CVD沉积工艺对SiC涂层结晶度与耐腐蚀性能的影响

doi:10.19936/j.cnki.2096-8000.20210328.011

复合材料科学与工程 ›› 2021, Vol. 0 ›› Issue (3): 71-77.DOI: 10.19936/j.cnki.2096-8000.20210328.011

CVD沉积工艺对SiC涂层结晶度与耐腐蚀性能的影响

刘桂良¹, 何宗倍¹, 王梓璇², 张瑞谦¹, 王继平^2*

1.中国核动力研究设计院反应堆燃料及材料重点实验室,成都610213;
2.西安交通大学材料科学与工程学院金属材料强度国家重点实验室,西安710049

收稿日期:2020-11-20 出版日期:2021-03-28 发布日期:2021-04-30
通讯作者: 王继平(1978-),男,博士,副教授,研究方向为复合材料和先进陶瓷材料,jpwang@xjtu.edu.cn。
作者简介:刘桂良(1982-),男,硕士,副研究员,研究方向为核材料。
基金资助:
国家自然科学基金(52001299)

EFFECT OF CVD DEPOSITION PROCESS ON CRYSTALLINITY AND CORROSION RESISTANCE OF SiC COATINGS

LIU Gui-liang¹, HE Zong-bei¹, WANG Zi-xuan², ZHANG Rui-qian¹, WANG Ji-ping^2*

1. Science and Technology on Reactor Fuel and Materials Laboratory, Nuclear Power Institute of China, Chengdu 610213, China;
2. State Key Laboratory for Mechanical Behavior of Materials, School of Materials Science and Engineering, Xi'an Jiaotong University, Xi'an 710049, China

Received:2020-11-20 Online:2021-03-28 Published:2021-04-30

摘要/Abstract

摘要： 通过化学气相沉积(CVD)SiC涂层来提高SiC_f/SiC复合材料的耐腐蚀性能,本文以CH₃SiCl₃(MTS)为源气体,在反应烧结SiC基体上制备SiC涂层,控制沉积温度、炉压及H₂/MTS摩尔比等工艺参数,通过X射线衍射实验(XRD)得到不同工艺条件下生成的碳化硅涂层的物相组成和结晶度,通过高温水腐蚀实验检测涂层的耐腐蚀性,并利用扫描电子显微镜(SEM)观察腐蚀前后的表面形貌。结果表明:当沉积时间为8 h,沉积温度从1050 ℃到1250 ℃,β-SiC涂层表面平整性提高,沉积厚度由12.97 μm急剧增加至71.10 μm,SiC晶粒尺寸逐渐增大,最终呈金字塔状;碳化硅涂层腐蚀60 d后,表面呈现针状结构,1250 ℃下沉积的SiC涂层耐腐蚀性能较好;β-SiC涂层的晶粒尺寸随沉积炉压的增大而增大,结晶度随沉积炉压增大而减小,在200 Pa以下,获得的β-SiC晶粒的结晶度最高(81.08%)、晶粒尺寸最小(13.7 nm);随着H₂/MTS摩尔比增加,β-SiC晶粒结晶度迅速下降,当H₂/MTS=6.5时,结晶度最高(95.91%)。

关键词: SiC_f/SiC, 复合材料, 耐腐蚀性, SiC涂层, 化学气相沉积, 结晶度

Abstract: The corrosion resistance of SiC_f/SiC composites was improved by chemical vapor deposition (CVD) SiC coatings. In this paper, SiC coatings are prepared on reaction sintering SiC matrix with CH₃SiCl₃ (MTS) as the source gas. Surface morphology and corrosion resistance of silicon carbide coatings were related with parameters in CVD such as deposition temperature, furnace pressure and mole ratio of H₂ and MTS. The phase composition and crystallinity of silicon carbide coating under different process conditions were obtained by X-ray diffraction experiment (XRD). The corrosion resistance of the coating was detected by high-temperature water corrosion experiment, and the surface morphology before and after the corrosion was observed by scanning electron microscope (SEM). The results showed that when the deposition time was 8 hours and the deposition temperature was from 1050 ℃ to 1250 ℃, the surface roughness of SiC coating was improved, the deposition thickness increased sharply from 12.97 μm to 71.10 μm, and the grain size of SiC gradually increased and finally presented a pyramid shape. After 60 days of corrosion of silicon carbide coating, the surface presents an acicular structure. The SiC coating deposited at 1250 ℃ had better corrosion resistance. With the increase of deposition furnace pressure, the crystallinity of β-SiC grains decreased sharply and the grain size increased sharply. The crystallinity of β-SiC was the highest (81.08%) and the grain size was smallest (13.7 nm) under 200 Pa. The crystallinity of β-SiC grain decreased sharply with the increase of the molar ratio of H₂ and MTS. When the molar ratio of H₂ and MTS was 6.5, the crystallinity reached its highest point (95.91%).

Key words: SiC_f/SiC, composites, corrosion resistance, SiC coating, chemical vapor deposition, crystallinity

中图分类号:

TB332

刘桂良, 何宗倍, 王梓璇, 张瑞谦, 王继平. CVD沉积工艺对SiC涂层结晶度与耐腐蚀性能的影响[J]. 复合材料科学与工程, 2021, 0(3): 71-77.

LIU Gui-liang, HE Zong-bei, WANG Zi-xuan, ZHANG Rui-qian, WANG Ji-ping. EFFECT OF CVD DEPOSITION PROCESS ON CRYSTALLINITY AND CORROSION RESISTANCE OF SiC COATINGS[J]. COMPOSITES SCIENCE AND ENGINEERING, 2021, 0(3): 71-77.

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CVD沉积工艺对SiC涂层结晶度与耐腐蚀性能的影响

EFFECT OF CVD DEPOSITION PROCESS ON CRYSTALLINITY AND CORROSION RESISTANCE OF SiC COATINGS

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