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Synthesis and Structural Determination of the Disordered Bixbyite Cu 3‐ x Sb 1+ x O 5.5+3 x /2 with Spin‐Glass Behaviour
Author(s) -
Spasovski Martin,
Avdeev Maxim,
Söhnel Tilo
Publication year - 2019
Publication title -
chemistry – an asian journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.18
H-Index - 106
eISSN - 1861-471X
pISSN - 1861-4728
DOI - 10.1002/asia.201801835
Subject(s) - bixbyite , crystallography , neutron diffraction , paramagnetism , magnetization , powder diffraction , ternary operation , magnetic susceptibility , rietveld refinement , materials science , x ray crystallography , chemistry , antimony , oxide , analytical chemistry (journal) , diffraction , crystal structure , inorganic chemistry , condensed matter physics , physics , optics , chromatography , quantum mechanics , magnetic field , computer science , programming language , metallurgy
The ternary copper antimony oxide Cu 3‐ x Sb 1+ x O 5.5+3 x /2 ( x= 0.23) has been synthesized under 0.8–1.3 MPa pO 2 at 1022–1082 °C. Rietveld refinements of X‐ray and neutron powder diffraction patterns concluded that the oxide adopts a bixbyite type structure, crystallising in the cubic space group Ia‐ 3 with the unit cell parameter a= 9.61164(4) Å at room temperature from powder neutron diffraction data. The cationic 8b and 24d sites were found to be occupationally disordered where both Cu and Sb could be found on both sites. This is supported by X‐ray absorption spectroscopy experiments showing more than one possible Cu environment. There was a significant net deficiency of oxygen in the compound which was first inferred from observations of a thermochromic‐like phenomena and also seen from in situ high temperature neutron diffraction experiments. Magnetic susceptibility and magnetization measurements show paramagnetic behaviour with spin‐glass like transition below 6 K.