由镁、铝醇盐配合物合成纳米粒子MgAl_2O_4尖晶石  

Synthesis of Nano-sized Spinel MgAl_2O_4 Particle by Magnesium and Aluminum Alkoxo Complex

作　　者：朱其永[1] 王凤武[1] 褚道葆[2] 

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

出　　处：《无机化学学报》2007年第7期1282-1286,共5页Chinese Journal of Inorganic Chemistry

基　　金：安徽省自然科学基金(No.070414270X;KJ2007B339ZC);淮师院科研重点项目(No.2006LKP01ZD)

摘　　要：制备尖晶石微粉的方法很多，主要有共沉淀法、焙烧法、溶胶．凝胶法、气相氧化法、热分解法及有机醇盐法。其中金属醇盐水解法效果很好，但由于传统化学方法合成醇盐是以MXn[X为Hal，R，H，NR2，N（SiMe3）2，O，OR]等与醇进行交换反应．有过程复杂且原料不易得到，产率低，纯度达不到要求及后续分离烦琐等缺点，因而应用受到限制。Mg and A1 alkoxide complex was synthesized in a cell without battery separator by electrochemical dissolution of aluminum for 6 h and magnesium for 1.8 h at 45℃ in ethanol solution of 0.04 mol ·dm^-3 （Bu4N）Br with a current density of 100 mA·cm^-2. IR and Raman spectroscopy were used to characterize the structure of the precursor of MgAl2O4. The results show that the current efficiency attains 98.4% and the precursor is MgA12 （OCH2CH3）5（acac）3. The acac-group-containing precursor could prevent it from agglomeration. The xerogel was obtained by drying in vacuum for 24 h and hydrolysis under pH≈8.5 of the precursor, which was heated at 350 ℃ for 2 h to obtain the nano-MgA12O4 powder. XRD and TEM were used to investigate the structure of nanoMgA12O4. The result suggests that the xerogel with an average particle size of 10 nm and the Nano-sized Spinel MgA12O4Particle of 12 nm thus obtained are with high purity.

关 键 词：电解 镁 铝醇盐 溶胶-凝胶 纳米MgAl2O4 

分 类 号：O646[理学—物理化学] TB321[理学—化学]