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The results of DSC studies of NaBH4–KBF4 mixtures are presented. It is shown by chemical analysis, XRD analysis, IR spectroscopy, and 11B and 9F MAS NMR that the decomposition of the mixtures starts at ~563 K to yield polyhedral borohydride compounds (predominantly B12H 12 2- ) in the solid residue. This temperature is much lower than the decomposition temperature of pure NaBH4 (749 K). The mechanism of formation of the B12H 12 2- anion has been proposed and confirmed. According to this mechanism, boron atoms from KBF4 are involved in the formation of this anion.
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