(武汉理工大学 材料复合新技术国家重点实验室, 武汉 430070)
摘 要: 采用自蔓延高温合成(Self-propagating high-temperature synthesis, SHS)技术和热压烧结(Hot pressing, HP)方法分别研究了Zr-B2O3-Mg和ZrO2-B4C-C体系反应原料的粒度和配比以及烧结温度对产物的影响规律, 并烧结得到ZrB2陶瓷。 采用X射线衍射和化学分析方法分析了材料的相组成, 利用SEM和TEM观察了显微结构; 并用阿基米德排水法测定了相对密度。 结果表明: 在Zr-B2O3-Mg体系中, 50 μm Zr粉和Mg过量15%(摩尔分数)的体系是最理想的SHS反应体系; SHS产物粒径、 酸洗产物粒径和烧结体粒径分别为2~5 μm、 0.5~2.0 μm和2~10 μm; 酸洗产物组成为94.59%ZrB2、 3.87%ZrO2和1.54%H3BO3(质量分数); 烧结体为单相ZrB2陶瓷, 相对密度为95.4%。 在ZrO2-B4C-C体系中, B4C过量15%和C过量10%(摩尔分数)的体系是最理想的反应体系; 烧结体相对密度为94%; 烧结体组成为95.44%ZrB2、 3.87%ZrO2、 0.32%B4C和0.37%C(质量分数)。
关键字: 二硼化锆; 自蔓延高温合成; 热压烧结
( State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China)
Abstract: ZrB2 ceramics were prepared by self-propagating high-temperature synthesis (SHS) and hot pressing (HP). The effects of granularities and dosages of raw materials in Zr-B2O3-Mg system on SHS process and product, as well as sintering temperature in ZrO2-B4C-C system on sintered product, were investigated. The phase constituent was analyzed by X-ray diffraction and chemical analysis. The microstructure of samples was observed by SEM and TEM. The density was measured based on Archimedes drainage method. The results indicate that, in Zr-B2O3-Mg system, the ideal SHS reactants are 50 μm Zr powder and 15% (molar fraction) excessive Mg powder; the particle sizes of SHS product, acid-leached product and sintered product are 2-5 μm, 0.5-2 μm and 2-10 μm respectively; the acid-leached product consists of 94.59%ZrB2, 3.87%ZrO2 and 1.54%H3BO3 (mass fraction); and the relative density of sintered product is 95.4%. In ZrO2-B4C-C system, the reaction system of excessive 15%B4C and excessive 10%C (molar fraction) are the best; for the sintered product, the relative density is 94%; and it is a mixture of 95.44%ZrB2, 3.87%ZrO2, 0.32%B4C and 0.37%C (mass fraction).
Key words: zirconium diboride ; self-propagating high-temperature synthesis; hot pressing