用非晶态合金和纳米晶合金作电极材料各有利弊,而用酸性溶液制备的Ni-Co合金镀层存在内应力较大且电流效率低等不足.为此,采用电沉积技术在碱性镀液中制备了非晶-纳米晶Ni·Mo合金,利用X射线衍射(XRD)、扫描电镜(SEM)、能谱(EDS)、极化曲线等研究了电沉积工艺对镀层Mo含量、结构及形貌的影响.结果表明:镀层Mo含量随镀液中钼酸盐浓度增加而增加,随柠檬酸盐浓度增加、镀液温度升高、电流密度增大先增加后减小,pH值对镀层结构有显著影响;镀层Mo含量在21.00%～26.00%时,Ni-Mo合金镀层为非晶与纳米晶混合结构,非晶态相含量占60%以上,纳米晶的晶粒尺寸较小,镀层表面均匀、颗粒细小、致密性较高;10.0 g/LNa2MoO4·2H2O,64.0 g/L Na3C6H5O7·H2O,pH值10.0,电流密度5～8 A/dm2,温度35℃时,获得的镀层为非晶与纳米晶混合结构,且表面质量较好.
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