Crystallite size dependent cation distribution in nanostructured spinels studied by nmr, mössbauer spectroscopy and XPS

Owing to the structural flexibility of spinels, providing a wide range of physical and chemical behavior, these materials have been considered as a convenient model system for the investigation of the size dependent properties of complex ionic systems. In this work, quantitative formation is obtained on the crystallite size dependent ionic configuration in nanosized spinel oxides prepared by mechanochemical processing of the corresponding bulk materials. Experimentally determined values of the crystallite size and of the mean degree of inversion of nanostructured spinels are used to calculate the volume fraction of interfaces/surfaces and their thickness in the nanomaterials

Mechanochemical synthesis of amorphous and crystalline Na₂P₂S₆-elucidation of local structural changes by X-ray total scattering and NMR

The development of all-solid-state sodium-ion batteries as an alternative energy storage system to lithium based techniques demands for sodium conducting solid electrolytes and an understanding of the sodium conduction mechanism governed by the local structure of these glass-ceramic materials. Na2P2S6 was synthesized in an amorphous state with subsequent crystallization. The change of the local structure before and after crystallization was analyzed in detail regarding the presence of structural building blocks such as [P2S6]2−, [P2S6]4−, [P2S7]4−, and [PS4]3−. The structure of the crystalline phase differs markedly compared to the corresponding amorphous phase