大气等离子喷涂MoSi2-30Al2O3电热涂层的组织结构及性能

doi:10.15541/jim20180394

无机材料学报 ›› 2019, Vol. 34 ›› Issue (6): 646-652.DOI: 10.15541/jim20180394

大气等离子喷涂MoSi₂-30Al₂O₃电热涂层的组织结构及性能

周炎哲^1,²,刘敏²(),杨焜²,曾威²,宋进兵²,邓春明²,邓畅光²

^1. 中南大学材料科学与工程学院, 长沙 410083
^2. 广东省新材料研究所, 现代材料表面工程技术国家工程实验室, 广东省现代表面工程技术重点实验室, 广州 510650

收稿日期:2018-09-03 修回日期:2018-10-31 出版日期:2019-06-20 网络出版日期:2019-05-23
作者简介:周炎哲(1993-), 男, 硕士研究生. E-mail:807537144@qq.com
基金资助:
广州市珠江科技新星专项(201710010130);广东省科学院实施创新驱动发展能力建设专项(2017GDASCX-0111);广东省科技厅省属科研机构改革创新稳定项目(2017A070701027);广东省科技项目(2014B070705007)

Microstructure and Property of MoSi₂-30Al₂O₃ Electrothermal Coating Prepared by Atmospheric Plasma Spraying

Yan-Zhe ZHOU^1,²,Min LIU²(),Kun YANG²,Wei ZENG²,Jin-Bing SONG²,Chun-Ming DENG²,Chang-Guang DENG²

^1. School of Materials Science and Engineering, Central South University, Changsha 410083, China
^2. The Key Lab of Guangdong for Modern Surface Engineering Technology, National Engineering Laboratory for Modern Materials Surface Engineering Technology, Guangdong Institute of New Materials, Guangzhou 510650, China

Received:2018-09-03 Revised:2018-10-31 Published:2019-06-20 Online:2019-05-23
Supported by:
Pearl River S&T Nova Program of Guangzhou(201710010130);GDAS’ Project of Science and Technology Development(2017GDASCX-0111);Science and Technology Planning Project of Guangdong Province, China(2017A070701027);Science and Technology Program of Guangzhou(2014B070705007)

摘要/Abstract

摘要：

以MoSi₂-30Al₂O₃混合粉末为原料, 利用大气等离子喷涂技术制备MoSi₂-Al₂O₃体系电热涂层。采用XRD、SEM、通电测试、热重-差热分析等对涂层的相组成、组织形貌和热稳定性进行表征。结果表明：MoSi₂-30Al₂O₃电热涂层体系组织均匀致密, 添加Al₂O₃能改善MoSi₂的电阻率及低温抗氧化性; MoSi₂-30Al₂O₃涂层电热性能优异, 在循环加热测试中, 能稳定地加热到320 ℃并长时间保温, 辊面温度分布均匀, 中部温差控制在25 ℃之内; 循环加热过程中的氧化及热应力的弛豫会导致涂层产生裂纹及孔隙进而导致涂层电阻率升高。

关键词: 电热材料, MoSi₂-Al₂O₃复合涂层, 等离子喷涂, 电热性能

Abstract:

With MoSi₂-30Al₂O₃mixed powders as the raw material, MoSi₂-30Al₂O₃ electrothermal coating was sprayed by atmospheric plasma spraying technology. The phase composition, microstructure and thermal stability of the coating were systematically studied by XRD, SEM, electrical test and differential thermal gravity analysis. The results show that MoSi₂-30Al₂O₃ electrothermal coating shows dense microstructure. Al₂O₃ can improve the electrical resistivity and oxidation resistance of MoSi₂materials in low temperature. The coating exhibits an excellent electrical-heating performance. In the heating cycle test, it could be heated to 320 ℃ stably and exhibit uniform thermal distribution in the surface area. The temperature variation in roll’s central area can be controlled within 25 ℃; Oxidation and thermal stress relaxation during heating cycle would generate cracks and pores in the coating which would increase electrical resistivity.

