In the temperature range between 600° and 965°, the progress of the reactions in NdF
3-Ca-CaCl
2 reaction system had been observed by use of a'hot thermocouple with a scoop' apparatus which was first introduced here for the direct visual observation of high temperature solid-solid or solid-liquid reactions. The direct visual observation with X-ray diffraction analysis revealed that in prior to reduction of NdF
3 a low melting liquid phase containing 0.8 wt.% of NdF
3 was primarily formed through the interaction of solid CaCl
2 at around 700°. The liquid was comprised of NdF
3, NdCl
3, CaCl
2, and CaClF. It clearly indicated that the reduction reaction of NdF
3 with Ca in Ca saturated Ca-CaCl
2 melt was a homogeneous liquid-liquid reaction and its reaction rate was fast. The Nd metal was produced as aggregates of each particulate because the reaction sites of NdF
3 are not confined at the NdF
3 surface but dispersed in the molten salt.
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