Serrano Francisco Javier, Montoya Noemí, Pizarro José Luis, Reventós María Mercedes, Kojdecki Marek Andrzej, Amigó José María, Alarcón Javier
Department of Geology, University of Valencia, 46100 Burjasot, Spain.
Acta Crystallogr B Struct Sci Cryst Eng Mater. 2013 Apr;69(Pt 2):110-21. doi: 10.1107/S2052519213001401. Epub 2013 Feb 26.
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.
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。