High surface area MgF2 was prepared by the sol–gel technique from magnesium alkoxides. The influence of different ratios of Mg(OCH3)2 to HF, of different magnesium alkoxides, catalysts, solvents as well as different aging times was investigated. XRD, MAS-NMR, FT-IR, thermal analysis and elemental analysis were applied to study the structure, composition and thermal behaviour of the bulk materials. The determination of the surface properties was accomplished with N2 and Ar adsorption–desorption isotherms.
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