以SnCl4·5H2O和氨水为原料,用超重力-水热法制备了纳米SnO2粉体。利用X射线衍射(XRD)、透射电镜(TEM)、高分辨透射电镜(HRTEM)和物理吸附仪(BET)等分析手段对其进行表征。考察了反应物浓度、反应温度和陈化时间等实验条件对纳米SnO2粉体的晶体结构、粒度及分散性的影响。结果表明,在SnO2溶液浓度为0.05mol/L、水热温度240~280℃以及陈化时间3~8h得到的粉体结晶性良好、比表面积大(90~170m2/g)、粉体的颗粒大小在2~6nm左右,并具有良好的分散性。
Abstract
SnO2 nanocrystals have been prepared by high-gravity precipitation followed by hydrothermal aging, using SnCl4·5H2O and ammonia as the starting materials. The structure and particle size of SnO2 were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM). The influence of varying the thermal hydrolys is temperature, reactant concentrations and hydrothermal aging time on the crystal structure, morphology and particle size are discussed. The SnO2 powder was shown to exhibit good crystallinity with a particle size of 2-6nm, high specific surface area (90-170m2/g) and good dispersibility. The optimized conditions were found to be thermal hydrolysis temperature 240-280℃, reactant concentration (SnCl4) 0.05mol/L and hydrothermal aging time 3-8h.
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1]李建平, 王悦, 高晓光, 等. 微结构气敏传感器敏感薄膜制备方法的研究[J]. 真空科学与技术, 2005, 20(3): 161-165.
[2]张谢群, 余家国, 赵修建, 等. 二氧化锡薄膜的制备和应用研究进展[J]. 化学试剂, 2003, 25(4): 203-206.
[3]张晓顺, 邱竹贤, 翟秀静, 等. 超声波化学沉淀法制备纳米二氧化锡[J]. 东北大学学报, 2005, 26(4): 265-267.
[4]连进军, 李先国, 冯丽娟, 等. 溶胶-凝胶-冷冻干燥技术制备纳米二氧化锡及其表征[J]. 化学世界, 2004(4): 171-174.
[5]文仕学, 陈士仁, 唐电, 等. 纳米级二氧化锡的制备及其形态结构[J]. 氯碱工业, 1996(8): 23-25.
[6]李泉, 曾广赋, 席时权. 二氧化锡纳米粉末的热处理与微结构[J]. 应用化学, 1995, 12(2): 67.
[7]苗鸿雁, 李永强, 罗宏杰, 等. 水热合成纳米氧化锡粉体工艺因素研究[J]. 中国粉体技术, 2003, 9(4): 26-29.
[8]SONG K C, KANG Y. Preparation of high surface area tin oxide powders
by a homogeneous precipitation method[J]. Materials Letters, 2000, 42(5):283-289.
[9]RAMSHAW C. Higee distillation—An example of process intensification
[J]. Chemical Engineering, 1983, 13: 389-397.
[10]CHEN Jianfeng, WANG Yvhong, GUO Fen, et al. Synthesis of nan-oparticles with novel technology:highgravity reactive Precipitation[J]. Industrial Engineering and Chemical Research, 2000, 39(4): 948-954.
[11]CHEN Jianfeng, WANG Yvhong, GUO Kai, et al. Synthesis of nano-cubic
CaCO3 by high-gravity reactive precipitation[J]. Acta Metallurgica Sinica,
1999, 35(2): 179-183.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}