant effect on the crystalline properties of the synthe-
sized nanomaterials. The calcination step perhaps has the most
influence on the properties of the synthesized material.
Selection of proper calcination temperature is of extreme
importance in the sol–gel process. Metal oxide materials occur in
various crystalline polymorphs and generally these polymorphs
are inter-convertible polymorphs. A typical example is titanium
dioxide (TiO2) which is more crystalline rutile phase when synthe-
sized at temperatures of more than 600 °C. Titanium dioxide
occurs mainly in two crystalline polymorphs viz. anatase and rutile
and the properties are typically decided based on the type of poly-
ab.pandit@ morph [13]. Thus, for obtaining phase purity and selectivity in syn-
thesis, selection of optimum calcination temperature is essential.

http://dx.doi.org/10.1016/j.ultsonch.2014.10.017
1350-4177/Ó 2014 Elsevier B.V. All rights reserved.
186 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191
The effect of calcination temperature on the properties of TiO2 syn-
thesized by ultrasound assisted (US) and conventional sol–gel
(NUS) synthesis has been established in our previous work [14].
It has been observed that as the calcination temperature increases,
the rutile content also increases and the observed trend was simi-
lar for both the approaches. However, use of ultrasound lowered
the required temperature (750 °C) for complete phase transforma-
tion as compared to the conventional approach (850 °C).
The second important parameter controlling the phase transfor-
mation is the calcination time. The effect of calcination time on a
particular material seems to be of particular importance as the time
period to which a material is subjected to high temperatures will
play a major role in deciding the crystalline microstructure that will
be developed in the material. A rapid calcination procedure will not
afford enough time for the lattice structure to get developed
completely thus creating a material with an inferior crystalline
structure. On the other hand, a sufficiently slow calcination process
will allow the lattices to get oriented properly thus creating a more
ordered microstructure and hence a more crystalline material.
Effect of calcination time on the formation of the product structure,
shape and size was studied by Reli et al. [15] and it was reported
that calcination time is very influential parameter affecting the
gelation as well as final product formation. Similarly, in the case
of ultrasound assisted approach, the sonication time is also an
important parameter that will affect the crystallite size and crystal-
linity of the synthesized nanoparticles [16]. In the present work, the
effect of calcination and sonication time on the properties of syn-
thesized TiO2 using the sol–gel process (ultrasound assisted and
conventional approach) has been studied in details.
2. Materials and methods
2.1. Materials
Titanium tetraisopropoxide (TTIP) precursor was obtained from
Spectrochem Pvt. Ltd., India. 2-propanol (99.9% pure) was procured
from S. D. Fine Chemicals Ltd. Mumbai, India. Glacial acetic acid
solution was obtained from Merck Ltd. Mumbai, India. All the
chemicals were used as received from the supplier without any
pretreatment.
2.2. Preparation of TiO2 by conventional (non-ultrasound assisted
(NUS) sol–gel method
5 mL of titanium tetraisopropoxide (TTIP) precursor was added
drop wise to 30 mL of 2-propanol. The resulting clear solution was
then added drop wise under stirring (Model RQ1210, Remi Metals
Limited, India) to 5 mL of glacial acetic acid solution. The obtained
sol was left at ambient temperature for 24 h. For getting nearly
100% conversion (i.e. for ensuring complete hydrolysis of TTIP pre-
cursor), the solution needed to be kept as such for around 24 h. The
obtained sol after 24 h was then converted into a gel by adding it to
30 mL of distilled water under stirring. The obtained gel was then
dehydrated in an air circulating oven at 110 °C for 3 h. The dehy-
drated material was then calcined in a muffle furnace (Expo Hi
Tech. Mumbai, India, Power input = 2 kW and Length 
Breadth  Height = 30 cm  10 cm  10 cm) at 750 °C for varying
time periods from 30 min to 3 h. The white powder obtained after
calcination was cooled, ground and weighed to estimate the yield
of the final product.
2.3. Preparation of TiO2 by ultrasound assisted (US) sol–gel method
The mixture of TTIP precursor, 2-propanol and glacial acetic
acid solution was subjected to sonication using an ultrasonic horn
(ACE Horn operating at 22 kHz, Rated output power: 750 W (at 40%
amplitude 300 W), Calorimetric efficiency: 10% giving net power
delivery of 60 W, Diameter of stainless steel tip of horn:
1.3  102 m, Surface area of ultrasound irradiating face:
1.32  104 m2, Intensity: 3.4  105 W/m2) operating at 40%
amplitude actually delivering 29.2 W of power for 10 min with a
5 s on and 5 s off cycle. The magnitude of power dissipation has
been selected on the basis of detailed optimization study per-
formed in the earlier work [14]. The sol thus obtained, after keep-
ing it for 24 h, was again ultrasonically irradiated by keeping same
parameters (output power and duty cycle). The remaining proce-
dure including the volume of the reactants was similar to that
described for the conventional approach. The use of dual sonication
