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以H6P2Mo18O62·23H2O和(NH4)2C2O4·H2O为原料,首次采用室温固相反应合成出(NH4)6P2Mo18O62·12H2O纳米粉体,并运用元素分析、FTIR、XRD、TEM、TG-DTA和BET等技术对其组成、结构和性能进行了表征。发现(NH4)6P2Mo18O62·12H2O纳米粉体平均粒径为40nm,保留着杂多阴离子的Dawson结构,具有Dawson结构的特征衍射峰,比表面积为143.9m2·g-1,在445℃以下杂多阴离子有良好的热稳定性。在该固相反应中,研磨和放热反应热能可加速反应物分子的扩散速率和生成物分子的成核速率,使产物粒径减小;反应物含有结晶水和生成物H2C2O4·2H2O对形成小粒径的(NH4)6P2Mo18O62·12H2O纳米粉体起关键作用。
(NH4) 6P2Mo18O62 · 12H2O nanopowders were synthesized by solid-state reaction at room temperature for the first time using H6P2Mo18O62 · 23H2O and (NH4) 2C2O4 · H2O as raw materials. The elemental analysis, FTIR, XRD, TEM, TG-DTA and BET techniques Its composition, structure and performance were characterized. The average particle size of (NH4) 6P2Mo18O62 · 12H2O nanopowder was 40nm, which was Dawson structure with heteropolyanion. The characteristic peak of Dawson structure was observed. The specific surface area was 143.9m2 · g-1. The heteropolyanion below 445 ℃ Have good thermal stability. In the solid phase reaction, the heat of grinding and exothermic reaction can accelerate the diffusion rate of the reactant molecules and the nucleation rate of the product molecules, so that the product particle size is reduced; the reactants contain the crystallization water and the product H2C2O4 · 2H2O to form Small particle size (NH4) 6P2Mo18O62 · 12H2O nanopowders play a key role.