Template-based growth of TiO₂ nanorods by sol-gel process
In this paper, the preparation of TiO2 nanorods by sol-gel-template process has been considered. The prepared sols were characterized by using FTIR spectroscopy, and the obtained nanorods were characterized by X-ray diffraction and SEM microscopy. SEM images show that TiO2 nanorods with uniform di...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2007
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| Cite this: | Template-based growth of TiO₂ nanorods by sol-gel process / A. Sadeghzadeh-Attar, M. Sasani Ghamsari, F. Hajiesmaeilbaigi, Sh. Mirdamadi // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2007. — Т. 10, № 1. — С. 36-39. — Бібліогр.: 21 назв. — англ. |
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| author | Sadeghzadeh-Attar, A. Sasani Ghamsari, M. Hajiesmaeilbaigi, F. Mirdamadi, Sh. |
| author_facet | Sadeghzadeh-Attar, A. Sasani Ghamsari, M. Hajiesmaeilbaigi, F. Mirdamadi, Sh. |
| citation_txt | Template-based growth of TiO₂ nanorods by sol-gel process / A. Sadeghzadeh-Attar, M. Sasani Ghamsari, F. Hajiesmaeilbaigi, Sh. Mirdamadi // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2007. — Т. 10, № 1. — С. 36-39. — Бібліогр.: 21 назв. — англ. |
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| container_title | Semiconductor Physics Quantum Electronics & Optoelectronics |
| description | In this paper, the preparation of TiO2 nanorods by sol-gel-template process has
been considered. The prepared sols were characterized by using FTIR spectroscopy, and the obtained nanorods were characterized by X-ray diffraction and SEM microscopy.
SEM images show that TiO2 nanorods with uniform diameter of about 100-200 nm and a
length of several micrometers. The results of XRD indicated that the TiO₂ nanorods were
crystallized in the anatase and rutile phases after annealing to 400-700 ºC up to 2 hours.
|
| first_indexed | 2025-11-30T22:39:20Z |
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Semiconductor Physics, Quantum Electronics & Optoelectronics, 2007. V. 10, N 1. P. 36-39.
© 2007, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
36
PACS 81.16.-c
Template-based growth of TiO2 nanorods by sol-gel process
A. Sadeghzadeh-Attar1, M. Sasani Ghamsari2, F. Hajiesmaeilbaigi2, Sh. Mirdamadi1
1Department of Metallurgy and Materials Engineering, Iran University of Science and Technology, Tehran, Iran
2Solid State Laser Research Group, Laser Research Center, AEOI, 11365-8486, Tehran, Iran
E-mail: msghamsari@yahoo.com
Abstract. In this paper, the preparation of TiO2 nanorods by sol-gel-template process has
been considered. The prepared sols were characterized by using FTIR spectroscopy, and
the obtained nanorods were characterized by X-ray diffraction and SEM microscopy.
SEM images show that TiO2 nanorods with uniform diameter of about 100-200 nm and a
length of several micrometers. The results of XRD indicated that the TiO2 nanorods were
crystallized in the anatase and rutile phases after annealing to 400-700 ºC up to 2 hours.
Keywords: TiO2 nanorods, sol-gel process, template-based growth, modifier ligands.
Manuscript received 23.12.06; accepted for publication 26.03.07; published online 01.06.07.
1. Introduction
In recent years, there has been increasing interest in one-
dimensional (1D) nanostructures (nanorods, nanowires,
nanotubes, nanofibers) because of numerous potential
applications in various areas such as photocatalysis,
solar energy, electronics, optics, sensor and so on [1-5].
Numerous methods have been developed for the
synthesis of 1D nanostructures such as vapor-liquid-
solid (VLS) [6], chemical vapor deposition (CVD) [7],
solution-liquid-solid (SLS) [8], laser-assisted catalytic
growth [9], electron beam lithography [10], sol-gel [11],
surfactant-directed [12], solvothermal [13], and the
filling of templates with colloidal oxide particles [14-
15]. Among them, the template assisted synthesis
method due to its uniform pore size, high density of
controllable-dimensions – shape pores, easy way of
preparation and relatively low cost of production has
been found as an effective way for the formation of 1D
nanostructures [16-17]. In this manner, the template is
dipped directly into the precursor solution for a required
period. Therefore, the preparation of nanorod materials
by template method needs to provide nanoparticles in
precursor solution. These nanoparticles can be prepared
by sol-gel process. This method is based on hydrolysis
and condensation reactions of molecular precursors such
as metal alkoxides and inorganic salts [18]. Metal
alkoxides which are used as precursor materials for sol-
gel process are generally highly reactive species. Thus,
the control of reactivity of metal alkoxides is necessary
in order to obtain sols and gels with desirable properties.
