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以乙酰丙酮钯为前驱体,聚乙烯吡咯烷酮(PVP)为稳定剂,N,N-二甲基甲酰胺(DMF)为溶剂,一氧化碳为还原剂,在一定量甲酰胺的存在下,控制CO的流速,100℃油浴加热3 h,可以得到形貌单一的四角枝状Pd纳米晶,单枝呈多级结构特征。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)对其结构进行表征。所合成的多级四角枝Pd纳米晶对甲酸的电催化氧化活性约为商业Pd黑的2.6倍。
In the presence of a certain amount of formamide, the precursor of palladium acetylacetonate, polyvinylpyrrolidone (PVP) as stabilizer, N, N-dimethylformamide (DMF) as solvent and carbon monoxide as reducing agent Flow rate and heated in oil bath at 100 ℃ for 3 h, a single tetragonal dendritic Pd nanocrystal was obtained. The single branch showed multi-stage structure. Its structure was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of the synthesized multi-order tetragonal Pd nanocrystal for formic acid was about 2.6 times that of commercial Pd black.