By Paul Hagenmuller

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Extra info for Inorganic Solid Fluorides. Chemistry And Physics

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This is the case for the alums M C r ( B e F ) « 1 2 H 0 (M = Rb, Cs, Tl, or N H ) (Lari-Lavassani et al, 1969) and manganese(III) derivatives such as C s M n F - H 0 (Riss and Vituhnovskaja, 1958), K M n F . H 0 (Edwards, 1971), and C s [ M n F ( H 0 ) ] (Bukovec and Kaucic, 1977). 2 4 2 6 5 3 4 2 2 4 2 7 4 2 2 4 2 2 2. 5 2 5 2 4 2 2 Hydrothermal Syntheses If hydroxyfluorides are prepared by hydrothermal synthesis (see Section III,A,2), single crystals either of hydrated fluorides or of anhydrous com­ pounds can also be grown.

Palladium tetrafluoride has been prepared in such a way by fluorinating P d F under 7 bars F at 300°C for several days (Rao et al, 1976). This method also allows one to collect very simply volatile fluorides after fluorination either of the corresponding metal (Ir I r F ; Bartlett and Rao, 1965) or of the oxide-fluoride ( T i O F -> T i F ) or even of a lower-valency fluoride ( B i F B i F ) (Tressaud et al, 1976b). The separation of fluorides having different volatilities also becomes easier: Tressaud et al (1976a) succeeded thus in isolating P t P t F from P t F .

Lithium fluoride crystals of 30 χ 30 χ 20 mm size obtained by this method are shown in Fig. 9. Finally, the possibility of growing small crystals by simple melting in gold or platinum tubes and slow cooling in a furnace must be pointed out. M a n y fluorides lead to crystals that can be used for x-ray diffraction studies, but no other details will be given on this very common technique. t x J C 2 + x 3 + 1 JC JC 4 2 2 2 2 D. CZOCHRALSKI METHOD The Czochralski method (1917) is a process for single-crystal pulling, starting with a small oriented seed.

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