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化学学报
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化学学报 ›› 2004, Vol. 62 ›› Issue (24): 2379-2385. 上一篇    下一篇

研究论文

过氧氨三乙酸钛配合物分子前体热分解制备纯钛基复氧化物

周朝晖, 洪麒明, 邓远富   

  1. 厦门大学化学系, 固体表面物理化学国家重点实验室, 厦门, 361005
  • 投稿日期:2004-04-15 修回日期:2004-06-28 发布日期:2014-02-17
  • 通讯作者: 周朝晖,E-mail:zhzhou@xmu.edu.cn E-mail:zhzhou@xmu.edu.cn
  • 基金资助:
    国家重点基础研究发展规划(No.001CB108906)和国家自然科学基金(No.20021002)资助项目.

Pure Ti-based Mixed Oxides Prepared from the Thermal Decompositions of Molecular Precursors of Peroxo Complexes Coordinated with Tris(hydroxycarbonylmethyl)amine Trivalent Anion Titanate(Ⅳ)

ZHOU Zhao-Hui, HONG Qi-Ming, DENG Yuan-Fu   

  1. Department of Chemistry, State Key Laboratory of Physical Chemistry of Solid Surfaces, Xiamen University, Xiamen 361005
  • Received:2004-04-15 Revised:2004-06-28 Published:2014-02-17

PDF

469

被引次数

19

在pH=2.5～4.0的条件下,以四氯化钛、过氧化氢和氨三乙酸为原料反应得到四种过氧酸钛配合物(NH4)4[Ti2O～(O2)2(ta)2]·4H2O (1), K4[Ti2O(O2)2(ta)2]·6H2O (2), Sr2[Ti2O(O2)2(ta)2]·10H2O (3)和Ba2[Ti2O(O2)2(ta)2]·10H2O (4) (H3ta=C6H6O6N).配合物的EA, UV-vis, IR和X射线单晶分析表明它们含有相同的双核过氧氨三乙酸钛的阴离子结构,钛原子与过氧基团、四齿氨三乙酸和桥氧七配位.3和4中的阳离子锶和钡分别与周围的水分子和羧基氧形成九配位和十配位.配合物1, 3和4在空气中600℃分解,XRD分析表明分别得到金红石型TiO2, SrTiO3和四方BaTiO3纯相.

关键词: 钛酸盐, 前驱体, 热分解, 过氧氨三乙酸

Different peroxo titanate(Ⅳ) complexes coordinated with tris(hydroxycarbonylmethyl)amine trivalent anion including ammonium, potassium, strontium and barium salts (NH4)4[Ti2O(O2)2(ta)2]·4H2O (1), K4[Ti2O(O2)2(ta)2]·6H2O (2), Sr2[Ti2O(O2)2(ta)2]·10H2O (3) and Ba2[Ti2O(O2)2(ta)2]·10H2O (4) were obtained directly from the triad system of TiCl4-H2O2-H3ta [H3ta=tris(hydroxycarbonylmethyl)amine] in pH 2.5～4.0. These complexes were characterized with elemental analysis, UV-vis and IR spectra. X-ray structural analysis shows that all complexes contain a similar dimeric anion structure, in which titanium atom is coordinated heptagonally by a peroxo group, a tetradenatate tris(hydroxycarbonylmethyl)amine trivalent anion ligand and a bridging oxygen atom. The cation Sr2+ and Ba2+ are coordinated enneahedrally and decagonally by water molecules and carboxyl groups of tris-(hydroxycarbonylmethyl)amine trivalent anion ligand respectively. The ammonium, strontium and barium salts can be decomposed stoichiometrically into the expected low-temperature phases of rutile TiO2, SrTiO3 and tetragonal BaTiO3 at the temperature of 600℃ respectively, which has been confirmed by XRD characterization.

Key words: titanate, precursor, thermal decomposition, peroxo tris(hydroxycarbonylmethyl)amine