A review on methods of synthesizing

nanostructures TiO2
Cite as: AIP Conference Proceedings 1963, 020067 (2018); https://doi.org/10.1063/1.5036913
Published Online: 09 May 2018

S. Munirah, Sh. Nadzirah, Z. Khusaimi, H. Fazlena, and M. Rusop

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AIP Conference Proceedings 1963, 020067 (2018); https://doi.org/10.1063/1.5036913 1963, 020067

© 2018 Author(s).
 A Review on Methods of Synthesizing Nanostructures TiO2

S. Munirah1, 2, a), Sh. Nadzirah1, Z. Khusaimi1, 2, H. Fazlena3, M. Rusop1, 4, b)

1
NANO-SciTech Centre (NST), Institute of Science (IOS), Universiti Teknologi MARA (UiTM), 40450
Shah Alam, Selangor, Malaysia.
2
Faculty of Applied Sciences, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor, Malaysia.
3
Faculty of Chemical Engineering, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor, Malaysia.
4
NANO-ElecTronic Centre (NET),Faculty of Electrical Engineering, Universiti Teknologi MARA (UiTM), 40450
Shah Alam, Selangor, Malaysia.

a)munirahsafiay@gmail.com
b)nanouitm@gmail.com

Abstract. Titanium dioxide (TiO2) is a well-known materials and being extensively investigated due to the stability of the
chemical structure, optical, physical, and electrical properties, also its biocompatibility. There are a lot of efforts have been
done to synthesis TiO2 since the previous years by using different kind of methods. In this review paper, we summarize the
methods of synthesizing nanostructured TiO2.

INTRODUCTION
TiO2 is a widely used nanomaterials because of its unique textural and structural characteristics [1]. TiO2 can be
deposited on many substrates such as glass slides [2], metal panels [3], silica glass [2], porcelain bricks, stainless steel
plates, quartz plates and many more [2]. TiO2 have been used in many applications such as photocatalytic systems [4],
solar cells [1], lithium batteries, protective anti-reflection coatings and wastewater treatment [5]. TiO2 exists in three
mineral forms which are anatase (tetragonal), rutile (tetragonal) and brookite (orthorhombic). Anatase phase mainly
used as photocatalyst [6], rutile phase used as white pigment in paint [1], while brookite phase are not much known
[7]. Hence, TiO2 are very versatile and can be used for so many other applications including solar cells, capacitors and
food colouring agent. Generally, TiO2 obtained in anatase phase at temperatures below 600°C and rutile phase starts
to occur at temperatures above 800°C. TiO2 mostly preferred in anatase phase because of high photocatalytic activity,
non-toxic, high specific area and photochemically stable [1].

FIGURE 1. Different phase of TiO2

8th International Conference on Nanoscience and Nanotechnology 2017 (NANO-SciTech 2017)

AIP Conf. Proc. 1963, 020067-1–020067-5; https://doi.org/10.1063/1.5036913
Published by AIP Publishing. 978-0-7354-1668-0/$30.00

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 TiO2 nanostructures are included nanorods, nanotubes, nanowires and mesoporous structures. In preparation of
TiO2 nanostructures, there are various different methods have been done such as hydrothermal method [1], chemical
vapor deposition [4], sputtering [2], spray pyrolysis [6], sol-gel method [8], anodization method [1], electron beam
evaporation [7], solvothermal method [1], electrodeposition [4] and sonochemical method [1]. This review will focus
on the different method of synthesizing TiO2 nanostructures.