helps in achieving good mixing characteristics throughout the syn-
thesis process [14]. In the case of pre-hydrolysis, sonication step
results in an efficient micromixing of the various reactants in the
reaction system and post-hydrolysis sonication helps in getting
smaller particles due to the possible mechanical effects of cavita-
tion which aids in avoiding agglomerations. After calcination, the
obtained TiO2 powder (white in color) was cooled, ground, checked
for yield and characterized using the same techniques as that used
for the NUS sol–gel synthesized specimens.
The calcination times used in the present work were 0.5, 1, 2
and 3 h. Accordingly, the conventional (NUS i.e. in the absence of
ultrasound) sol–gel synthesized TiO2 specimens were labeled as
TC0.5NUS, TC1NUS, TC2NUS, and TC3NUS while the ultrasound
assisted sol–gel synthesized TiO2 specimens were labeled as
TC0.5US10, TC1US10, TC2US10 and TC3US10. The heating rate for
both the NUS and US sol gel approaches were kept the same and
the sonication time for these experiments was kept constant at
10 min.
After calcination time was optimized for both the NUS and US
specimens at 3 h, the effect of sonication time was investigated
by varying the sonication time at time t = 0 h and t = 24 h. The
two additional sets of experiments were performed using sonica-
tion time of 5 min and 15 min. For clarity, these two specimens
are described as TC3US5 and TC3US15 respectively in the subse-
quent discussions.
3. Characterization
TiO2 specimens were first characterized by studying their X-ray
diffraction patterns on a Rigaku Mini-Flex X-ray diffractometer.
Crystallite sizes were determined using the Debye–Scherrer equa-
tion. Scanning electron microscopy of the specimens was carried
out on a JEOL JSM 680LA 15 kV SEM to estimate the surface char-
acteristics of the specimen. The XRD and SEM analysis provides
exact knowledge regarding the crystallite size and crystalline char-
acteristics of the synthesized TiO2.
The procedure for the estimation of percentage rutile content
(%) has been based on the details given in the earlier work
[17,18]. The anatase form of TiO2 shows a peak at 2h = 25° while
the presence of rutile form is indicated by a peak at 2h = 28o and
this has been used in the calculations of the rutile content. The
equation used for the calculation is as follows:
% R ¼ 100=½ðA=RÞ  0:884 þ 1 ð1Þ
where % R = Rutile content in percent, A = peak intensity of the peak
at 2h = 25°, R = peak intensity of the peak at 2h = 28°.
The crystallite sizes of the specimens have been calculated by
using the Debye–Scherrer equation, as given below:
Dhkl ¼ Kk=ðBhkl  cos hhkl Þ ð2Þ
where B is the width of the peak at half maximum intensity of a
specific phase (hkl) in radians; K is a constant that varies with the
 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191
method of taking the breadth (generally speaking 0.89 < K < 1 and
in the present work, the constant has been considered as K = 0.9);
k is the wavelength of incident X-rays, which is1.54 Å for Cu Ka; h
is the center angle of the peak and finally, D is the crystallite length
or primary crystallite size.
4. Results and discussion
The first objective of the study was to optimize the calcination
time required for attaining 100% phase transformation from ana-
tase to rutile in the synthesized titanium dioxide. Table 1 shows
the average yields obtained for the synthesis in the presence and
absence of ultrasound. It can be observed that the synthesis in
the presence of ultrasound resulted in much higher yield as com-
pared to the NUS process and this is attributed to the ability of
acoustic cavitation to improve the reaction kinetics by improved
mass transfer (on account of the micro-mixing caused by the
acoustic shock wave and energy release on collapse of the cavita-
tion bubble) and increase in the reaction rates due to the cavitating
conditions created by bubble collapse [19,20].
4.1. X-ray diffractometer (XRD) study for calcination time
optimization
The XRD patterns of the TiO2 specimens prepared by non ultra-
sound (NUS) sol–gel method and Ultrasound (US) sol–gel method
are shown in Figs. 1 and 2, respectively.
4.1.1. Phase transformation in TiO2 synthesized by conventional (NUS)
sol gel method
The X-ray diffraction patterns of the specimens synthesized by
the conventional sol–gel technique (NUS) have been shown in
Fig. 1. From the XRD patterns, it is clear that with an increase in
the calcination time there is an increase in the rutile content. The
conclusion is based on a continuous increase in the intensity of
the peak at 2h = 28°. The specimen calcined for 30 min i.e. 0.5 h
Table 1
Average yields obtained for the NUS and US sol–gel processes.
Synthesis method Yield (%)
NUS or conventional sol gel technique 83.22 ± 3.5
Ultrasound assisted or US sol–gel technique 95 ± 2.3
Fig. 1. X-ray diffraction patterns of conventional sol–gel synthesized nano-TiO2 at various calcination times.
187
(TC0.5NUS) shows the least rutile content while the specimen cal-
cined for 3 h (TC3NUS) shows the maximum rutile content
amongst the NUS synthesized specimens (Fig. 3). The observed
results can be attributed to the fact that when sufficiently large
time is provided for the calcination process, the heat supplied per-
