Issue 35, 2022

Scrutinizing particle size related bond strengthening in anatase TiO2

Abstract

A series of small, middle, and large anatase TiO2 particles were synthesized through the hydrolysis of titanium tetraisopropoxide (TTIP) to investigate the size-related chemical bond length and strength variation. Unit cell volume contraction with decreasing particle size is identified from Rietveld refinement of high-resolution synchrotron powder X-ray diffraction (PXRD) patterns. More titanium vacancies are also found for smaller anatase particles. Contrary to the variation in unit cell volume, a larger Debye temperature ΘD(TiO2) derived from the linear and nonlinear fitting of atomic displacement parameters (Uiso(TiO2)) as a function of temperature is revealed for smaller anatase particles. The length of the Ti–O bond is also shorter for smaller anatase particles. Furthermore, optical phonon frequencies blue-shifting with the decrease in anatase particle size are determined by Raman spectroscopy. X-ray photoelectron spectroscopy (XPS) analysis rules out the presence of a large amount of Ti3+, while optical diffuse reflectance measurement eliminates the existence of a large number of oxygen vacancies in all particles. Combining the analysis results of PXRD, thermogravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FTIR), more structural and surface hydroxyls (–OH) appear to exist in smaller anatase particles. It is the structural and surface –OH that are responsible for the size-related chemical bond length and strength variation in the as-synthesized anatase particles.

Graphical abstract: Scrutinizing particle size related bond strengthening in anatase TiO2

Supplementary files

Article information

Article type
Paper
Submitted
02 jul 2022
Accepted
05 avg 2022
First published
08 avg 2022

Dalton Trans., 2022,51, 13515-13526

Scrutinizing particle size related bond strengthening in anatase TiO2

J. Yu, A. Mamakhel, F. Søndergaard-Pedersen, M. Ceccato and B. B. Iversen, Dalton Trans., 2022, 51, 13515 DOI: 10.1039/D2DT02128E

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