This control may be achieved through the addition of
"modifiers" such as β -diketones (e.g. acetylacetone),
carboxylic acids or other complex ligands [19].
However, there are some limitations and difficulties with
this technique such as weak driving force and low solid
content. Heating-sol-gel-template and sol-gel
electrophoresis are two reported methods for the
preparation of dense TiO2 nanorods, which can
overcome the limitations of the direct sol filling method
[20-21]. In this paper, the formation of TiO2 nanorods by
the method of template-assisted sol-gel has been
investigated. Also, the influence of a number of
processing parameters on the growth, structure and
morphology of TiO2 nanorods has been reported. The
studied samples were characterized by using FTIR, XRD
and SEM microscopy.
2. Experimental
2.1. Preparation of the TiO2-sol
The TiO2-sol is formed by mixing of titanium
tetraisopropoxide (TTIP, Merck %98≥ ), acetylacetone
(ACAC, Merck %5.99≥ ), deionized water and ethyl
alcohol (EtOH, Merck %8.99≥ ) at molar ratios of
1:1:3:20, 1:3:40:70 and 1:1:275:86. Briefly, TTIP is
dissolved in ethanol and then, a second solution is
prepared by mixing ethanol with water and ACAC. The
EtOH/ACAC/H2O solution was slowly added into the
TTIP/EtOH solution to form the TiO2 sol. The mixture
was then stirred for approximately 2 h at the room
temperature.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2007. V. 10, N 1. P. 36-39.
© 2007, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
37
2.2. Synthesis of TiO2 nanorods
The formation of TiO2 nanorods was done using direct
sol filling and heating-sol-gel-template method. The
porous anodic alumina templates (Whatman Anodisc 25)
with 60 µm thickness and 100-200 nm diameter pores
were used as template. The anodic alumina membranes
(AAMs) were firstly boiled in ethanol at about 75-77 ºC
for 10 min to enhance the hydrophilicity of alumina pore
with TiO2-sol, and then these anodic alumina templates
were immersed into TiO2-sol solutions (at room
temperature and about 80 ºC) for different dipping times
(10-60 min). After drying in the air at room temperature
for 24 h, the prepared specimens were put into a muffle
furnace and then were heat-treated as the followed
procedure. The samples were firstly held at 100 ºC for 8-
10 h to completely remove the residual water. For
preparation of anatase TiO2, the samples were heated up
to 400 and 500 ºC at the rate of 2.5 ºC/min and held at
this temperature for 2 h. For preparation of rutile TiO2,
the specimen heated up to 700 ºC rapidly to avoid the
formation of the low temperature phase of anatase and
held at this temperature for 2 h, the furnace was shut
down and the samples were cooled back to room
temperature naturally.
2.3. Characterization of TiO2 nanorods
The size and morphology of TiO2 nanorods were
characterized by scanning electron microscopy (SEM,
CamScan MV2300). The surface layer was removed by
mechanical polishing of the anodic alumina membrane
and then the anodic alumina membrane was dissolved
away by immersion in the 6M NaOH solution at room
temperature at 10 min. Finally, it was washed several
times with distilled water to remove the dissolved AAM
and the remaining NaOH solution. FTIR spectra were
recorded at the room temperature with a Bruker (model
Vector 22) spectrophotometer in the range of 400-
4000 cm−1. The phase structure characterization of TiO2
nanorods was carried out by a Philips PW 1800 diffrac-
tometer using filtered monochromatized CuKα radiation.
3. Results and discussion
For a better control of the hydrolysis-condensation
process and preparation of stable TiO2 sol, we have to
use the acetylacetone as modifier. Fig. 1 shows FTIR
spectra of TiO2 sols at various molar ratios in the
presence of acac-modifier. Infrared spectra (Fig. 1c)
clearly exhibit bands at 1590 cm−1 (ν (C-O)+ν (C-C)),
1450 and 1380 cm−l ( δ (CH3)), 1180 and 1080 cm−l
( ρ (CH3)) due to acetylacetonat-groups which have
bound to titanium.
Acetylacetone provides a strongly bind with
precursors and complex species that remain bound to
titanium. The hydrolysis reaction in the presence of
acetylacetone is incomplete and acetylacetonat-groups
still remain bound to Ti even when hydrolysis is
preformed with a large excess amount of water (H2O/Ti
ratio = 275).
