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在镀液中悬浮粒径为200～400 nm的ZrO2固体颗粒,以电沉积方法制备了Ni-S-Co/ZrO2复合电极。XRD和SEM测试结果表明,沉积层由非晶态的Ni、Co、S和单斜晶型的ZrO2粒子组成。镀层表面呈团粒状结构,无裂隙,与基体结合牢固。电化学测试结果表明,25℃时,Ni-S-Co/ZrO2复合电极在质量分数28%NaOH水溶液中,在电流密度100 mA/cm2下的超电势为145 mV,与未复合纳米ZrO2粒子的Ni-S-Co电极相比降低了50 mV。表明超细ZrO2的掺入有效提高了电极对析氢反应的催化效果。实验表明,沉积的最佳电流密度为70 mA/cm2,最适宜的ZrO2用量为15 g/L,采用Ni-S-Co作为过渡层可以显著改善复合镀层与基体的结合。
Ni-S-Co / ZrO2 composite electrode was prepared by electrodeposition of ZrO2 solid particles with particle size of 200-400 nm suspended in the bath. The results of XRD and SEM show that the deposited layer consists of amorphous Ni, Co, S and monoclinic ZrO2 particles. Coating surface was granular structure, no cracks, combined with the solid substrate. The results of electrochemical tests showed that the overpotential of Ni-S-Co / ZrO2 composite electrode was 145 mV at current density of 100 mA / cm2 in 28% NaOH aqueous solution at 25 ℃, which was in agreement with that of uncoated nano ZrO2 particles Ni-S-Co electrode is reduced by 50 mV. It indicates that the incorporation of ultrafine ZrO2 effectively improves the catalytic effect of the electrode on the hydrogen evolution reaction. The experimental results show that the optimal current density is 70 mA / cm2 and the optimum amount of ZrO2 is 15 g / L. Using Ni-S-Co as the transition layer can significantly improve the combination of the composite coating and the substrate.