非水体系中电解镍中间产物制备纳米NiO  

Electrochemical Dissolution of Nickel in Nonaqueous Solution

作　　者：周幸福[1] 韩爱杰[1] 褚道葆[1] 林昌健[2] 田中群[2] 

机构地区：[1]安徽师范大学化学与材料科学学院有机化学研究所,芜湖241000 [2]厦门大学固体表面物理化学国家重点实验室,厦门361005

出　　处：《物理化学学报》2002年第7期613-616,共4页Acta Physico-Chimica Sinica

基　　金：国家自然科学基金(29873039); 安徽省自然科学基金(00046112); 安徽省教育厅科研资助(2002kj116)项目

摘　　要：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.Metallic nickel was electrochemically dissolved in absolute ethanol and acetylacetone solution in the presence of Bu4NBr(as electron conductive additive). The electrolyte solution containing the precursor was then directly hydrolyzed to obtain nanocrystalline NiO. The precursor was characterized by FTIR?1HNMR?Raman spectra and the nano powder was characterized by XRD and TEM. The results showed that the NiO powder after hydrolysis was amorphous but formed the cubic NaCl structure when calcined at 350 ℃,the NiO powder have a narrow size distribution of 5～10 nm after annealed at 600 ℃. Characterization of the electrochemical product revealed that Ni(OEt)2(acac)2 was formed by anode dissolution of nickel in ethanol and acetylacetone mixed solution. The experiments also showed that the precursor of the nanocrystalline NiO prepared by this method can be dissolved in ethanol solution when temperature increase to 40～50 ℃region.

关 键 词：电解 纳米NIO 镍阳极 非水体系 溶胶-凝胶 拉曼光谱 纳米氧化镍 

分 类 号：O646[理学—物理化学]