高温氮气下镁碳耐火材料的物相重构与微结构演变

doi:10.3969/j.issn.1001-1935.2022.02.001

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

• 研究开发 • 下一篇

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)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

收稿日期:2021-05-12 出版日期:2022-04-15 发布日期:2022-04-21
通讯作者: 刘开琪,男,1969年生,博士,研究员。E-mail: kqliu@ipe.ac.cn
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)

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)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

摘要/Abstract

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(Mg₃Al_nN_n₊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Mg₃Al_nN_n₊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

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 (Mg₃Al_nN_n₊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 Mg₃Al_nN_n₊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

中图分类号:

TQ175

闫明伟, 杨裕民, 仝尚好, 张佳钰, 孙广超, 刘开琪. 高温氮气下镁碳耐火材料的物相重构与微结构演变[J]. 耐火材料, 2022, 56(2): 93-100.

Yan Mingwei, Yang Yumin, Tong Shanghao, Zhang Jiayu, Sun Guangchao, Liu Kaiqi. Phase reconstruction and microstructure evolution of magnesia-carbon refractories at high temperatures in nitrogen[J]. Refractories, 2022, 56(2): 93-100.

图/表 6

图1 1 300~1 600 ℃氮气条件下热处理后试样的XRD图谱

Fig.1 XRD patterns of samples treated at 1 300-1 600 ℃ in nitrogen

图2 试样S1300中晶须的SEM照片和EDS图谱

Fig.2 SEM images and EDS spectrum of MgO whiskers in sample S1300

图3 试样S1300的SEM照片

Fig.3 SEM images of heat-treated sample S1300

图4 Mg3AlnNn+2的SEM照片及其面扫描

Fig.4 SEM-mapping image of Mg3AlnNn+2

图5 热处理后试样S1400和S1500的SEM照片

Fig.5 SEM images of samples S1400 and S1500 after heat treatment

图6 试样S1600的SEM照片

Fig.6 SEM images of heat-treated sample S1600

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高温氮气下镁碳耐火材料的物相重构与微结构演变

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

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