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In this paper we investigate the high-temperature structure of Co3O4, a compound that has been studied extensively over the last 60 years due to its unresolved high-temperature structure. In situ thermal analysis and x-ray diffraction confirm previously reported high-temperature structural changes and show that these changes are unrelated to the high-temperature decomposition to CoO. Raman-active peaks are also extinguished over the same temperature range. By considering the changing lattice parameter, A-O, and B-O bond lengths as well as cation size we are able to calculate the degree of inversion which reaches a maximum of 0.6. To further study the structure in this experimentally inaccessible range we quench samples and perform ex situ measurements including redox titration, x-ray photoelectron spectroscopy, and neutron diffraction. We do not observe any evidence of large oxygen vacancy concentrations or octahedral CoB3+ ions with high spin state. However, we do show an evolution in the magnetic moment from magnetic structure refinement from (2.4 μB) to (2.7 μB) that coincides exactly with the high-temperature anomaly and suggests partial inversion (0.46) of the spinel structure in fairly good agreement with the inversion calculated from bond lengths.

physical review. b./physical review. b

High-temperature structure of <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"><mml:mrow><mml:msub><mml:mi>Co</mml:mi><mml:mn>3</mml:mn></mml:msub><mml:msub><mml:mi mathvariant="normal">O</mml:mi><mml:mn>4</mml:mn></mml:msub></mml:mrow></mml:math> : Understanding spinel inversion using <i>in situ</i> and <i>ex situ</i> measurements

High-temperature structure of Co3O4 : Understanding spinel inversion using in situ and ex situ measurements