锂离子导电微晶玻璃晶相与残余玻璃相定量分析∗

摘要

In this paper,fabrication and characterization of sheet specimens based on the Li2 O-Al2 O 3 -GeO 2 -P2 O 5 glass ceramics system are reported.Based on Rietveld method of X-ray techniques,volume additivity rule, ICP and SEM-EDS,a new method was developed to quantitatively analyze the crystal phase composition and ox-ide composition of residual in glass ceramics after crystallized at different temperature.As a result,the major phase of the glass ceramics was found to be LiGe2 (PO 4 )3 ,with GeO 2 and AlPO 4 as the impurity phases.More ever,quantitative analysis of crystal phases and the residual glass phase in the glass ceramics can be achieved using the rietveld method.This quantitative analysis method can be widely used in other glass ceramics due to its accuracy and feasibility.%以 Li2 O-Al2 O 3-GeO 2-P2 O 5锂离子导电微晶玻璃为研究对象,通过 XRD、SEM-EDS、ICP 和 Ri-etveld 结构精修等测试分析方法,对微晶玻璃样品的微观结构形貌进行了表征,对不同晶化制度条件下制得的微晶玻璃样品物相组成、各晶相含量和残余玻璃相内部各种氧化物的摩尔比进行了定性和定量分析。结果表明,经600~950℃晶化处理的微晶玻璃主晶相均为 LiGe2(PO 4)3,杂质相为 GeO 2和 AlPO 4,各晶相含量和残余玻璃相成分可以精确定量化,这种定量分析方法准确可行,在微晶玻璃的定量分析中具有重要推广作用。