Abstract

Hollandite-type compounds, KxNbyT8 - yO16 (x ≤ 1.15, 0 ≤ y ≤ 1) were prepared by high temperature reaction under H2 atmosphere. Black single crystals of Holladite-type K1.15Nb0.67Ti7.33O16 were obtained by heating a mixture of K2CO3, TiO2 and Nb2O5 with the molar ratio of 1 : 1 : 1 under H2 atmosphere at 1200°C for 1h. From single crystal X-ray diffraction analysis, the tetragonal lattice parameters of this compound are a = 1.02260(7) and c = 0.2974(1)nm, and the cystal structure refinement led to the final R-factors of R = 0.037 and Rw = 0.041 for 773 unique diffractions. The extent of solubility of niobium for powder samples was found to be y ≤ 1 in KxTi8 - yNbyO16 from solid state reaction under H2 atmosphere at 1200°C and the value of x ranged from 0.8 to 0.9.

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