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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >In-situ energy dispersive X-ray diffraction studies of the crystallization of (1,2-DAPH(2))(2)Ge-9(OH)(4)O-18 center dot 2 H2O under solvothermal conditions
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In-situ energy dispersive X-ray diffraction studies of the crystallization of (1,2-DAPH(2))(2)Ge-9(OH)(4)O-18 center dot 2 H2O under solvothermal conditions

机译:溶剂热条件下(1,2-DAPH(2))(2)Ge-9(OH)(4)O-18中心点2 H2O结晶的原位能量色散X射线衍射研究

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摘要

The solvothermal synthesis of the three-dimensional germanate (1,2-DAPH(2))(2)Ge-9(OH)(4)O-18 (.) 2 H2O has been studied with the in-situ energy dispersive X-ray powder diffraction technique (EDXRD). The temperature dependence of the extent of reaction (alpha) has been investigated at 160 degreesC, 170 degreesC and 175 degreesC. In this temperature region no crystalline precursors or intermediates could be detected. The crystallization proceeds in more than one step suggesting a change of the kinetics during the formation of the crystalline material. The evaluated reaction exponents for the different steps are in good agreement with different Avrami nucleation models. The shape of the crystals was investigated with scanning electron microscopy after quenching the products after different reaction times. In agreement with the different nucleation models significant changes of the crystal sizes and shapes were observed. For the investigation of the effect onto the crystal growth of the compound seed crystals were added to the starting material. Again, the results indicate that over the temperature range the crystallization can be modeled by nucleation-controlled processes with two or three dimensional growth of the crystals.
机译:用原位能量色散X研究了三维锗酸盐(1,2-DAPH(2))(2)Ge-9(OH)(4)O-18(。)2 H2O的溶剂热合成射线粉末衍射技术(EDXRD)。已经在160℃,170℃和175℃下研究了反应程度α的温度依赖性。在此温度范围内,未检测到结晶前体或中间体。结晶进行了一个以上的步骤,表明在结晶材料形成过程中动力学发生了变化。评估的不同步骤的反应指数与不同的Avrami成核模型非常吻合。在不同的反应时间后将产物淬灭后,通过扫描电子显微镜研究晶体的形状。与不同的成核模型一致,观察到晶体尺寸和形状的显着变化。为了研究对化合物的晶体生长的影响,将晶种添加到起始材料中。再次,该结果表明,在该温度范围内,可以通过具有二维或三维晶体生长的成核控制过程来模拟结晶。

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