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Reproduced from [126], A. I. Agulyansky, E. L. Tikhomirova, V. Y. Kuznetsov, V. T. Kalinnikov, Zh. Neorg. Khim. 33 (1988) 85, Copyright 1988, with permission of "Nauka" (Russian Academy of Sciences) publishing. Synthesis of Ta and Nb fluorides 51 LiNbOF4 and remainders of LiF, yielding Li2NbOF5 (curve 6) [126]. Thus, the sequence of phases that are formed in hydrofluoride synthesis of lithium-niobium fluoride compounds is: (NH4)3NbOF6 - (NH4)2NbOF5 LiNbOF 4 - Li2NbOF5. The same method was successfully used for the synthesis of other alkali metal oxyfluoroniobates, MNbOF4 and M2NbOF5, where M = Li, Na, K, Rb and Cs.

Rakov et al. also describe the preparation of Ca(NbF6)2 [79] and MgNbF7 [80]. Galy, Andersson and Portier reported on the thermal treatment (at 700°C), in a sealed ampule, of a mixture containing LiF, Nb2O5 and NbF5, leading to the preparation of Li2NbOF5 [81]. 25 Synthesis ofTa and Nb fluorides Table 8. Physical-chemical properties ofNbF5 and TaF5 (after Galkin [71] and Rabinovich and Havin [72]). 8 HC1; HNO3; Cone. H2SO4; Ethanol; Chloroform; CC14; CH3COOH Cone. HNO3; Cone. HC1; Hot H2SO4; Chloroform; CC14; CS2 Vapor pressure - P(t°C), ton- Dissolves in The process can be represented as follows: lOLiF + Nb 2 O 5 + 3NbF 5 = 5 Li 2 Nb0F 5 (8) The same compound, Li2NbOF5, can be obtained by another method as well [81], in which LiF interacts with gaseous NbOF3.

Ikrami and coworkers investigated interactions that take place in systems containing either lithium carbonate or alkali earth metals or some transition metals and ammonium hydrofluoride. Thus, the fluorination of lithium carbonate, Li2CO3, [106], Magnesium oxide, MgO, [107], oxides or carbonates of calcium and barium [108] results in the formation of simple fluorides characterized by a low oxygen impurity level. Fluorination of cobalt oxide, CoO, and nickel oxide, NiO, yield stable complex fluorometalates of ammonium - (NH4)2MF4 and (NH4)3MF5, where M = Co or Ni.

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