meates into the recesses of the specimen and sufficient exposure to
the high temperature (750 °C) results in the phase transformation
in the TiO2 specimens from the meta-stable anatase phase to the
more stable rutile phase.
The percentage crystallinity of the specimens has been calcu-
lated on the basis of detailed procedure explained elsewhere
[14]. It was observed that with an increase in rutile content, there
is an increase in the crystallinity (Fig. 4). The rutile polymorph of
TiO2 shows better packing density, specific gravity and lower unit
cell volume which results in higher crystallinity than the anatase
which has lower packing density, specific gravity and higher unit
cell volume. The obtained data for the crystallite size and predom-
inant crystalline phase have been reported in Table 2. Similar to
the observed trends in crystallinity, there is an increase in the aver-
age crystallite size as the calcination time is increased thereby
serving as an indicator for the increased rutile content. Overall,
TC0.5NUS which has been calcined for the minimum time shows
a lower crystallite size (24 nm) as compared to the TC3NUS which
has been calcined for a maximum time (size of 35 nm).
4.1.2. Phase transformation in TiO2 synthesized by ultrasound assisted
(US) sol gel method
The X-ray diffraction patterns of the specimens synthesized by
the ultrasound assisted sol–gel technique have been shown in
Fig. 2. The major facet of the effect of calcination time on the rutile
content of the US synthesized specimens was the 100% conversion
from anatase to rutile as observed in the specimen TC3US10. Acous-
tic cavitation causes an increase in the effective surface area,
thereby increasing the rate of heat transfer to the bulk of the spec-
imen. Thus, the rate is faster than that obtained for the NUS synthe-
sized specimens and hence 100% phase transformation occurs at a
much lower temperature (750 °C) for the US synthesized specimens
as compared to the NUS synthesized specimens. Also, similar effect
is observed with respect to the required time for calcination.
As calcination time is increased from 0.5 h to 3 h, increase in the
rutile content in the case of US specimens is much more pro-
nounced than that observed amongst the NUS specimens (Fig. 3).
The observed results can be explained on the basis of cavitational
effects. The pre-hydrolysis sonication ensures an efficient
188 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191
Fig. 2. X-ray diffraction patterns of ultrasound assisted sol–gel synthesized nano-TiO2 at various calcination times.
micromixing of the various reactants in the reaction system. Thus,
the reactants are contacted properly in the conditions of significant
turbulence and liquid circulation exerted on the system during the
10 min of pre-hydrolysis sonication. The post-hydrolysis
sonication results in the formation of nanoparticles (as nuclei) with
smaller average particle sizes. This also ensures that during calci-
nation the heat was transferred more efficiently into the bulk of
the material thereby subjecting all of the particles in the bulk to
the maximum possible temperature in the lowest possible time.
The combined effect of the sonication at two stages helps in the
acceleration of phase transformation from anatase to rutile.
4.2. Scanning electron microscopy study
The SEM micrographs of the specimens are shown in Fig. 5. The
TiO2 synthesized using the US method and calcinated at 750 °C has
a block-type structure as shown in the micrograph of specimen
TC3US10 (Fig. 5C). No such block-type structure is observed in
the corresponding NUS specimen TC3NUS (Fig. 5A). The reason
for this behavior can be explained as follows: the specimen synthe-
sized by the US method and calcinated for 3 h at 750 °C (TC3US10)
is a 100% rutile polymorph form of TiO2 and hence more crystalline
than the TC3NUS specimen which is expected to contain both
Fig. 3. Variation of rutile content of the TiO2 specimens (NUS and US) with
calcination time.
anatase and rutile content [21]. Overall, the surface micrograph
of TC3US10 showed a more close packed and ordered appearance
than that of TC3NUS and can be considered as one of the advanta-
ges of using ultrasound during the synthesis.
It has also been observed that for the US synthesized specimens,
a calcination time of 3 h was enough to produce 100% phase trans-
formation from anatase to rutile in the synthesized titanium diox-
ide. Therefore, using this calcination time, two new titanium
dioxide specimens were synthesized using the ultrasound assisted
sol–gel method but using a different sonication time of 5 min and
15 min respectively. These specimens have also been analyzed
using the XRD and SEM methods and their properties (morphology
and phase presence) compared with the TC3NUS and TC3US10
specimens.
4.3. XRD study of the specimens synthesized with varying sonication
times
The X-ray diffractograms of the specimens synthesized using
differing sonication times are shown in Fig. 6. It can be seen from
the figure that the titanium dioxide synthesized by the US method
shows the presence of 100% rutile content (as indicated by absence
of any peak at 2h = 25°) when calcinated at 750 °C irrespective of
Fig. 4. Variation of crystallinity of the TiO2 specimens (NUS and US) with
calcination time.
 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191 189

