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The KBH4−NaBF4 mixture was studied by thermal analysis (differential scanning calorimetry). Chemical analysis, X-ray powder diffraction analysis, IR spectroscopy, and 11B and 19F MAS NMR spectroscopy showed that the primary stage of the complex pyrolysis process is a metathesis reaction between components to form a new mixture, NaBH4−KBF4, the decomposition of which with the release of gaseous products and the formation of polyhedral borohydride compounds (mainly B12H122-) in the solid residue begins at a temperature of about 563 K. At a certain ratio between reactants in the initial mixture KBH4−NaBF4, the B12H122- anion can form with the material participation of the BF4- anion.
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