物理化学学报 >> 2010, Vol. 26 >> Issue (03): 795-798.doi: 10.3866/PKU.WHXB20100241

材料物理化学 上一篇    

溶胶-凝胶法制备多孔晶体材料C12A7-Cl-

孙剑秋, 宫璐, 沈静, 林舟, 李全新   

  1. 中国科学技术大学化学物理系, 生物质洁净能源实验室, 合肥 230026
  • 收稿日期:2009-10-13 修回日期:2009-12-03 发布日期:2010-03-03
  • 通讯作者: 李全新 E-mail:liqx@ustc.edu.cn

Sol-Gel Preparation of Porous C12A7-Cl- Crystals

SUN Jian-Qiu, GONG Lu, SHEN Jing, LIN Zhou, LI Quan-Xin   

  1. Laboratory of Biomass Clean Energy, Department of Chemical Physics, University of Science&Technology of China, Hefei 230026, P. R. China
  • Received:2009-10-13 Revised:2009-12-03 Published:2010-03-03
  • Contact: LI Quan-Xin E-mail:liqx@ustc.edu.cn

摘要:

利用溶胶-凝胶法制备了多孔晶体材料C12A7-Cl- (Ca12Al14O32Cl2), 制备凝胶的原料是四水合硝酸钙、九水合硝酸铝、氯化钙、尿素和乙二醇. 混合溶液经过搅拌2-3 h形成溶胶, 再经350 ℃热处理后形成凝胶体, 最终在流动氩气气氛中1000 ℃烧结后得到材料. 用X射线衍射, 场发射扫描电子显微镜, 热重分析, 电子顺磁共振和离子色谱等方法表征合成的C12A7-Cl-多孔晶体材料. 结果表明, 利用溶胶-凝胶法成功地生成了C12A7 结构, 氯负离子是材料中存储的主要负离子. 此外, 从C12A7-Cl-晶体材料表面发射的氯负离子也被飞行时间质谱观测到. 上述结果说明溶胶-凝胶法可被用于制备C12A7-Cl-晶体材料.

关键词: 溶胶-凝胶, C12A7-Cl-, 表征, 发射

Abstract:

Present study provides an approach to produce porous crystal material of C12A7-Cl- (Ca12Al14O32Cl2) by sol-gel method. Reactants for the gel were Ca(NO3)2·4H2O, Al(NO3)3·9H2O, CaCl2, urea, and ethylene glycol. The mixture solution was stirred for 2-3 h to form the sol, after thermal treatment at 350 ℃, the formed gel was then sintered under flowing argon at 1000 ℃. The prepared porous crystal material was investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), thermogravimetric analysis (TGA), electron paramagnetic resonance (EPR), and ion chromatography (IC). Results indicated that the C12A7-Cl-material was successfully prepared via sol-gel method and the Cl- anions were the dominant anions stored in the bulk of the material. The emission of Clanions from the C12A7-Cl- surface was detected by time-of-flight mass spectrometry (TOF-MS). Our results show that the sol-gel method can be potentially useful in the development of C12A7-Cl- materials.

Key words: Sol-gel, C12A7-Cl-, Characterization, Emission

MSC2000: 

  • O647