利用表面活性剂十二烷基磺酸钠(SDSN)的调控合成不同粒径的硒模板和铂纳米空球(Pthollow),并将其修饰于玻碳(GC)基底即可制得Pthollow/GC电极;采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HR-TEM)和X射线光电子能谱等观察表征了Pthollow样品的形貌与组成;以甲醇为探针分子,研究Pthollow/GC和电沉积铂电极(Ptnano/GC)对甲醇氧化的电催化活性.结果表明,由铂原子簇团构筑的多孔铂纳米空球粒径均匀,分散性好;用4μmol·L^-1SDSN控制合成的直径为130 nm的Pthollow制备的Pthollow/GC电极对甲醇氧化的电催化活性最佳.
The selenium (Se) templates and hollow platinum (Pthollow) nanospheres with different sizes were controllably synthesized by adjusting the concentration of sodium dodecyl sulphonate (SDSN, CSDSN, μmol· L^-1) which was used as a surfactant. Accordingly, the Pthollow nanospheres modified glassy carbon electrode (Pthollow/GC) was prepared. The morphology and composition of Pthollow nanospheres were characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDX), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and X-ray diffraction (XRD) techniques. The electrocatalytic activities of Pthollow/GC and electrodeposited Pthollow particles modified glassy carbon electrode (Pthollow/GC) toward methanol oxidation were studied. The results showed that the uniform diameter sizes with well distributions were obtained with the synthesized porous Pthollow nanospheres constructed by Pt atom clusters. The best electrocatalytic activity toward methanol oxidation was achieved with the Pthollow/GC having a diameter of 130 nm synthesized with CSDSN = 4μmol· L^-1.