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By Paul Hagenmuller
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Extra info for Inorganic Solid Fluorides. Chemistry And Physics
Sample text
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.