A vacuum-tight cell for infrared spectroscopic investigations of extremely corrosive melts, e.g., molten fluorides, has been constructed and tested up to 750 degrees C. The cell has a gold-lined sample chamber and a diamond window transparent for the infrared light. It can be furnished with a gold piston that enables the recording of short-pathlength FTIR spectra of liquid samples. Solutions of Nb(V) in LiF-NaF-KF eutectic (FLINAK) with and without oxide additions have been investigated by FTIR and Raman spectroscopy. The presence of NbE72-, NbOF52-, and NbO2F43- complexes was established in the molten state at 600 degrees C. After solidification NbF72- was still the only Nb(V) all-fluoro complex present. Three oxofluoro complexes, NbOF63-, NbOF52-, and NbO2F43-, have been identified in the solid state. Typical frequency regions for the different complexes are established. Finally, it was shown that K2NbF7 can be used as an indicator to determine the oxide content of the sample melts.
