以高纯的单质硼粉和石墨粉为原料,采用放电等离子烧结(Spark Plasma Sintering,SPS)技术,得到了一系列不同化学计量比的硼-碳陶瓷材料.用X射线衍射分析了该系列材料的物相组成,用化学分析法确定了材料的化学计量比,用透射电镜观察了材料的显微结构.结果表明:该系列硼-碳陶瓷的相对致密度均大于90%,具有细晶粒结构(晶粒大小在1 μm左右),由作为主相的碳化硼相(B_(13)C_2)与不同含量的石墨相所组成,并且石墨相含量随原料中硼碳比的增加而减小.化学分析结果显示,随原料中硼碳比的增加,烧结体中的硼碳化学计量比逐渐偏离理论曲线,根据此结果可拟合得到控制烧结体中硼碳比的经验曲线.
In this study, boron-carbon ceramics with different stoichiometries (B~xC, x: 3～10) were prepared by spark plasma sintering technique (SPS) from high purity elemental boron and graphite powders. X-ray diffraction (XRD), chemical analysis (CA) and transmission electron microscopy (TEM) were employed to examine the phase, B/C atomic ratio and microstructure of the samples, respectively. The results show that the related density of all the samples reached 90% and the main phases were boron carbide (B_(13)C_2) with different amounts of free carbon. With increasing molar ratio of boron to carbon, the amount of free carbon decreased and the discrepancy in theoretical and tested stoichiometry was observed. The boron-carbon ceramics with different stoichiometries showed a fine structure with grain size about 1μm.
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