以乙酰丙酮钯为前驱体,甲醛为还原剂,聚乙烯吡咯烷酮( PVP)为保护剂, N,N-二甲基甲酰胺( DMF)为溶剂,在一定量碘化钾存在下,采用油浴法快速合成出形貌单一、大小均匀的立方体Pd纳米颗粒,平均粒径约10 nm。利用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、 X-射线粉末衍射(XRD)、 X-射线光电子能谱(XPS)等对产物进行了表征。制备Pd纳米立方体的最适宜Pd(acac)2:PVP:KI摩尔比为1:9:4。所制备的Pd纳米立方体对甲酸电氧化的催化活性是商业Pd黑的1.8倍。
Pd nanoparticles with uniform size and well-defined cubic structures were synthesized with palladium acetylacetonate as a precursor , formaldehyde as a reducing agent , polyvinylpyrrolidone ( PVP) as a stabilizer, N, N-dimethyl formamide as a solvent in the presence of an appropriate amount of KI by oil-bath heating for 3 h.The products were characterized by transmission electron microscopy ( TEM ) , scanning electron microscopy ( SEM ) , X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD).The optimum molar ratio of Pd(acac)2:PVP:KI for the preparation of Pd nanocubes was 1:9:4.The electrocatalytic activities of the as-prepared Pd nanocubes towards formic acid oxidation demonstrated 1.8 times greater than that of Pd black .