Nb-doped TiO2 particles were prepared by heating a mixture of peroxotitanic acid and peroxoniobic acid in air. When the heating temperature was more than 1173 K, the dominant phase obtained was rutile TiO2, along with a small amount of TiNb2O7. The relationship between the lattice parameters of the obtained rutile TiO2 depended on the molar fraction of Nb/(Ti + Nb). In the case where peroxo compounds were used as a precursor, a change in the lattice parameters of the rutile TiO2 was observed within the lower XNb range, as compared to the alkoxide method. The results indicate that a homogeneous dispersion of doped Nb5+ ions in the obtained rutile TiO2 lattice was achieved by using peroxo compounds. Furthermore, the oxide particles obtained by using peroxo compounds had a lower activation energy of the carrier electrons (Ea) and oxygen vacancies, even though the heating procedure was carried out in air. The UV-vis absorption spectra and Raman spectra of the obtained oxide particles indicated that the dominant reaction of the decomposition of O22− ions in the TiO2 lattice was O22− → O2 + 2e− as a reducing agent.
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