| 水热法合成多金属氧酸盐棒状超细晶体 |
| Hydrothermal Synthesis of Rodlike Ultrafine Polyoxometalate Crystallite |
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| 摘要: 以SrCl2·6H2O、(NH4)6P2Mo18O62·nH2O为原料，在PEG-600/H2O微乳体系中于80～130 ℃温度下水热反应8～12 h，从而制得一种多金属氧酸盐棒状超细晶体，组成是Sr3P2Mo18O62·nH2O。该超细晶体具有长棒状形貌、高结晶度且分散性能较好，长度范围在10.0～20.0 μm，径度在1.0～2.0 μm。对反应体系中的PEG-600/H2O体积比(VPEC-600∶VH2O)、水热温度以及(NH4)6P2Mo18O62·nH2O/SrCl2·6H2O质量比(WPOMs∶WSrCl2·6H2O)3个影响因素进行了探讨，结果表明：VPEC-600∶VH2O主要对棒状超细晶体的形貌、长径比以及晶体结晶度有着重要影响，体积比在范围VPEC-600∶VH2O=(1.50～2.00)∶1.00有利于大长径比的棒状超细晶体的形成；水热温度则优选80～130 ℃范围，过低则不发生反应，过高则发生了多金属氧酸盐与PEG-600的氧化-还原反应；WPOMs∶WSrCl2·6H2O基本上不影响超细晶体的形成。还初步探讨了该棒状超细晶体的形成机理。 |
| 关键词: 微乳体系 水热合成 超细晶体 多金属氧酸盐化合物 |
| 基金项目: |
| Abstract: The rodlike ultrafine polyoxometalate crystallite, Sr3P2Mo18O62·nH2O, was synthesized via a facile hydrothermal process at a temperature of 80～130 ℃ for 8～12 h in a PEG-600/H2O microemulsion system, using (NH4)6P2Mo18O62·nH2O and SrCl2·6H2O as the raw materials. The structure and morphology of the ultrafine polyoxometalate crystallite were characterized by XRD, SEM, FTIR and ICP-ES. The results show that the ultrafine polyoxometalate crystallite is well crystallized with long rodlike morphology; the diameter and length of the ultrafine polyoxometalate crystallite are 1.0～2.0 μm and 10.0～20.0 μm, respectively. The influence of the three main factors, the volume ratio of PEG-600 to H2O (VPEC-600∶VH2O), the hydrothermal temperature, and the weight ratio of (NH4)6P2Mo18O62·nH2O to SrCl2·6H2O (WPOMs∶WSrCl2·6H2O) was investigated. The results reveal that the morphology, length to diameter ratio and crystallinity of the ultrafine polyoxometalate crystallite are importantly influenced by the VPEC-600∶VH2O value, and the ranges of VPEC-600∶VH2O=(1.50～2.00)∶1.00 are propitious to synthesize the rodlike ultrafine polyoxometalate crystallite with large length to diameter ratio. The suitable hydrothermal temperature is in the range of 80～130 ℃, the reaction does not occur when the temperature is lower than 80 ℃, whereas there will be occurring a red-ox reaction between the polyoxometalates and PEG-600 when the temperature is higher than 130 ℃. The WPOMs∶WSrCl2·6H2O value almost has no influence on the formation of the rodlike ultrafine polyoxometalate crystallite. The possible crystal growth mechanism is proposed. |
| Keywords: microemulsion system hydrothermal synthesis ultrafine crystallite polyoxometalates |
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| 杨发达,李荣先,张渊明,钟立峰,范涛,杨建.水热法合成多金属氧酸盐棒状超细晶体[J].无机化学学报,2007,23(4):569-576. |
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