物理化学学报 >> 2004, Vol. 20 >> Issue (12): 1472-1475.doi: 10.3866/PKU.WHXB20041215

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乙二醇甲醚中电解锡电解液直接水解制备纳米SnO2

周幸福; 赵俊峰; 何惠; 褚道葆   

  1. 安徽师范大学化学与材料科学学院,芜湖 241000
  • 收稿日期:2004-05-13 修回日期:2004-07-29 发布日期:2004-12-15
  • 通讯作者: 周幸福 E-mail:Zhouxf@nju.edu.cn

Electrochemical Dissolution of Tin in Ethylene Glycol Monomethyl Ether and Direct Hydrolysis of the Electrolyte for Preparation of Nano-sized SnO2

Zhou Xing-Fu; Zhao Jun-Feng; He Hui; Chu Dao-Bao   

  1. School of Chemistry and Materials Science, Anhui Normal University, Wuhu 241000
  • Received:2004-05-13 Revised:2004-07-29 Published:2004-12-15
  • Contact: Zhou Xing-Fu E-mail:Zhouxf@nju.edu.cn

摘要: 采用锡金属为阳极,在无隔膜电解槽中,电化学溶解锡于乙二醇甲醚中制备得到纳米SnO2前驱体Sn(OCH2CH2OCH3)4,将电解液直接水解经溶胶-凝胶法制备纳米SnO2,前驱体通过拉曼和红外光谱进行表征.纳米SnO2采用X射线粉末衍射(XRD)和透射电子显微镜(TEM)进行表征.实验表明,电解合成的Sn(OCH2CH2OCH3)4能够溶解于乙醇中, 适宜作为溶胶-凝胶(sol-gel)法制备纳米SnO2的原料,制得的纳米SnO2经600 ℃煅烧后呈球形单分散结构,晶型为四方锡石型, 比表面为62.58 m2·g-1,平均粒径在(10.0±0.4) nm左右.产率为89.3%,电流效率为86.9%.

关键词: Sn(OCH2CH2OCH3)4,  锡,  有机电解合成,  溶胶-凝胶,  纳米SnO2

Abstract: Metallic tin was directly dissolved in ethylene glycol monomethyl ether and Sn(OCH2CH2OCH3)4 was obtained. The products were characterized by using FT-IR and Raman spectrum. The results show that direct electrochemical preparation of tin complexes has high current efficiency and electrolysis yield, and Sn(OCH2CH2OCH3)4 can be dissolved in ethanol solution and directly used as sol-gel precursor for preparation of nanometer SnO2. The results also show that nano-sized SnO2 prepared by this method has tetragonal cassiterite structure with a narrow size distribution of (10.0±0.4) nm.

Key words: Sn(OCH2CH2OCH3)4,  Tin,  Organic electrolysis preparation,  Sol-gel,  Nano-sized SnO2