...

1 2 3 3

. ) (TiOSO4
) (NaCl . -
9 1 4 600C
750C 30 . 100C
. (XRD) X
) (TEM . 4
10 1
10-15 nm . NaCl
.
: X

1
2
3
4
5

. ) (TiO2

] .[1
] [23456 ] [78 ] [7
. TiO2
) (
.
.
.
] .[3
.

.
20-60nm .

.
.
].[910
TiO2
Billik . [9] Plesch TiO2 TiCL4 .
(NH4)2CO3 Billik . Plesch

] [10 TiOSO4 .
Na2CO3 TiOSO4 TiO2 .

 ...

TiO2 TiOSO4 NaCl

.
.

TiO2 4 .
36 .
10 1 20mm 10mm
. 4 400rpm .
600C 750C . NaCl
100C .
X .
XRD 1 :
] D = 0.9 /[(Bs Bm ). cos

)(1
D Bs CuK Bm
X ] .[910
SiO2 .
XRD
) (TEM . TEM
.
2
.

1 X 4
.
TiO2 TiOSO4 .

Scherer
grid

1
2

.1 4 .TiO2

2 3 X 600C 750C
. 2
600C . 3
750C .

.2 TiO2 30 600C .

.3 TiO2 30 750C .

 ...

4 TEM 30 600C
.
.

.4 TEM .TiO2 30 600C .

1
NaCl
.
.
2 30 600C
.

. NaCl 1
. ) (1
2
7 nm .
3 750C
.
2 .
600C

750C
700C .
.
) (A
R .
.
] .[11 1
12nm 20 nm
.
.
TEM 4
10-15 nm .
.
. TEM
.
.
.
.

.
.

X
.
.
. TEM
) X (10-15nm .

...

[1] K.D. Kim, T.J. Lee and H.T. Kim,"Optimal Conditions for Synthesis of TiO2
Nanoparticles in Semibatch Reactor", Colloid. Sur. A: Physicochem. Eng. Aspects 224
(2003) 1-9
[2] J. Yang, S. Mei and J.M.F. Ferreira, "Hydrothermal Synthesis of TiO2 Nanopowders
from Tetraalkylammonium Hydroxide Peptized Sols", Mater. Sci. Eng.C 15 (2001)
183185
[3] K. INSOO et al., "Method for Synthesizing Nano-Sized Titanium Dioxide
Particles", J. Etro. Sci. Eng. 2006
[4] J.G. Li, H. Kamiyama, X.H. Wang, Y. Moriyoshi AND T. Ishigaki, "TiO2
Nanopowders via Radio-Frequency Thermal Plasma Oxidation of Organic Liquid
Precursors: Synthesis and Characterization", J. Euro. Ceram. Soc. 26 (2006) 423428
[5] S.M. Oh and T. Ishigaki "Preparation of Pure Rutile and Anatase TiO2 Nanopowders
Using RF Thermal Plasma", Thin Solid Films 457 (2004) 186191
[6] P.T.M. Chau and U.T. D. Thuy, "Synthesis and Characterization of Nano-TiO2
Powder", Proceedings of the Ninth Asia Pacific Physics Conference (9th APPC), Hanoi,
Vietnam, October 2004, 25-31,
[7] W. Ye, T. Cheng, Q. Ye, X. Guo, Z. Zhang and H. Dang, "Preparation and
Tribological Properties of Tetrafluorobenzoic Acidmodified TiO2 Nanoparticles as
Lubricant Additives", Mater. Sci. Eng. A 359 (2003) 82-85
[8] G.L. Li and G.H. Wang, "Synthesis of Nanometer-Sized TiO2 Paeticles by a
Microemulsion Method", NanoStruc. Mater. 11 (1999) 663668
[9] P. Billik and G. Plesch, "Mechanochemical synthesis of nanocrystalline TiO2 from
liquid TiCl4", Scripta Materialia 56 (2007) 979-982
[10] P. Billik, et al., J. Phys. Chem. Solids (2007), doi:10.1016/j.jpcs.2007.02.010
[11] Z. Yuan and L. Zhang, "Influence of ZnO+Fe2O3 Additives on the
Anatase-to-Rutile Transformation of Nanometer TiO2 Powders", NanoStruc. Mater. 10
(1998) 1127-l 133

Mechanochemical Synthesis of Titanium Dioxide Nanoparticles

M. Salarii, M. Rezaeeii, S.M.M. Koieiii, S.P.H. Marashiiii, Z.M. Shabestariiv
i
m_salari@cic.aut.ac.ir
ii
m_rezaee@cic.aut.ac.ir
iii
piroozmarashi@maharfan.com
iv
zmsh@aut.ac.ir

Abstract
Nanosized titania particles, with typical particle size in the range of 10-15 nm have been
synthesized by the use of mechanochemical reduction. In this process, Titanyl sulphate
(TiOSO4) and NaCl powders were used as reactant and diluent phases, respectively. The
starting mixture of TiOSO4 and NaCl powders was loaded into a planetary ball mill at 400
rpm. Experiments were carried out at weight ratio NaCl:TiOSO4; 9:1. Milling was carried
out for four hours. After milling, the powder was annealed at 600C and 750C in an air
atmosphere for 30 minutes to form crystalline TiO2 particles. The NaCl powder was
removed by washing the annealed powder with distilled water. Annealed powders were
investigated by X-Ray Diffraction (XRD) and Transmission electron microscope (TEM).
Keywords: mechanochemical reduction, TiO2 nanoparticles, XRD, TEM

MSc Student, Department of Mining and Metallurgical Engineering, Amirkabir University of Technology
PhD Student, Department of Mining and Metallurgical Engineering, Amirkabir University of Technology
iii
Assistant Professor, Department of Mining and Metallurgical Engineering, Amirkabir University of Technology
iv
Lecturer, Department of Mining and Metallurgical Engineering, Amirkabir University of Technology
ii