A pseudo-tetragonal tungsten bronze superstructure: a combined solution of the crystal structure of K-6.4(Nb,Ta)(36.3)O-94 with advanced transmission electron microscopy and neutron diffraction

作者：Sena Robert Paria; Babaryk Artem A^*; Khainakov Sergiy; Garcia Granda Santiago; Slobodyanik Nikolay S; Van Tendeloo Gustaaf; Abakumov Artem M; Hadermann Joke

来源：Dalton Transactions, 2016, 45(3): 973-979.

DOI：10.1039/c5dt03479e

The crystal structure of the K6.4Nb28.2Ta8.1O94 pseudo-tetragonal tungsten bronze-type oxide was determined using a combination of X-ray powder diffraction, neutron diffraction and transmission electron microscopy techniques, including electron diffraction, high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), annular bright field STEM (ABF-STEM) and energy-dispersive X-ray compositional mapping (STEM-EDX). The compound crystallizes in the space group Pbam with unit cell parameters a = 37.468(9) angstrom, b = 12.493(3) angstrom, c = 3.95333(15) angstrom. The structure consists of corner sharing (Nb, Ta)O-6 octahedra forming trigonal, tetragonal and pentagonal tunnels. All tetragonal tunnels are occupied by K+ ions, while 1/3 of the pentagonal tunnels are preferentially occupied by Nb5+/Ta5+ and 2/3 are occupied by K+ in a regular pattern. A fractional substitution of K+ in the pentagonal tunnels by Nb5+/Ta5+ is suggested by the analysis of the HAADF-STEM images. In contrast to similar structures, such as K2Nb8O21, also parts of the trigonal tunnels are fractionally occupied by K+ cations.

• 出版日期2016