在(25±2)℃下,从含有50 g/L RuCl3·nH2O、30.0 g/L乙酸钠、30.0 g/L二水合柠檬酸钠和15.0～50.0 g/L NiSO4·6H2O的溶液(pH 3.0)中,以1O～90 mA/cm2在铜基底上电沉积制备了Ru含量为5%～70%(原子分数)的Ni-Ru合金.采用X射线衍射(XRD)、扫描电子显微镜(SEM)和电化学方法,研究了镀液中NiSO4质量浓度和电流密度对沉积层组成、表面形貌、结构及电催化析氢活性的影响.结果表明,溶液中Ru优先析出并能促进Ni的沉积,镀层中Ru含量随着镀液中Ni2+质量浓度的提高而降低,低电流密度有利于获得Ru含量高的镀层.随着镀液中Ni2+质量浓度的降低或电流密度的提高,镀层表面形貌由较为平整、均匀变为多孔的颗粒状.镀层主要呈现面心立方Ni结构特征,且晶粒尺寸随镀层中Ru含量的增加而变小.Ni-Ru合金电极的析氢活性优于纯Ni,当镀层的Ru原子分数超过15%时,其析氢活性与纯Ru电极接近.
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