Key words: electrothermal material, MoSi₂-Al₂O₃composite coating, atmospheric plasma spraying, electrical- heating performance

中图分类号:

TQ174

周炎哲, 刘敏, 杨焜, 曾威, 宋进兵, 邓春明, 邓畅光. 大气等离子喷涂MoSi₂-30Al₂O₃电热涂层的组织结构及性能[J]. 无机材料学报, 2019, 34(6): 646-652.

Yan-Zhe ZHOU, Min LIU, Kun YANG, Wei ZENG, Jin-Bing SONG, Chun-Ming DENG, Chang-Guang DENG. Microstructure and Property of MoSi₂-30Al₂O₃ Electrothermal Coating Prepared by Atmospheric Plasma Spraying[J]. Journal of Inorganic Materials, 2019, 34(6): 646-652.

图/表 13

表1 大气等离子喷涂工艺参数

Table 1 Atmospheric plasma spraying parameters

Sample	Current/A	Voltage/V	Distance/mm	Flux of Ar/(L?min^-1)	Flux of H₂/(L?min^-1)	Powder feed rate/(g?min^-1)
NiAl	600	70	110	45	8	20
MgAl₂O₄	630	75	110	40	11	19
MoSi-Al₂O₃	600	76	110	41	12	24

图1 MoSi2-30Al2O3粉末和涂层的XRD衍射图谱

Fig. 1 XRD patterns of MoSi2-30Al2O3 powder and coating

图2 MoSi2-30Al2O3涂层表面SEM形貌照片

Fig. 2 SEM images of MoSi2-30Al2O3 coating

图3 电热涂层系统(a)和MoSi2-30Al2O3涂层(b, c)的抛光截面SEM形貌与对应点能谱图(1, 2, 3)

Fig. 3 Polished cross-section morphologies of electrothermal coating system (a) and MoSi2-30Al2O3 coating (b, c); EDS analysis of corresponding points (1,2,3)

图4 MoSi2-Al2O3涂层的热重分析曲线

Fig. 4 Thermogravimetric (TG) curves of MoSi2-Al2O3 coating

图5 MoSi2-30Al2O3涂层的热重-差热分析曲线

Fig. 5 Thermogravimetric (TG) and differential scanning calorimeter (DSC) curves for MoSi2-30Al2O3 coating

图6 陶瓷电热辊实物图(a)及保温状态时的红外热图像(b)

Fig. 6 Photograph of ceramic heating roller (a) and infrared thermal image of the heating roller during insulation stage (b)

图7 MoSi2-Al2O3加热辊加热的t-T曲线

Fig. 7 Heating t-T curves of MoSi2-Al2O3 heating roller

图8 MoSi2-30Al2O3加热辊循环加热的t-T曲线

Fig. 8 Cyclic heating t-T curve of MoSi2-30Al2O3 heating roller

图9 涂层电阻率与加热时间的变化关系

Fig. 9 Relationship between resistivity of coating and heating time

图10 涂层电阻率与温度的变化关系

Fig. 10 Relationship between resistivity of coating and temperature

图11 MoSi2-30Al2O3涂层经过5个加热周期后的XRD图谱

Fig. 11 XRD pattern of MoSi2-30Al2O3 coating after 5 heating cycles

图12 加热5个周期后的MoSi2-30Al2O3涂层表面形貌(a)、截面形貌(b)及断面形貌(c)及对应点能谱图(1)

Fig. 12 Surface (a), cross-section (b) and fracture (c) morphologies of MoSi2-30Al2O3 coating after 5 cycles; EDS analysis of corresponding point (1)

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大气等离子喷涂MoSi₂-30Al₂O₃电热涂层的组织结构及性能

Microstructure and Property of MoSi₂-30Al₂O₃ Electrothermal Coating Prepared by Atmospheric Plasma Spraying

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