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In Situ X-ray Diffraction Study of the Thermal Decomposition of Selenogallates Cs 2 [Ga 2 (Se 2 ) 2- x Se 2+ x ] ( x = 0, 1, 2).
Inorganic Chemistry 2018 May 8
The selenogallates CsGaSe3 and Cs2 Ga2 Se5 release gaseous selenium upon heating. An in situ high-temperature X-ray powder diffraction analysis revealed a two-step degradation process from CsGaSe3 to Cs2 Ga2 Se5 and finally to CsGaSe2 . During each step, one Se2 2- unit of the anionic chains in Cs2 [Ga2 (Se2 )2- x Se2+ x ] ( x = 0, 1, 2) decomposes, and one equivalent of selenium is released. This thermal decomposition can be reverted by simple addition of elemental selenium and subsequent annealing of the samples below the decomposition temperature. The influence of the diselenide units in the anionic selenogallate chains on the optical properties and electronic structures was further studied by UV/vis diffuse reflectance spectroscopy and relativistic density functional theory calculations, revealing increasing optical band gaps with decreasing Se2 2- content.
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