Refractories ›› 2022, Vol. 56 ›› Issue (2): 93-100.DOI: 10.3969/j.issn.1001-1935.2022.02.001

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Phase reconstruction and microstructure evolution of magnesia-carbon refractories at high temperatures in nitrogen

Yan Mingwei1,2)(), Yang Yumin3), Tong Shanghao4), Zhang Jiayu1), Sun Guangchao1,2), Liu Kaiqi1,2)()   

  1. 1)State Key Laboratory of Multiphase Complex Systems,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China
  • Received:2021-05-12 Online:2022-04-15 Published:2022-04-21
  • Contact: Liu Kaiqi

高温氮气下镁碳耐火材料的物相重构与微结构演变

闫明伟1,2)(), 杨裕民3), 仝尚好4), 张佳钰1), 孙广超1,2), 刘开琪1,2)()   

  1. 1)中国科学院过程工程研究所 多相复杂系统国家重点实验室 北京100190
    2)中科院过程工程研究所 南京绿色制造产业创新研究院 江苏南京 211135
    3)中航天水高新磨具有限公司 甘肃天水 741024
    4)洛阳利尔功能材料有限公司 河南洛阳471039
  • 通讯作者: 刘开琪
  • 作者简介:闫明伟:男,1989年生,博士,助理研究员。E-mail: mwyan@ipe.ac.cn
  • 基金资助:
    国家重点研发计划课题(2019YFC1904304);多相复杂系统国家重点实验室自主研究课题(MPCS-2021-C-01);中科南京绿色制造产业创新研究院资助(E0010717)

Abstract:

Magnesia-carbon refractories were prepared using fused magnesia,flake graphite and metal aluminum powder as starting materials,phenolic resin as the binder,heat-treating at 1 300-1 600 ℃ in a nitrogen atmosphere.The phase reconstruction and the microstructure evolution of the obtained magnesia-carbon refractories were analyzed.The formation mechanisms of magnesia crystals with different morphologies by chemical vapor deposition were revealed.The results show that at 1 300-1 500 ℃,the non-oxides within the samples are aluminum carbide (Al4C3),aluminum nitride (AlN) and magnesium aluminum nitride (Mg3AlnNn+2,n=2 or 3);at 1 600 ℃,the diffraction characteristic peak intensity of Al4C3 and AlN decreases sharply,and sharp diffraction characteristic peaks of nitrogen aluminum carbide (Al7C3N3) appear.Mg(g) is produced by the aluminothermic reduction and carbothermal reduction of magnesia.On the surface of the samples,Mg(g) reacts with oxygen to form MgO whiskers.Inside the samples,Mg(g) and O2(g) undergo a CVD chemical deposition reaction to form cubic MgO crystals.There is a phase relationship between flake AlN and flake Mg3AlnNn+2,and they are so associated with each other that the morphology is difficult to distinguish.

Key words: magnesia-carbon refractories, phase reconstruction, non-oxide, magnesia

摘要:

以电熔镁砂、鳞片石墨和金属铝粉为原料,酚醛树脂为结合剂,在氮气气氛中,经1 300~1 600 ℃热处理后制备了镁碳耐火材料。分析了镁碳耐火材料的物相重构和微结构演变,揭示了化学气相沉积反应形成两种不同形貌氧化镁的机制。结果表明:在1 300~1 500 ℃时,试样的非氧化物组成为碳化铝(Al4C3)、氮化铝(AlN)和镁铝氮化物(Mg3AlnNn+2, n=2或3);在1 600 ℃时,热处理后试样中碳化铝和氮化铝的衍射特征峰值强度急剧降低,出现氮碳化铝(Al7C3N3)的尖锐衍射特征峰。铝热还原MgO和碳热还原MgO产生了Mg(g)。在试样表面,Mg(g)与氧气反应形成MgO晶须;在试样内部,Mg(g)与氧气发生CVD化学沉积反应形成立方MgO晶体。在热处理后试样的微区组织结构中,片状AlN与片状Mg3AlnNn+2存在一定的位相关系,二者伴生存在,形貌难以区分。

关键词: 镁碳耐火材料, 物相重构, 非氧化物, 氧化镁

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