催化学报

催化学报 ›› 2007, Vol. 28 ›› Issue (11): 963-969.

• 研究论文 • 上一篇    下一篇

一种含有亚微米孔洞的新型微孔磷酸盐晶体材料的合成及其生长机理

张莹1,2,田鹏1,周帆1,2,刘广宇1,2,刘中民1   

  1. 1 中国科学院大连化学物理研究所, 辽宁大连 116023; 2 中国科学院研究生院, 北京 100049
  • 收稿日期:2007-11-25 出版日期:2007-11-25 发布日期:2011-10-13

Hydrothermal Synthesis and Crystallization Mechanism of a Novel Microporous Phosphate with Submicron Holes

ZHANG Ying1,2, TIAN Peng1, ZHOU Fan1,2, LIU Guangyu1,2, LIU Zhongmin1*   

  1. 1 Dalian Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116023, Liaoning, China; 2 Graduate University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2007-11-25 Online:2007-11-25 Published:2011-10-13

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摘要： 采用水热法成功地合成了一种含有亚微米级孔洞的微孔磷酸盐晶体材料(记为HAP-TAP), 其形貌特征是: 六棱柱形的晶体表面分布着大量0.4～0.8 μm的亚微米级孔洞,孔洞内长有片层状晶体. 在样品晶化的过程中,通过控制合成时间,获得了纯六棱柱形晶体的大单晶(记为HAP). 使用扫描电子显微镜(SEM)、粉末X射线衍射(XRD)、红外光谱和电子能谱(EDX)对HAP-TAP独特形貌的形成机理进行了研究和揭示. HAP的单晶XRD数据表明, HAP是一种具有二维空旷骨架结构的新型微孔磷酸铝晶体,其分子式为Al5(OH)2(PO4)7(C2N2H10)3•0.5H2O. EDX分析结果表明,生长于六棱柱形晶体孔洞内的片层状晶体为磷酸钛铝材料.

关键词: 亚微米孔洞, 微孔磷酸盐, 水热合成, 生长机理

Abstract: Microporous phosphate crystals with submicron holes, HAP-TAP, was hydrothermally prepared. HAP-TAP is composed of two different crystals, the hexagonal prism crystals and the layer crystals. Its morphology was characterized by abundant submicron holes (0.4-0.8 μm) distributing on the surface of hexagonal prism crystals and the layer crystals growing in the holes. The process of crystallization was investigated by scanning electronic microscopy, powderX-raydiffraction (XRD), infrared spectroscopy, and energy dispersiveX-ray(EDX) spectroscopy. The hexagonal prism single-crystal HAP was obtained by adjusting the crystallization time. The single-crystal XRD results showed that HAP is a novel microporous aluminum phosphate with a formula of Al5(OH)2(PO4)7(C2N2H10)3•0.5H2O and two-dimensional open-framework structure. EDX results showed that the layer crystals located in submicron holes were titanic aluminum phosphates.

Key words: submicron hole, microporous phosphate, hydrothermal synthesis, crystallization mechanism