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Multiple Fluorine-Substituted Phosphate Germanium Fluorides and Their Thermal Stabilities.
Inorganic Chemistry 2016 December 6
Anhydrous compounds are crucially important for many technological applications, such as achieving high performance in lithium/sodium cells, but are often challenging to synthesize under hydrothermal conditions. Herein we report that a modified solvo-/hydro-fluorothermal method with fluoride-rich and water-deficient condition is highly effective for synthesizing anhydrous compounds by the replacement of hydroxyl groups and water molecules with fluorine. Two anhydrous phosphate germanium fluorides, namely, Na3 [GeF4 (PO4 )] and K4 [Ge2 F9 (PO4 )], with chainlike structures involving multiple fluorine substitutions, were synthesized using the modified solvo-/hydro-fluorothermal method. The crystal structure of Na3 [GeF4 (PO4 )] is constructed by the common single chains∞ 1 {[GeF4 (PO4 )]3- } built from alternating GeO2 F4 octahedra and PO4 tetrahedra. For K4 [Ge2 F9 (PO4 )], it takes the same single chain in Na3 [GeF4 (PO4 )] as the backbone but has additional flanking GeOF5 octahedra via an O-corner of the PO4 groups, resulting in a dendrite zigzag single chain∞ 1 {[Ge2 F9 (PO4 )]4- }. The multiple fluorine substitutions in these compounds not only force them to adopt the low-dimensional structures because of the "tailor effect" but also improve their thermal stabilities. The thermal behavior of Na3 [GeF4 (PO4 )] was investigated by an in situ powder X-ray diffraction experiment from room temperature to 700 °C. The modified solvo-/hydro-fluorothermal method is also shown to be effective in producing the most germanium-rich compounds in the germanophosphate system.
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