残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响

doi:10.15541/jim20150579

无机材料学报 ›› 2016, Vol. 31 ›› Issue (6): 661-666.DOI: 10.15541/jim20150579

残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响

刘泽华^{1, 2}, 齐倩², 闫永杰², 张辉², 刘学建², 罗宏杰¹, 黄政仁²

(1. 上海大学材料科学与工程学院, 上海 200444; 2. 中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海200050)

收稿日期:2015-11-24 出版日期:2016-06-20 网络出版日期:2016-05-19
作者简介:刘泽华. E-mail: liuzehualxtx@126.com

Effect of Residual Phase and Grain Size on Corrosion Resistance of SiC Ceramics in Mixed HF-HNO₃ Acid Solution

LIU Ze-Hua^{1, 2}, QI Qian², YAN Yong-Jie², ZHANG Hui², LIU Xue-Jian², LUO Hong-Jie¹, HUANG Zheng-Ren²

(1. School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China; 2. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China)

Received:2015-11-24 Published:2016-06-20 Online:2016-05-19
About author:LIU Ze-Hua(1989–), male, candidate of master degree. E-mail: liuzehualxtx@126.com
Supported by:
National Natural Science Foundation of China (51202270);Strategic Pilot of Science and Technology of Chinese Academy of Sciences (Class A: XDA02040206)

摘要/Abstract

摘要：

本工作主要研究了残余相和晶粒尺寸对碳化硅的抗混酸(HF-HNO₃)腐蚀特性。通过不同的烧结方法(固相烧结、液相烧结、反应烧结)制备出残余相不同的碳化硅材料。结果表明: 与液相烧结碳化硅(LPS SiC)和反应烧结碳化硅(RB SiC)相比, 固相烧结碳化硅(SSiC)具有更好的腐蚀抗性, 这是由于残余相石墨的抗腐蚀性强, 以及残余相在材料中形成不能相互联通的岛状结构。通过调节碳化硅的烧结温度, 可以影响材料中的晶粒尺寸, 研究结果发现相同烧结温度下随着残余相含量的增加, 材料腐蚀失重线性增加, 对曲线进行线性拟合, 其Y轴截距的绝对值代表不含碳的试样在该烧结温度下的腐蚀失重。研究表明随着烧结温度由2100℃升高到2160℃, 晶粒尺寸由2 μm增加到6 μm。此时其Y轴截距的绝对值分别为9.22(2100℃), 5.81(2130℃), 0.29(2160℃), 表明晶粒尺寸的增加有利于提高材料的抗腐蚀能力。

关键词: 碳化硅, 抗腐蚀, 残余相, 晶粒尺寸

Abstract:

Effect of residual phase and grain size the corrosion resistance of SiC ceramics in mixed HF-HNO₃ acid solution was investigated. Three kinds of fabrication methods (SSiC-solid state sintered SiC, LPS SiC-liquid phase sintered SiC and RB SiC-reaction bonded SiC) were adopted to prepare SiC ceramics. Besides, the grain size in SiC ceramics was adjusted under different sinter temperatures. Compared to RB SiC and LPS SiC ceramics, SSiC ceramics showed a better corrosion resistance for the good corrosion resistance of residual graphite and ‘island’ structure of residual phase in ceramics. The grain size of SiC ceramics sintered at temperature between 2100℃ and 2160℃ increase from 2 μm to 6 μm, and the absolute values of Y intercept, which reflect the corrosion of SSiC ceramics with none residual phase, are 9.22 μg/cm² (2100℃), 5.81 μg/cm² (2130℃) and 0.29 μg/cm² (2160℃), which demonstrate that large grain size is beneficial to the corrosion resistance of SiC ceramics.

Key words: SiC, corrosion resistance, residual phase, grain size

中图分类号:

TQ174

刘泽华, 齐倩, 闫永杰, 张辉, 刘学建, 罗宏杰, 黄政仁. 残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响[J]. 无机材料学报, 2016, 31(6): 661-666.

LIU Ze-Hua, QI Qian, YAN Yong-Jie, ZHANG Hui, LIU Xue-Jian, LUO Hong-Jie, HUANG Zheng-Ren. Effect of Residual Phase and Grain Size on Corrosion Resistance of SiC Ceramics in Mixed HF-HNO₃ Acid Solution[J]. Journal of Inorganic Materials, 2016, 31(6): 661-666.

图/表 6

Table 1 Characteristics of the Samples

Specimen	Composition / wt%					Density/(g·cm^-3)	Relative density/%
Specimen	Si	Al₂O₃	Y₂O₃	C	B₄C	Density/(g·cm^-3)	Relative density/%
RB SiC	15.02	—	—	—	—	3.05	99.47
LPS SiC	—	3.01	3.99	—	—	3.29	99.32
SSiC	—	—	—	5	0.6	3.18	98.75

Fig. 1 The relative density of SSiC ceramics with different contents of C sintered at different temperatures. (a) 5wt% C; (b) 6wt%C; (c) 7wt% C; (d) 8wt% C

Fig. 2 The mass loss of different type SSiC ceramics (a), XRD patterns (b-d) of different SiC ceramics before and after corrosion. RB SiC (b), LPS SiC (c) and SSiC with 8wt% C (d)

Fig. 3 Mass loss versus the content of residual phase (a) and cross-sectional micrograph of corroded SSiC with 5wt% C sintered at 2130℃ (b)

Fig. 4 SEM micrographs of the surface for different SiC ceramics. Before corrosion: (a) RB SiC; (b) LPS SiC; (c) SSiC. After corrosion: (d) RB SiC; (e) LPS SiC; (f) SSiC

Fig. 5 Mass loss of SSiC with different contents of C versus sintering temperatures (a): A 5wt%C, B 6wt %C, C 7wt %C and D 8wt%C. The mass loss versus the content of residual phase of SSiC sintered at different temperatures: (b) 2100℃; (c) 2160℃. SEM micrographs of surface for different corroded specimens with 5wt% C sintered at different temperatures: (d) 2100℃; (e) 2130℃; (f) 2160℃

参考文献 14

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残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响

Effect of Residual Phase and Grain Size on Corrosion Resistance of SiC Ceramics in Mixed HF-HNO₃ Acid Solution

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残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响

Effect of Residual Phase and Grain Size on Corrosion Resistance of SiC Ceramics in Mixed HF-HNO3 Acid Solution

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Effect of Residual Phase and Grain Size on Corrosion Resistance of SiC Ceramics in Mixed HF-HNO₃ Acid Solution