以ZrB₂-SiC-ZrC复相超高温陶瓷为研究对象, 对X射线衍射的K值法、二次电子像结合背散射电子像、电子背散射衍射结合能谱面扫描三种相组成的定量分析方法进行了比较, 结果显示K值法使用简单、方便; SEM的两种定量方法不仅可以定量分析相组成, 还能反映相分布与相关系。三种定量方法的结果较一致, 均显示该复相陶瓷实际相组成远远偏离反应烧结设计相组成, 其中, ZrO₂杂质相实际含量多于5vol%, ZrC相含量远低于理论值5vol%, K值法显示其含量甚至低于1vol%。相组成的定量分析为进一步开展微结构研究及复合材料设计提供了必要的技术基础。

Three methods were applied and compared to perform quantitative phase analysis of ZrB₂-SiC-ZrC ultra- high temperature ceramic composites: the K value method by powder X-ray diffraction, two SEM methods to combine secondary electron and backscattered electron images, and electron backscatter diffraction and energy dispersive X-ray spectroscope (EDS) mapping. K value method could be applied conveniently and simply, while the two SEM methods could not only be performed quantitative phase analysis but also reveal phase distribution and relationships. Results from the three methods all show significant deviation of phase compositions from the composite designing of reactive sintering, while they are largely consistent with each other. The content of impurity ZrO₂ phase is detected more than 5vol%, and in contrast, the content of secondary ZrC phase is found substantially below the theoretical 5vol% level and even below 1vol% as calculated by the more sensitive K value method. These quantitative phase analysis could provide technical supports to study the true composite microstructure and phase designing.