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Macroscopic and micro-structural aspects of the lithium metaphosphate glass crystallization

机译:偏磷酸锂玻璃结晶的宏观和微观结构

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The LiPO3 glass crytallization have been investigated according to isothermal and non-isothermal approaches by using various techniques such as thermal analysis, helium pycnometry, scanning electronic microcospy and X-ray powder diffraction. Different experimental procedures have been developed to determine the crystallized volume fraction. The different results are a good agreement and leadto a better comprehension at a "macroscopic" scale of this first order transition. In addition, from "ex-situ" X-ray powder diffraction experiments, the understanding of the diffraction line intensities as a function of the annealing time, at a fixed temperature, has revealed a new metastable crystalline form of LiPO3 (named alpha) stable over a short time range. Attempts for indexing led to a possible monoclinic system close to that reported in literature for the thermodynamical stable variety (named beta). The micro-structure of annealed samples has been discussed in terms of crystallite sizes and lattice micro-distorsions at a nanometer scale. This study based on diffraction line broadening analysis was carried out with the integral breadth method. Finally, from "in-situ" X-ray powder diffraction experiments, evidence was shown that the LiPO 3 glass matrix crystallizes first in a metastable LiPO 3-alpha form which, in turn, transforms into the beta form.
机译:通过使用各种技术,例如热分析,氦比重瓶法,扫描电子显微镜和X射线粉末衍射,根据等温和非等温方法研究了LiPO3玻璃的晶化。已经开发了不同的实验程序来确定结晶的体积分数。不同的结果是很好的一致性,并且可以在这种一阶转换的“宏观”规模上获得更好的理解。此外,通过“异位” X射线粉末衍射实验,在固定温度下对衍射线强度与退火时间的函数关系的了解,揭示了一种稳定的新的LiPO3亚稳晶体(称为α)。在短时间内。索引的尝试导致可能的单斜晶系接近热力学稳定品种(称为β)的文献报道。已经根据纳米尺度上的微晶尺寸和晶格微畸变讨论了退火样品的微观结构。基于衍射线加宽分析的这项研究是采用积分宽度法进行的。最后,从“原位” X射线粉末衍射实验中,证据表明LiPO 3玻璃基质首先以亚稳LiPO3-α形式结晶,然后转变为β形式。

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