For the purpose developing an insoluble anode, nickel-tantalum and nickel-niobium alloys of 19 different compositions were prepared by vacuum arc melting and electron beam remelting processes. Anodic behavior of the alloys was studied in 0.5M H
2SO
4 and 1M NaCl at room temperature. The results showed that hypo-eutectoid nickel alloys containing less than 30wt.%Ta(Nb) dissolved severely both in sulfuric acid and in chloride solution at an anodic current of 5A/dm
2. The intermetallic compound, Ni
3Ta(Ni-50wt.%Ta) showed the lowest dissolution rate of 0.3g/A·Y and 1.69V vs. SCE in 0.5M H
2SO
4, while the compound Ni
3Nb showed somewhat higher dissolution rate in sulfuric acid under the galvanostatic condition. Electrode performance of the berthollide compound, Ni
3Nb was better in 1M NaCl than that in 0.5M H
2SO
4. However, the lowest dissolution rate of the alloy in 1M NaCl was 6.2g/A·Y at 5A/dm
2. Electron beam remelting of the alloys decreased chlorine and oxygen overvoltage remarkably and improved their electrochemical properties for the insoluble anode.
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