The size and shape of the final product is deeply
dependent on the size and shape of template. So, a
uniform template means regular and ordered guest.
Fig. 2 shows a SEM image of AAM template used in
this article. From the cross-sectional image, it can be
confirmed that the uniform-size pores were arranged
ideally over the sample.
Fig. 3 shows the XRD spectra of TiO2 nanorods
annealed at 400, 500 and 700 ºC for 2 h. The peak
positions and their relative intensities in samples are
consistent with the standard powder diffraction pattern
of anatase TiO2 for Fig. 3a, b and rutile TiO2 for Fig. 3c,
respectively. Comparison of the XRD patterns shows
that there are identical peaks in both samples. The broa-
dening of TiO2 peaks is due to the small particle size.
Fig. 2. SEM images of AAM template: (a) top and (b) side views.
Fig. 1. FTIR spectra of the TiO2 sols with various molar
ratios of TTIP/ACAC/EtOH/H2O 1:1:275:86 (a), 1:3:40:70
(b), 1:1:3:20 (c).
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2007. V. 10, N 1. P. 36-39.
© 2007, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
38
Fig. 3. XRD pattern of the TiO2 nanorods annealed at 400 ºC
(a), 500 (b), 700 (c).
Fig. 4. SEM images of TiO2 nanorods grown in AAM
template: lower (a) and higher (b) magnification images of the
nanorods.
Fig. 4 shows SEM image of the grown TiO2
nanorods in the AAM template with diameter of 100-
200 nm and length of several micrometers. The length
and diameter of nanorods can be changed by changing of
the dipping time.
Fig. 4b shows an individual TiO2 nanorods picture
that is continuous and uniform through the entire length
of the rods. The diameter of these nanorods almost
coincides with AAM template pores diameter. This
indicates that the diameter of the prepared nanorods is
controllable by the pore size of AAM template.
Meanwhile the high density of the nanorods fabricated
by heating-sol-gel process is compared with direct sol
filling process without hitting.
4. Conclusions
In summary, TiO2 nanorods with the anatase and rutile
structures have successfully been prepared by sol-gel
template process. Uniformly sized TiO2 nanorods of
approximately 100-200 nm in diameter, length of several
micrometers and with large areas have been grown. The
nanorods have the desired stochiometric chemical
composition with anatase and rutile crystal structures
after annealing at 400, 500 and 700 ºC for 2 h,
respectively.
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|
| id | nasplib_isofts_kiev_ua-123456789-117771 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-8034 |
| language | English |
| last_indexed | 2025-11-30T22:39:20Z |
| publishDate | 2007 |
| publisher | Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| record_format | dspace |
| spelling | Sadeghzadeh-Attar, A. Sasani Ghamsari, M. Hajiesmaeilbaigi, F. Mirdamadi, Sh. 2017-05-26T17:20:51Z 2017-05-26T17:20:51Z 2007 Template-based growth of TiO₂ nanorods by sol-gel process / A. Sadeghzadeh-Attar, M. Sasani Ghamsari, F. Hajiesmaeilbaigi, Sh. Mirdamadi // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2007. — Т. 10, № 1. — С. 36-39. — Бібліогр.: 21 назв. — англ. 1560-8034 PACS 81.16.-c https://nasplib.isofts.kiev.ua/handle/123456789/117771 In this paper, the preparation of TiO2 nanorods by sol-gel-template process has been considered. The prepared sols were characterized by using FTIR spectroscopy, and the obtained nanorods were characterized by X-ray diffraction and SEM microscopy. SEM images show that TiO2 nanorods with uniform diameter of about 100-200 nm and a length of several micrometers. The results of XRD indicated that the TiO₂ nanorods were crystallized in the anatase and rutile phases after annealing to 400-700 ºC up to 2 hours. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics Template-based growth of TiO₂ nanorods by sol-gel process Article published earlier |
| spellingShingle | Template-based growth of TiO₂ nanorods by sol-gel process Sadeghzadeh-Attar, A. Sasani Ghamsari, M. Hajiesmaeilbaigi, F. Mirdamadi, Sh. |
| title | Template-based growth of TiO₂ nanorods by sol-gel process |
| title_full | Template-based growth of TiO₂ nanorods by sol-gel process |
| title_fullStr | Template-based growth of TiO₂ nanorods by sol-gel process |
| title_full_unstemmed | Template-based growth of TiO₂ nanorods by sol-gel process |
| title_short | Template-based growth of TiO₂ nanorods by sol-gel process |
| title_sort | template-based growth of tio₂ nanorods by sol-gel process |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/117771 |
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