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Direct Conversion of TiO2 Sol to Nanocrystalline Anatase at 85 °C

Published online by Cambridge University Press:  31 January 2011

K. I. Gnanasekar ,
V. Subramanian ,
J. Robinson ,
K. I. Gnanasekar ,
K. I. Gnanasekar ,
K. I. Gnanasekar ,
J. C. Jiang ,
Fanney E. Posey  and
B. Rambabu
K. I. Gnanasekar
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
V. Subramanian
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
J. Robinson
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
K. I. Gnanasekar
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
K. I. Gnanasekar
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
K. I. Gnanasekar
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
J. C. Jiang
Affiliation:
Mechanical Engineering Department, Louisiana State University, Baton Rouge, Louisiana 70803
Fanney E. Posey
Affiliation:
Biotechnology Center For Fuels and Chemicals, National Renewable Energy Laboratory, 1617 Cole Blvd, Golden, Colorado 80401
B. Rambabu*
Affiliation:
Surface Science, Spectroscopy and Solid State Ionics Laboratory, Department of Physics, Southern University and A&M College, Baton Rouge, Louisiana 70813.
*
a)Address all correspondence to this author. e-mail: rambabu@grant.phys.subr.edu
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Abstract

Nanocrystalline TiO2 anatase with particle size in the range of 5–7 nm has been prepared by in situ cracking of the sol at 85 °C, thereby avoiding the intermediate gel formation process. Hydrolysis of Ti(O-isoPr)4 was carried out in excess of 2-propanol to keep the suspension of fine particles from agglomeration. Differential thermal analysis, thermogravimetric analysis, differential scanning calorimetry, powder x-ray diffraction (XRD), and electron microscopy have been used to characterize the samples. Gel to crystalline conversion, which requires a temperature of at least 400 °C, can be achieved by digesting the TiO2 sol at 85 °C. XRD and selected area electron diffraction patterns show the presence of a small amount of brookite phase along with the major anatase phase. High-resolution transmission electron microscopy shows that the average grain size of TiO2 particle remains around 5–9 nm even when heated at 510 °C.

Type
Articles
Information
Journal of Materials Research , Volume 17 , Issue 6 , June 2002 , pp. 1507 - 1512
Copyright
Copyright © Materials Research Society 2002

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