碳载Sb-Pb-Pt电催化纳米材料的制备与结构表征

Preparation and Characterization of Nano material of Pt Pb Sb Supported on Glassy Carbon

:通过电化学方法在玻碳表面沉积催化物质研制Sb Pb Pt合金纳米材料。运用循环伏安(CV)、石英晶体微天平 (EQCM)、扫描隧道显微镜 (STM)和X 光电子能谱 (XPS)等技术对其进行表征。结果指出 ,碳载Sb Pb Pt电催化纳米材料的稳定性明显高于电有机合成中常用的Pb和Sb等电极。在酸性介质中碳载Sb Pb Pt电催化纳米材料电极上氢的析出电位负移至 - 0 45V ,有较高的电还原应用价值。通过EQCM技术对纳米薄膜合金电极的形成过程进行原位跟踪和STM观察 ,表明所研制的Sb Pb Pt纳米材料是由粒度均匀的纳米颗粒组成的合金薄膜。

The electrocatalysts Pt-Pb-Sb nano-material supported on glassy carbon(GC) were prepared by electrochemical co-deposition method.The structure and properties of these electrocatalysts were studied through techniques of cyclic voltammetry,electrochemical quartz microbalance (EQCM),scanning tunneling microscopy (STM.) and X-ray photoelectron spectroscopy (XPS).The results demonstrated that the hydrogen evolution on the prepared electrocatalysts was postponed to -0.45 V,i.e.,200 mV was shifted negatively in comparison with the hydrogen evolution on a platinum electrode.In addition,the oxidation potential of Pb and Sb components in the alloy film was positively shifted to above 0.15 V,which was much higher than the oxidation potential of Pb and Sb metal electrode.The stability of the alloy thin film electrode was confirmed to be higher than that of Pb,Sb,Cu metal electrodes employed usually in organic electrosynthesis.The process of formation of alloy film was studied by means of EQCM,STM and XPS.The results converged to illustrate that the surface of the alloy thin-film was constructed of nano-particles with regular size of about 10 nano-meters.