Table 2 However, it is seen that the specimen TC3US10 is showing the

Crystallite size (nm) and dominant crystalline phase of the TiO2 specimens highest crystallinity amongst all the samples, which can be
synthesized at different calcination times.
explained on the basis of the crystallite size and also the yield of
Synthesis technique Specimen Crystallite Dominant phase (A: the reaction. The values of crystallite size (Table 3) show that the
size (nm) anatase, R: rutile) specimen TUS 3 is having the maximum crystallite size, which also
NUS or conventional sol TC0.5NUS 24 ± 1 A confirm that TC3US10 has the most rutile character. However, it is
gel technique TC1NUS 30 ± 1 A also important to note here that there is not much of a significant
TC2NUS 31 ± 1 A
difference amongst the US specimens but they do show a marked
TC3NUS 35 ± 1 R
Ultrasound assisted or US TC0.5US10 25 ± 1 A increase in rutile content and crystallinity as compared to the
sol–gel technique TC1US10 29 ± 1 A NUS specimen.
TC2US10 33 ± 1 R
TC3US10 39 ± 1 R
4.4. Effect of sonication time on the yield

The extent of yields obtained for the various specimens with

the sonication time used during the synthesis. From the diffracto-
grams, we can get the data related to the rutile content, crystallin-
ity and crystallite sizes of the specimens and this data has been
shown in Fig. 7, and Table 3 respectively.
From Fig. 7, it is seen that there is no difference in the rutile
content (100%) obtained for the three US synthesized specimens
while the NUS specimen (TC3NUS) shows much lower rutile con-
tent. Thus, it can be concluded that the use of ultrasound signifi-
cantly accelerates the phase transformation in titanium dioxide
from anatase to rutile. The trend in percentage crystallinity
(Fig. 7) also depicts a similar behavior. The rutile polymorph of
TiO2 shows better packing and more stable crystalline structure
than the meta-stable anatase polymorph and hence the US speci-
mens, which show rutile as the pre-dominant phase, show higher
percentage crystallinity as compared to the NUS specimen.
varying sonication time have been given in Table 4. It is seen again
that the US specimens show a good improvement in the yields as
compared to the NUS specimen. It is seen that initially as the son-
ication time is increased, an increase in the yield from TC3US5 to
TC3US10 (subjected to 10 min sonication) is observed and thereaf-
ter a marginal decrease in the yield from TC3US10 (subjected to
10 min sonication) to TC3US15 is obtained. This is attributed to
the fact that as the sonication time is increased initially, the overall
cavitational effects in the system increases and an increased expo-
sure to such cavitating conditions results in improvement in mass
transfer and reaction rates and thus a consequent increase in
yields. However, as the sonication time increases beyond 10 min
(TC3US10 specimen), the enhanced heat dissipation in the reaction
system results in partial vapourisation of the volatile 2-propanol
used as the reaction medium resulting in a shift of the reaction

