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采用纯镍为阳极,乙酰丙酮和乙醇的混合溶液中加入少量有机胺导电盐为电解液,施加一定电流使镍溶解,然后将电解液直接水解,控制一定的水解条件,制备得到纳米NiO粉体.采用拉曼光谱、红外光谱、元素分析、XRD和TEM分别对电解得到的纳米NiO前驱体和纳米NiO进行了分析与表征,并探讨了电化学溶解镍金属法制备纳米NiO反应的影响因素.电化学溶解镍金属得到的前驱体为Ni(OEt)2(acac)2,这种不溶性镍醇盐配合物升温至40～50℃即可溶解于乙醇溶液中,可直接应用于溶胶-凝胶(Sol-gel)过程.水解后的纳米NiO呈无定形结构,350℃煅烧后形成立方晶型NaCl结构,纳米NiO经600℃煅烧后粒径分布在5～10nm.该方法理论上为二价不溶性金属醇盐经溶胶凝胶工艺制备纳米氧化物材料提供了一条新的途径
Adopting pure nickel as the anode, adding a small amount of organic amine conductive salt into the mixed solution of acetylacetone and ethanol as the electrolyte, applying a certain current to dissolve the nickel, and then directly hydrolyzing the electrolyte to control certain hydrolysis conditions to prepare the nano-NiO powder The nano NiO precursor and nano NiO obtained by electrolysis were analyzed and characterized by Raman spectroscopy, infrared spectroscopy, elemental analysis, XRD and TEM, respectively. The influencing factors of NiO nano - reaction prepared by electrochemical dissolution of nickel metal were also discussed. Ni (OEt) 2 (acac) 2 is obtained by electrochemical dissolution of nickel metal. This insoluble nickel alkoxide complex can be dissolved in ethanol solution when heated to 40 ~ 50 ℃ and can be directly applied to sol - gel (NiO) nanomaterials were obtained by sol-gel process.The nanosized NiO was amorphous and calcined at 350 ℃ to form cubic NaCl.After calcined at 600 ℃, the NiO particles had a size distribution of 5 ~ 10nm.The method was theoretically bivalent Insoluble metal alkoxide provides a new way to prepare nanometer oxide material by sol-gel process