石墨基体上ZrC/MoSi<sub>2</sub>微叠层涂层的制备及抗超高温氧化性能

doi:10.11902/1005.4537.2016.128

中国腐蚀与防护学报

2016, Vol. 36

Issue (5): 476-482 DOI: 10.11902/1005.4537.2016.128

本期目录 | 过刊浏览

石墨基体上ZrC/MoSi₂微叠层涂层的制备及抗超高温氧化性能

杨甜甜^1,²,徐敬军¹(

),钱余海¹,李美栓¹

1. 中国科学院金属研究所沈阳材料科学国家 (联合) 实验室沈阳 110016
2. 中国科学院大学北京 100039

Preparation and Ultra-high Temperature Oxidation Resistance of Micro-laminated ZrC/MoSi₂ Coating on Siliconized Graphite

Tiantian YANG^1,²,Jingjun XU¹(

),Yuhai QIAN¹,Meishuan LI¹

1. Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2. University of Chinese Academy of Sciences, Beijing 100039, China

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摘要:

采用粉末包埋渗和磁控溅射的方法在石墨基体上制备了以SiC作为过渡层的ZrC/MoSi₂微叠层涂层,并用XRD和SEM对涂层的相组成和显微结构进行了分析,同时用感应加热超高温实验系统测试了涂层在1600 ℃以上空气中的抗氧化性能。结果表明：磁控溅射所制备的ZrC/MoSi₂微叠层涂层较为致密;涂层在1800 ℃的空气中具有较好的抗氧化能力,氧化15 min后单位面积氧化失重率为0.3×10^-2 g/cm²,仅为石墨的2.9%。氧化后生成具有层状结构的SiO₂和m-ZrO₂,熔融态SiO₂可愈合ZrO₂层内的空洞和微裂纹,有效地阻挡氧向内扩散。氧化层由ZrO₂和SiO₂组成,氧化产物呈层状结构且各层较为致密。

关键词 ：超高温氧化, 微叠层涂层, 渗硅, 磁控溅射

Abstract：

To improve the ultra-high temperature oxidation resistance of graphite-based materials, a SiC transition layer of about 150 μm in thickness was prepared on graphite substrate by siliconizing method, and then a micro-laminated ZrC/MoSi₂ coating of 22.5 μm in total thickness (corresponding five modulation cycles) was deposited on siliconized graphite by DC magnetron sputtering. The crystallographic structure and morphology of the ZrC/MoSi₂-SiC composite coating before and after ultra-high temperature oxidation were examined by X-ray diffraction (XRD), scanning electron microscope (SEM) with energy dispersion spectroscope (EDS). An ultra-high temperature oxidation testing apparatus based on induction heating was used to test the isothermal oxidation rate of the coating. After oxidation at 1800 ℃ in air for 15 min, the weight loss of the micro-laminated coating was 0.3×10^-2 g/cm², only 2.9% of that of the bare graphite. The oxide scale exhibited layered structure, composed alternatively of ZrO₂ grains and molten SiO₂. The existence of the molten SiO₂ could seal the pores and micro-cracks in the ZrO₂ layer. As a result, the oxide scale had ow oxygen permeability.

Key words： ultra-high temperature oxidation micro-laminated coating siliconizing magnetronsputtering

基金资助:国家自然科学基金项目 (51401209和51571203) 及国家重大科学仪器专项项目 (2011YQ14014504) 资助

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引用本文:

杨甜甜,徐敬军,钱余海,李美栓. 石墨基体上ZrC/MoSi₂微叠层涂层的制备及抗超高温氧化性能[J]. 中国腐蚀与防护学报, 2016, 36(5): 476-482.
Tiantian YANG, Jingjun XU, Yuhai QIAN, Meishuan LI. Preparation and Ultra-high Temperature Oxidation Resistance of Micro-laminated ZrC/MoSi₂ Coating on Siliconized Graphite. Journal of Chinese Society for Corrosion and protection, 2016, 36(5): 476-482.

链接本文:

https://www.jcscp.org/CN/10.11902/1005.4537.2016.128 或 https://www.jcscp.org/CN/Y2016/V36/I5/476

图1 ZrC/MoSi2微叠层涂层结构示意图

图2 感应加热超高温氧化实验系统中真空室内样品加热示意图

图3 石墨粉末包埋渗硅后的表面和截面形貌

图4 磁控溅射制备的ZrC/MoSi2微叠层涂层的XRD谱

图5 磁控溅射制备的ZrC/MoSi2微叠层涂层表面形貌

图6 磁控溅射制备的ZrC/MoSi2微叠层涂层的断面形貌和EDS线扫描结果

图7 ZrC/MoSi2微叠层涂层在1800 ℃空气中氧化15 min后的XRD谱

图8 ZrC/MoSi2微叠层涂层在1800 ℃空气中氧化5和15 min后的表面微观形貌

图9 ZrC/MoSi2微叠层涂层在1800 ℃空气中氧化15 min后的断面形貌

表1 ZrC和MoSi2与O2完全反应后的PBR值

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