Journal
INORGANIC CHEMISTRY
Volume 56, Issue 21, Pages 13349-13359Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.7b02105
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Funding
- CAMPUS FRANCE (PHC STEFANIK Project) [31799NM]
- Slovak bilateral project [SK-FR-2013-0039]
- Slovak Grant Agencies [APVV-15-0738, APVV-15-0479, VEGA-2/0116/14, VEGA-2/0114/16]
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Precise investigation of part of the phase diagram of KF-Al2O3 system was performed in an experiment combining different techniques. Solidified mixtures of KF-Al2O3 were studied by X-ray powder diffraction and high-field solid-state NMR spectroscopy over a wide range of compositions. To help with the interpretation of the NMR spectra of the solidified samples found as complex admixtures, we synthesized the following pure compounds: KAlO2, K2Al22O34, alpha-K3AlF6, KAlF4, and K2Al2O3F2. These compounds were then characterized using various solid-state NMR techniques, including MQMAS and D-HMQC. NMR parameters of the pure compounds were finally determined using first-principles density functional theory calculations. The phase diagram of KF-Al2O3 with the alumina content up to 30 mol % was determined by means of thermal analysis. Thermal analysis was also used for the description of the thermal stability of one synthesized compound, K2Al2O3F2.
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