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The intercalation reactions of carbon cathode during electrolysis in molten Na3AlF6-Al2O3-CaF2, NaF and NaCl were studied. Samples of cokes heat-treated at several different temperatures were used as cathode in the electrolysis.It was observed that the d (002) spacing of the cokes changed during electrolysis, indicating the formation of lamellar compounds.The change was most appreciable in the system Na3 AlF6-Al2O3-CaF2.For the cokes heat-treated at low temperatures showed greater changes in d (002) than those heat-treated at high temperatures.This relation was very similar to that for reactions of carbons with metallic sodium.The compounds thus formed by electrolysis were, however, found to be fairly stable in the open air or in the water, in contrast to the instability of the sodium-carbon lamellar compounds.It was indicated by solid-mass spectrometry that a small amount of fluorine was present, in addition to sodium, in the product by electrolysis.

Reaction of Carbon Cathode with Electrolytes during Electrolysis in Molten Na3AlF6-Al2O3-CaF2