酸蒸气水热法合成钒取代水合碱式钨钼酸锆纳米晶体及热收缩Zr(WMo)_(0.93)V_(0.14)O_(7.93)化合物

Nanocrystals of Tungstate/Molybdate Zirconium Hydroxide Hydrate Substituted by Vanadium and Zr(WMo)_(0.93)V_(0.14)O_(7.93) Contraction Compound:Synthesis with Acidic Steam Hydrothermal Method

研究了酸蒸气水热法(ASH)合成VWMo.H2O时,酸蒸气源溶液的浓度,反应温度,填满度与反应时间等4个因素对晶体成核和生长两个阶段的影响。确定了以上4个影响因素的优化匹配条件,制备了VWMo.H2O纳米晶棒,并且对产物进行了表征。HCl-ASH法和HNO3-ASH法合成的VWMo.H2O化学式分别为Zr(WMo)0.93V0.14O6.93(OH0.92Cl0.08)2.(H2O)2和Zr(WMo)0.93V0.14O6.93(OH)2.(H2O)1.64;两者都与ZrMo2O7(OH)2.(H2O)2为同构化合物。以VWMo.H2O为前驱物在773K合成了立方热收缩化合物β-Zr(WMo)0.93V0.14O7.93。

The influences of the concentration of the acidic steam source solution,reaction temperature,filling degree of the container and the duration of the ASH on the nucleation and crystal growth processes were discussed when synthesizing VWMo·H2O by Acidic Steam Hydrothermal（ASH） route.Conditions for the above four factors to prepare VWMoH2O nanocrystalline rods were optimized and the products were characterized using ICP,XRD,TG-DSC,SEM,FTIR,TMA.The chemical formulas of VWMo·H2O are Zr（WMo）0.93V0.14O6.93（OH0.92Cl0.08）2·（H2O）2 and Zr（WMo）0.93V0.14O6.93（OH）2·（H2O）1.64 for the title nanocrystals prepared by HCl-ASH and HNO3-ASH routes,respectively.Both of them are isomorphic compounds with ZrMo2O7（OH）2·（H2O）2.By annealing VWMo·H2O at 773 K,the cubic β-Zr（WMo）0.93V0.14O7.93 was prepared and its negative thermal expansion property was measured.