SYNTHESIZING METHODS FOR TIO2 NANOSTRUCTURES

1) Sol-gel Method

Sol-gel method is a simple and widely used method in synthesizing TiO2 nanostructures. This method has some
advantages for deposition of thin film such as homogeneity, purity and ease of operation [8]. In sol-gel process, a sol
is formed from the hydrolysis and condensation of precursor molecules, which are usually metal alkoxides. The most
familiar and being used precursors are the tetra-ethoxide, iso-propoxide and n-butoxide of Ti [7]. The transition from
the liquid sol into the solid gel are due to the complete polymerization and loss of solvents [1]. In TiO2 sol-gel process,

Ti [OCH (CH3)2]n + H2O Ti [OCH (CH3)2]n-1 (OH) + CH (CH3)2 (OH) -------------------- (1)

Hydrolysis in (1) are to remove the remaining alkyl group from the precursor. Then, oxygen bridge was formed
via condensation within titanium metal through either route (2) or route (3). Equation (4) shows the formation of TiO2.

Ti (OH) + Ti (OH) Ti-O-Ti + H2O --------------------- (2)

Ti [OCH (CH3)2] + Ti(OH) Ti-O-Ti + CH (CH3)2 (OH) ---------------------- (3)

Ti [OCH (CH3)2]4 + 2H2O TiO2 + 4CH (CH3)2 (OH) ----------------------- (4)

Thin films can be deposited on substrates by dip-coating or spin-coating [9]. The limitations of sol-gel process is
the need to calcine the films at temperatures between 400°C-600°C to achieve good crystallinity and good bonding of
the sol-gel films with the substrates [7].

FIGURE 2. The SEM images of TiO2 nanostructures prepared by sol-gel method.

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 2) Hydrothermal Method
Hydrothermal method is conducted in steel pressure vessels called autoclaves with or without Teflon liners. The
synthesis are done in controlled pressure or temperature with the reaction is in aqueous solutions. The internal pressure
produced was determined by the temperature and the amount of the solution that added to the autoclave. Besides TiO2
nanoparticles, TiO2 nanowires, TiO2 nanorods and TiO2 nanotubes also can be produced by hydrothermal method.

FIGURE 3. TEM images of TiO2 nanoparticles prepared FIGURE 4. SEM images of TiO2 nanowires prepared
by hydrothermal method [10]. by hydrothermal method [1].

FIGURE 5. TEM images of TiO2 nanorods prepared FIGURE 6. TEM images of TiO2 nanotubes prepared
by hydrothermal method [1]. by hydrothermal method [1].

3) Electrodeposition

Electrodeposition is one of the most common technique in synthesizing TiO2. Electrodeposition is generally used
to produce a coating on a surface by the action of reduction at the cathode. The substrate to be coated is used as cathode
and immersed into a solution which contains a salt of the metal to be deposited. Salt solution of Ti-compound used in
electrodeposition are TiCl4, TiCl3 and Ti(SO4)2 [7]. Extra careful step needed to be taken in order to prevent the chosen
salt does not dissolved in the solvent and caused precipitation. Hence, hydrogen peroxide is added as an oxidant and

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surfactants also added to promote the growth and structure of TiO2 thin films [7]. TiO2 nanowires can be produced by
electrodeposition with the use an anodic alumina membrane (AAM) as template [1].

FIGURE 7. SEM image of TiO2 nanowires electrodeposited in AAM pores [1].

Another related technique is anodization of Ti metal which thin film is deposited on the surface of the anode.
Anodization of Ti metal produced TiO2 nanotubes and all anodization are regularly conducted at an ambient
temperatures [1].

FIGURE 8. SEM images of surface and cross-sectional morphologies of TiO2 nanotubes prepared by anodization method [1].

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 CONCLUSION
In this review, we summarize a few methods of synthesizing TiO2 nanoparticles, nanowires, nanorods and
nanotubes. TiO2 can be synthesis by variety of techniques such electrodeposition, sol-gel method, anodization and
hydrothermal method. A lot of effort have been done in synthesizing and investigating TiO2 nanoparticles and the
progresses in modifications of TiO2 nanostructures have brought many new applications and improve the
performances.

ACKNOWLEDGMENTS
The authors would like to thank NANO-Scitech Centre (NST), Institute of Science (IOS), Universiti Teknologi
MARA (UiTM) and Faculty of Applied Sciences UiTM and Universiti Teknologi MARA (UiTM).

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