金属阳极溶解法制备纳米氧化物NiAl_2O_4  

Synthesis of Nanosized NiAl_2O_4 by Sacrificial Anode

作　　者：朱传高[1] 朱其永[1] 周幸福[2] 褚道葆[2] 

机构地区：[1]淮南师范学院化学系,安徽淮南232001 [2]安徽师范大学有机化学研究所,安徽芜湖241000

出　　处：《精细化工》2005年第2期135-137,共3页Fine Chemicals

基　　金：安徽省高校青年教师科研资助计划(2004jq185)

摘　　要：在乙醇和乙酰丙酮混合溶液中,50～55℃,导电盐Bu4NBr浓度为0 040mol/L,控制阳极电流0 2A电解铝片6h,再电解镍片2h,制得前驱体NiAl2(OCH2CH3)(8 y)(acac)y[acac为乙酰丙酮基]。将电解液控制pH=8 5直接水解形成凝胶,凝胶经洗涤、干燥后在350℃煅烧2h,制得纳米NiAl2O4粉体,粒径20～30nm。用红外(IR)、差热-热重分析(TG-DTA)、X射线衍射(XRD)、电子透射技术(TEM)等手段对前驱体和纳米NiAl2O4进行了表征。The precursor NiAl_2(OCH_2CH_3)_((8-y))(acac)_y was synthesized by electrochemical dissolution of aluminum for 6 h and then nickel for 2 h at 0.2 A in ethanol and acetylacetone solution.Nanon NiAl_2O_4 powder was prepared from the electrolytic solution by direct sol-gel process under pH=8.5,drying and calcining at 350 ℃ for 2 h. IR spectrum,TG-DTA,XRD and TEM were used to investigate the structure of the precursor and nanosized NiAl_2O_4.The experiments showed that during electrolysis,the temperature controlled at 54～60 ℃ and concentration of Bu_4NBr of 0.040～0.045 mol/L as conductive additive could improve the current efficiency,and nanosized NiAl_2O_4 with a narrow size distribution of 20～30 nm can be obtained at a low calcination temperature of 350 ℃.

关 键 词：纳米NiAl2O4 电合成 镍、铝配合物 溶胶-凝胶 

分 类 号：O646[理学—物理化学]