The influences of annealing on the microstructure and the performance of electrocatalytic oxidation of Cu46Zr44·5Al7.5Gd2 amorphous alloy were investigated by operating heat treatment in the vacuum annealing furnace. It is found that structural relaxation occurred in the internal structure of amorphous alloy after annealing treatment, which will cause a significant effect on the relative electrochemical performance. Choosing annealing temperature of 300 °C and holding time of 20 min, hydrofluoric acid corrosion treatment was applied on the relaxation structural stage ribbons. According to cyclic voltammetry and chronoamperometry curve graphs, it is found that it has a high oxidation peak as an electrode, whose corresponding electric potential is −0.11 V and current density is 0.0187 A cm−2. After reusing the experimental samples for 20 cycles, the electrocatalytic oxidation property on methyl alcohol is found to gradually decline and then stabilize. At 1-5 experiment cycles, the effect of electrocatalyst is relatively good, which proves that the sample ribbons can be recycled.
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