In situ synchrotron powder X-ray diffraction (PXRD) study was conducted on sodium and potassium tetrafluoroborate (NaBF and KBF) to elucidate structural changes across solid-solid phase transitions over multiple heating-cooling cycles. The phase transition temperatures from diffraction measurements are consistent with the differential scanning calorimetry data (∼240 °C for NaBF and ∼290 °C for KBF). The crystal structure of the high-temperature (HT) NaBF phase was determined from synchrotron PXRD data.
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