A B

C D
Fig. 5. SEM micrographs of the specimens synthesized using various sonication times. (A) TC3NUS, (B) TC3US5, (C) TC3US10, (D) TC3US15.
190 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191

Fig. 6. X-ray diffractograms of the specimens synthesized at various sonication times.

Therefore, the TiO2 synthesized at higher sonic time input shows

lower crystallinity as depicted in Fig. 7. In the case of TC3US10
(10 min sonication time), the likely scenario is that there would
be an ideal balance between heat dissipation and cavitational
effects which would not cause local volatilization of 2-propanol
but rather the generated heat energy is utilized solely for acceler-
ating the phase transformation process.

4.5. SEM study of the specimens synthesized at various sonication

times

The SEM micrographs of the specimens synthesized at various

sonication times have been shown in Fig. 5. It is seen that with
an increase in the sonication time, a slow development of a block
type structure in the synthesized TiO2 is observed. The develop-
Fig. 7. % Rutile content and % crystallinity of the specimens synthesized at various ment of an ordered surface morphology is a characteristic of the
sonication times. US process. The structure however, seems to vanish at the speci-
men TC3US15 which seems to suggest that the higher sonication
times are having a detrimental effect on the synthesized product.
Table 3 At lower sonication times, the heat generated due to bubble col-
Crystallite sizes of the specimens synthesized using varied sonication times. lapse hastens the phase transformation from a meta-stable anatase
Specimen Crystallite size Dominant phase to more stable and crystalline rutile form which thereby shows an
(nm) (A: anatase, R: rutile) increasingly ordered surface morphology but at higher sonication
TC3NUS 35 ± 1 A times the integrity of the block type structure is lost. It may be
TC3US5 35 ± 1 R due to the fact that the more sustained impact over longer sonica-
TC3US10 39 ± 1 R tion times on the surface of the TiO2 ruptures the formed block
YC3US15 33 ± 1 R
type structure.

5. Conclusions
Table 4
Yields of the specimens obtained using varied sonication times.
The effect of calcination and sonication time on the phase trans-
Specimen Yields with variation (%)
formation of sol–gel synthesized (conventional and ultrasound-
TC3NUS 83.2 ± 1.9 assisted) TiO2 has been studied. With an increase in the calcination
TC3US5 84.32 ± 1
time (at constant temperature of 750 °C), there is an increase in the
TC3US10 93.2 ± 2.1
YC3US15 90.10 ± 1.5 rutile content of the specimens, signifying that at lower calcination
times the entire bulk of the specimen could not be exposed to the
high temperature and hence the meta-stable anatase phase was
intact. The introduction of ultrasound helped to produce reaction
contents with a lesser degree of agglomeration and thus helped
equilibrium to the left by Le-Chatelier’s principle and hence a the high temperature reach the inner recesses of the specimen
reduction in the yield is obtained. In addition, the significant quicker, hastening the phase transformation and achieve 100%
exposure to cavitating conditions over enhanced sonication time conversion from the anatase phase (favoured by the conventional
can disrupt the formation of a close-packed crystal structure. sol–gel process) to the rutile phase. After the optimization of
 D.V. Pinjari et al. / Ultrasonics Sonochemistry 23 (2015) 185–191
calcination time, the sonication time was also varied to study the
effect of sustained ultrasound contact on the reaction system. It
has been established that as the sonication time is increased till
an optimum time (10 min), there is an increase in the rutile con-
tent, crystallinity and yields. Increase beyond the optimum time
resulted in a detrimental effect on the system as the cavity collapse
energy was utilized for volatilization of reactants instead of the
main objective of accelerating the phase transformation. Thus, a
calcination time of 3 h and a sonication time of 10 min were estab-
lished as being the optimum parameters for obtaining 100% rutile
TiO2 with better morphological characteristics.
Acknowledgements
Authors would like to thank UGC (Govt. of India) and CSIR
(Govt. of India) for providing fellowship to carry out the proposed
research work.
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