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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Synthesis and Crystal Structures of a Stable, a Metastable and a High Temperature Modification of Pb2NaIO6
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Synthesis and Crystal Structures of a Stable, a Metastable and a High Temperature Modification of Pb2NaIO6

机译：稳定，亚稳和高温修饰的Pb2NaIO6的合成和晶体结构

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摘要

In analogy to the synthesis of polycrystalline M2NaIO6 (M = Ca, Sr, Ba) by precipitation in water at 90 degrees C, the title compound was first prepared as a metastable compound. The stable modification of Pb2NaIO6 was obtained by a heat treatment to 400 degrees C followed by cooling to room temperature. The crystal structure was refined from powder diffraction data [space group P2(1)/c (14), a = 5.9040(2), b = 5.7526(2), c = 10.1104(3)angstrom, beta = 125.341(1)degrees]. On heating, at ca. 125 degrees C, a phase transition to a cubic high temperature modification was observed. The crystal structure was refined from XRD data measured at 200 degrees C [space group Fm (3) over barm (225), a = 8.2678(1) angstrom]. Depending on the precipitation temperature between 90 degrees C and 0 degrees C, several metastable modifications were obtained, which can be distinguished by significantly different lattice parameters. The XRD pattern of a powder precipitated at room temperature is pseudocubic. The crystal structure was refined at room temperature in P2(1)/c with a = 5.8201(4), b = 5.8473(4), c = 10.0798(5)angstrom, beta = 125.074(3)degrees. This modification behaves almost as a cubic lattice on heating as found from XRD and DSC measurements.
机译：与通过在90°C的水中沉淀合成多晶M2NaIO6（M = Ca，Sr，Ba）相似，首先将标题化合物制备为亚稳化合物。通过热处理至400摄氏度，然后冷却至室温，可获得Pb2NaIO6的稳定修饰。根据粉末衍射数据[空间群P2（1）/ c（14），a = 5.9040（2），b = 5.7526（2），c = 10.1104（3）埃，β= 125.341（1）细化晶体结构。度]。加热时，约在125℃下，观察到向立方高温改性的相变。从在200摄氏度[巴姆（225）上的空间群Fm（3），a = 8.2678（1）埃]下测量的XRD数据中提炼晶体结构。根据在90摄氏度和0摄氏度之间的沉淀温度，获得了几种亚稳态修饰，可以通过明显不同的晶格参数来区分它们。在室温下沉淀的粉末的XRD图谱是假立方的。在室温下以a = 5.8201（4），b = 5.8473（4），c = 10.0798（5）埃，β= 125.074（3）度在室温下以P2（1）/ c精炼晶体结构。根据XRD和DSC测量，这种修改几乎表现为加热时的立方晶格。

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