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合成六方镁钴堇青石固溶体(Mg(2 - 2x)Co(2x)Al4Si5O18)的晶体结构和微观结构

Crystal structure and microstructure of synthetic hexagonal magnesium-cobalt cordierite solid solutions (Mg(2-2x)Co(2x)Al4Si5O18).

作者信息

Serrano Francisco Javier, Montoya Noemí, Pizarro José Luis, Reventós María Mercedes, Kojdecki Marek Andrzej, Amigó José María, Alarcón Javier

机构信息

Department of Geology, University of Valencia, 46100 Burjasot, Spain.

出版信息

Acta Crystallogr B Struct Sci Cryst Eng Mater. 2013 Apr;69(Pt 2):110-21. doi: 10.1107/S2052519213001401. Epub 2013 Feb 26.

Abstract

Co(2+)-containing cordierite glasses, of nominal compositions (Mg(1-x)Co(x))2Al4Si5O18 (with x = 0, 0.2, 0.4, 0.6, 0.8 and 1), were prepared by melting colloidal gel precursors. After isothermal heating at 1273 K for around 28 h, a single-phase α-cordierite (high-temperature hexagonal polymorph) was synthesized. All materials were investigated using X-ray powder diffraction and field-emission scanning electron microscopy. The crystal structure and microstructure were determined from X-ray diffraction patterns. Rietveld refinement confirmed the formation of magnesium-cobalt cordierite solid solutions. The unit-cell volume increased with the increase of cobalt content in the starting glass. The crystalline microstructure of the cordierites was interpreted using a mathematical model of a polycrystalline material and characterized by prevalent crystallite shape, volume-weighted crystallite size distribution and second-order crystalline lattice-strain distribution. Hexagonal prismatic was the prevalent shape of α-cordierite crystallites. Bimodality in the size distribution was observed and interpreted as a consequence of two paths of the crystallization: the nucleation from glass of μ-cordierite, which transformed into α-cordierite with annealing, or the nucleation of α-cordierite directly from glass at high temperatures. Scanning electron microscopy images agreed well with crystalline microstructure characteristics determined from the X-ray diffraction line-profile analysis.

摘要

通过熔融胶体凝胶前驱体制备了标称组成为(Mg(1 - x)Co(x))2Al4Si5O18(x = 0、0.2、0.4、0.6、0.8和1)的含Co(2+)堇青石玻璃。在1273 K等温加热约28 h后,合成了单相α-堇青石(高温六方多晶型物)。使用X射线粉末衍射和场发射扫描电子显微镜对所有材料进行了研究。根据X射线衍射图谱确定了晶体结构和微观结构。Rietveld精修证实了镁-钴堇青石固溶体的形成。晶胞体积随着起始玻璃中钴含量的增加而增大。使用多晶材料的数学模型解释了堇青石的晶体微观结构,并通过普遍的微晶形状、体积加权微晶尺寸分布和二阶晶格应变分布进行了表征。六方棱柱是α-堇青石微晶的普遍形状。观察到尺寸分布的双峰性,并将其解释为两种结晶途径的结果:μ-堇青石从玻璃中形核,退火后转变为α-堇青石,或α-堇青石在高温下直接从玻璃中形核。扫描电子显微镜图像与通过X射线衍射线轮廓分析确定的晶体微观结构特征吻合良好。

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