Fused salt electrolysis obtaining uranium dioxide has been demonstrated to be applicable to uranyl fluoride resulting from the hydrolysis of uranium hexafluoride. The potential-pO
2- (negative logarithm of the activity of O
2- ion) diagram was referred for guidance in electrowinning of UO
2 from fused halides. Acceptors of O
2- ion were found to produce good melts with sufficient dryness for obtaining sound UO
2. Polarograms of uranyl reduction showed that uranium oxide would exist in the form of UO
2 as an intermediate species at low concentrations of UO
2(VI). Carbon anodes in molten solution containing UO
2(VI) would act as UO
2 electrodes prior to the electrolysis, so that low cell voltages such as 0.05V were sufficient at low current densities. Crystalline UO
2 particles produced in an electrolytic pilot unit with a capacity of 1kg oxide had a density of up to 10.75g/cm
3 and total impurities were less than 0.1%.
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