Differential Scanning Calorimetry Study of Complex Fluorides of Zirconium, Tin, Vanadium, Silicon, Antimony, Molybdenum and Tellurium

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The enathalpy and temperature of the sublimation, evaporation and dissociation of nitrosyl or nitryl fluoride-zirconium, tin, vanadium, silicon, antimony, molybdenum and tellurium fluoride adducts were determined from DSC measurements. A closed-cell DSC technique was employed for this purpose and to postulate possible reaction mechanisms of the dissociation. Adducts of nitrosyl or nitryl fluoride with fluorides of zirconium, tin, vanadium, silicon, antimony, molybdenum and tellurium were produced using 80 mol% HF-20 mol% NO_2 as solvent. The following facts were found from the DSC measurements of these adducts. (NO)_2ZrF_6 and (NO)_2SnF_6 are converted into ZrF_4 and SnF_4, respectively, through two thermal dissociation steps. NOVF_6, (NO)_2SiF_6 and NOSbF_6 sublimate without prior thermal dissociation, but in the case of NOSbF_6 two transitions are observed. NO_2MOF_4 and (NO)_3Te_2F<11> are converted into glassy melts with thermal dissociation prior to final evaporation. The enthalpies and temperatures of all these reactions are estimated from the DSC measurements.
東北大学の論文