电化学方法制备纳米NiO及反应机理初探

采用电化学法一步制备了镍醇盐配合物Ni(OEt) 2 (acac) 2 (acac为乙酰丙酮基 ) ,并以其作为前驱体 ,控制一定水解条件制得胶体 ,分别在 4 5 0℃ ,60 0℃煅烧均得到具有立方晶型的纳米NiO粉体 .通过红外光谱 (FT_IR)、核磁共振 (1HNMR)、拉曼光谱 (Ramanspectrum)、X_射线粉末衍射 (XRD)、透射电子显微镜 (TEM)等手段对前驱体和NiO粉体进行了表征 .结果表明 ,电解合成的最佳温度为 30～ 4 0℃ ,不溶性镍醇盐配合物升温到 4 0～ 5 0℃即可溶解 .电解法制备得到的纳米NiO层呈球形单分散结构 ,粒径在 10～ 15nm左右 .本文同时讨论了电合成纳米NiO的反应机理

Electrochemical Preparation and Reaction Mechanism of Nanocrystalline NiO

Metallic nickel was electrochemically dissolved in absolute ethanol and acetylacetone mixed solutions and in the presence of Bu 4NBr (as an electron-conductive additive). The electrolyte solution containing the precursor was then directly hydrolyzed to obtain nanocrystalline NiO. The precursor was characterized by FTIR?HNMR?Raman spectra and the nano-powder was characterized by XRD and TEM. The results showed that the NiO powder after calcined at 450 ℃ had formed the cubic NaCl structure and the nanocrystalline NiO prepared by this method had narrow size distribution of 10～15 nm. Moreover, the product yield could be improved by controlling temperature below 30～40 ℃. The reaction mechanism was also discussed in this paper.