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熔盐碳热/镁热还原低温合成ZrB2-SiC复合粉体
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武汉科技大学省部共建耐火材料与冶金国家重点实验室,,武汉科技大学省部共建耐火材料与冶金国家重点实验室

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国家自然科学基金资助(项目号51502211, 51272188, 51472184),湖北省自然科学基金青年项目(2014CFB800),湖北省自然科学基金重点项目(项目号2013CFA086),湖北省科技支撑计划对外科技合作项目(项目号2013BHE002),第59批中国博士后科学基金面上资助(2016M590721)


Low Temperature Preparation of ZrB2-SiC Composite Powders by a Combined Molten Salt and Carbothermal/magnesium Reduction Method
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The State Key Laboratory of Refractories and Metallurgy,,The State Key Laboratory of Refractories and Metallurgy

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    摘要:

    以氧化锆、氧化硅、氧化硼及活性炭粉为起始原料,以镁粉为还原剂,以NaCl-KCl为熔盐介质,采用熔盐碳热/镁热还原的方法合成了ZrB2-SiC复合粉体。采用X射线衍射仪研究了合成粉体的物相组成,并研究了锆/硅摩尔比、氧化硼用量、镁粉用量及炭粉用量等因素对熔盐碳热/镁热合成ZrB2-SiC复合粉体的影响。结果表明:在摩尔比为1:1的NaCl-KCl复合熔盐体系中,固定锆/硅摩尔比为1:1,当B2O3加入量120 mol%、C加入量120 mol %、Mg粉加入量150 mol %时,可以在1 200 ℃反应2 h的条件下合成纯度很高的ZrB2-SiC复合粉体,复合粉体中ZrB2及SiC的含量分别为59 wt%和35 wt%。 FE-SEM结果表明,合成的ZrB2-SiC复合粉体存在团聚现象,其粒径约为0.5 μm。相较于常规的碳热/镁热方法,该方法可以降低ZrB2-SiC复合粉体的合成温度约200 ℃左右。

    Abstract:

    ZrB2-SiC composite powders were prepared in NaCl-KCl flux using zirconium, silica, boron oxide as main raw materials, magnesium powder as reducing agent by a combined molten salt and carbothermal/magnesium reduction method. The phase compositions of the resulted powders were investigated by X-ray diffraction. The influences of molar ratio of Zr/Si, content of activated carbon, silica and boron oxide on the phase composition and contents of the crystalline phase of ZrB2-SiC composite powders were investigated. The results show that high purity ZrB2-SiC composite powders can be synthesized with the molar ratio of n(Zr)/n(Si) is 1 and the amount of activated carbon, silica and boron oxide was respectively 120 mol%, 120 mol% and 150 mol% in NaCl-KCl flux with the molar ratio of n(NaCl)/n(KCl) is 1 at 1 200 ℃ for 2 h, and the amount of ZrB2 and SiC was calculated as 59 wt% and 35 wt% in the prepared powders. FE-SEM results show that there exits aggregation in the final powders with the particle size of about 0.5μm. Compared with the conventional carbothermal/magnesium reduction method, the synthesis temperature of ZrB2-SiC composite powders was reduced about 200 ℃ in the present work.

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李发亮,李文,张海军.熔盐碳热/镁热还原低温合成ZrB2-SiC复合粉体[J].稀有金属材料与工程,2018,47(S1):185~189.[Li Faliang, Li Wen, Zhang Haijun. Low Temperature Preparation of ZrB2-SiC Composite Powders by a Combined Molten Salt and Carbothermal/magnesium Reduction Method[J]. Rare Metal Materials and Engineering,2018,47(S1):185~189.]
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  • 收稿日期:2017-06-18
  • 最后修改日期:2017-06-18
  • 录用日期:2018-01-29
  • 在线发布日期: 2018-10-22
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