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利用化学置换法在ｐ型Ｓｉ（１１１）表面制备了纳米微晶Ｐｄ，对其析氢反应催化活性进行了考察。采用阳极溶出法对沉积层进行了研究，并借助于Ｘ光电子能谱（ＸＰＳ）对表面和界面进行了分析，结果表明，表面沉积微晶Ｐｄ的ｐ型Ｓｉ电极在０．５ｍｏｌ／ＬＨ２ＳＯ４中的析氢过电位比裸Ｓｉ电极下降了近４５０ｍＶ；阳极溶出曲线在０．３６～０．３９Ｖ附近出现Ｐｄ的溶出峰；ＸＰＳ测试证明Ｐｄ沉积层呈不连续微晶弥散分布于基底表面，在Ｓｉ／Ｐｄ界面上形成了Ｐｄ的硅化物；ＸＲＤ分析结果证实Ｐｄ为纳米微晶结构。
Nanocrystalline Pd was prepared on the surface of p-type Si (111) by chemical substitution. The catalytic activity of hydrogen evolution reaction was investigated. The deposited layer was studied by anodic stripping method and the surface and interface were analyzed by means of XPS. The results showed that the p-type Si electrode with surface deposited microcrystalline Pd in 0.5mol / LH 2 SO 4 The hydrogen evolution overpotential decreased by nearly 450mV compared with that of bare Si electrode. The dissolution peak of Pd appeared near 0.36 ~ 0.39V in anodic dissolution curve. The XPS test showed that the Pd deposit was discontinuous and dispersed in the surface of Si / Pd interface formed on the Pd silicide; XRD analysis confirmed that the Pd nanocrystalline structure.