无机材料学报

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磷酸镍空旷结构材料的水热合成及其影响因素

王秀丽1,2; 高秋明1   

  1. 1. 中国科学院上海硅酸盐研究所高性能陶瓷和超微结构国家重点实验室, 上海 200050; 2. 中国科学院研究生院, 北京 100039
  • 收稿日期:2004-05-28 修回日期:2004-07-12 出版日期:2005-05-20 网络出版日期:2005-05-20

Hydrothermal Syntheses and Effect Factors of Nickel Phosphates with Open-frameworks

WANG Xiu-Li1,2; GAO Qiu-Ming1   

  1. 1.State key Laboratory of High Performance Ceramics and Superfine Microstructure; Shanghai Institute of Ceramics; Chinese Academy of Sciences; Shanghai 200050; China; 2.Graduate School of Chinese Academy of Sciences; Beijing 100039; China
  • Received:2004-05-28 Revised:2004-07-12 Published:2005-05-20 Online:2005-05-20

摘要: 在水热条件下,考察了1NiCl2·6H2O-mH3PO4-nNH4F-pNH3·H2O-40H2O(n=0、3) 体系中空旷结构过渡金属磷酸镍材料的合成影响因素(原料、pH值、Ni/P比、模板剂和矿化剂等),并给出了材料的晶化区域图.在实验过程中得到的产物包括已知结构的24元环微孔材料VSB-1[1]和VSB-5[2]、12元环微孔材料A、层状材料B[3]、氢键型微孔材料C[4].采用XRD、FT-IR和TG对所合成的材料进行了表征.所合成几种材料的XRD图都在较低的2θ角处出现了衍射峰,表明它们可能具有比较空旷的骨架结构.实验证明该体系中矿化剂、pH 值和Ni/P比对产物的影响较大.值得说明的是文献报道在没有F离子的情况下不能合成出VSB-1[1],而我们在没有F离子的条件下合成了VSB-1.

关键词: 水热合成, 空旷结构材料, 磷酸镍, 影响因素

Abstract: Under hydrothermal synthetic conditions and from 1NiCl2·6H2O-mH3PO4-nNH4F-pNH3·H2O-40H2O(n=0, 3) system, we synthesized five kinds of materials
containing microporous VSB-1 and VSB-5 with 24 member rings, microporous sample A Ni12(HPO4)6(PO4)2(OH)6 with 12 member rings, layered
structural sample B NH4NiPO4·H2O, and microporous sample C (C2H10N2)[Ni(H2O)6](HPO4)2 with 8 member rings linked
by hydrogen bonds. They were characterized by XRD, FT-IR and TG. The effect factors of raw materials, pH, Ni/P ratio, template agents, and mineralization agent on synthetic products were investigated. The phase maps were also provided.
The effect factors of pH, Ni/P ratio, and mineralization agent play important roles in the synthetic processes. It is important that we synthesized VSB-1
without F ions.

Key words: hydrothermal syntheses, materials with open frameworks, nickel phosphates, effect factors

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