柠檬酸络合法制备NiTiO3纳米粉体  

PREPARATION OF NANO-SIZED NiTiO_3 PARTICLES BY CITRIC ACID CHELATING PROCESS

作　　者：郝品[1] 黄剑锋[1] 曹丽云[1] 贺海燕[1] 

机构地区：[1]教育部轻化工助剂化学与技术重点实验室 陕西科技大学,西安710021

出　　处：《硅酸盐学报》2010年第5期868-872,共5页Journal of The Chinese Ceramic Society

基　　金：国家自然科学基金(50942047);教育部博士点基金(2007070-8001);陕西科技大学科研创新团队基金(TD09–05);陕西科技大学博士科研基金(BS08–09);陕西科技大学研究生创新基金资助项目

摘　　要：以无机镍盐和钛酸四丁酯为起始原料,柠檬酸为络合剂,采用溶胶–凝胶法制备了NiTiO3纳米粉体。通过X射线衍射、扫描电镜和红外光谱研究了柠檬酸加入量对钛酸镍纳米粉体相组成、显微结构以及晶粒生长活化能的影响。结果表明:在制备过程中加入柠檬酸能明显降低其晶粒生长活化能;随柠檬酸加入量从0g增加至柠檬酸与溶液中阳离子(Ni2++Ti4+)的摩尔比为1:1时,纳米NiTiO3的晶粒生长活化能由60.19kJ/mol降低到43.07kJ/mol;制备的粉体为纯净的NiTiO3物相,结晶性较好。700℃煅烧后NiTiO3粉体颗粒形状为六方形片状结构,粉体的粒子尺寸分布均匀,粒径约为20～30nm。NiTiO3 nanocrystallite powder was prepared via the sol–gel method using inorganic nickel salt and tetrabutyl titanate as raw materials, and citric acid as chelating agent. The influences of citric acid addition on the phase composition, microstructure and growth activation energy of the powders were investigated by X-ray diffraction, scanning electron microscopy and infrared spectros-copy. The results show that the growth activation energy of NiTiO3 nanocrystallite can be significantly decreased by adding citric acid. With the increase of the mole ratio of citric acid to cations （Ni2＋ ＋ Ti4＋） in the solution from 0 to 1：1, the growth activation energy decreases from 60.19 kJ/mol to 43.07 kJ/mol, and the as-prepared NiTiO3 powder is monophase and well-crystallized nanocrystallite. The NiTiO3 powder calcined at 700 ℃ has hexagonal flake structure and the uniformed powder particle size distribution, and the particle size is about 20–30 nm.

关 键 词：钛酸镍 柠檬酸 溶胶–凝胶法 纳米粉体 

分 类 号：TQ138.13[化学工程—无机化工]