董天下,孟凡桂,陈红梅,张九阳,高超,王宗玉.石墨表面TaC涂层的熔盐法制备及表征[J].表面技术,2023,52(2):297-306.
DONG Tian-xia,MENG Fan-gui,CHEN Hong-mei,ZHANG Jiu-yang,GAO Chao,WANG Zong-yu.Preparation and Characterization of TaC Coating on Graphite via Molten Salt Method[J].Surface Technology,2023,52(2):297-306 |
| 石墨表面TaC涂层的熔盐法制备及表征 |
| Preparation and Characterization of TaC Coating on Graphite via Molten Salt Method |
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| DOI：10.16490/j.cnki.issn.1001-3660.2023.02.028 |
| 中文关键词: 熔盐法 高温热处理 石墨 TaC涂层 耐腐蚀性 |
| 英文关键词:molten salt method high-temperature treatment graphite TaC coating corrosion resistance |
| 基金项目: |
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| Author | Institution |
| DONG Tian-xia | School of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China |
| MENG Fan-gui | School of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China |
| CHEN Hong-mei | Hunan Provincial Key Laboratory of Fine Ceramics and Powder Materials, Hunan University of Humanities, Science and Technology, Hunan Loudi 417000, China;Hunan International Economics University, Changsha 410205, China |
| ZHANG Jiu-yang | SICC Co., Ltd., Jinan 250000, China |
| GAO Chao | SICC Co., Ltd., Jinan 250000, China |
| WANG Zong-yu | SICC Co., Ltd., Jinan 250000, China |
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| 中文摘要: |
| 目的 以K2TaF7和Ta粉为主要原料，在石墨材料表面制备TaC涂层。方法 反应物在1 200 ℃的熔盐体系中保温3 h，反应生成碳化物，经后续2 300 ℃真空保温1 h后，得到TaC涂层材料。采用XRD和SEM对涂层的组成结构进行表征，采用拉开法对涂层的和石墨基体的结合强度进行测量，采用纳米压痕对涂层的硬度和弹性模量进表征，最后对TaC涂层的抗腐蚀性能进行模拟测试评估和实际的SiC长晶测试。结果 熔盐法制备的TaC涂层连续地覆盖在石墨表面，保持了原始石墨的形貌，其物相组成为TaC，呈现出亮黄色，厚度为20~40 μm，涂层的晶粒无择优取向生长，呈现出无序堆积的状态。TaC涂层与石墨基体的结合强度为9.49 MPa，硬度和弹性模量分别为14.42 GPa和123.32 GPa。TaC涂层样品于2 300 ℃的SiC腐蚀气氛环境下保温3 h，质量损失率仅为0.01 g/(m2.h)，远低于同测试条件下无涂层石墨样品的质量损失率4.67 g/(m2.h)。在2 300 ℃氩气气氛下保温3 h的SiC粉包埋TaC涂层的接触腐蚀试验中，SiC和TaC涂层的界面清晰，没有发生相互的扩散。TaC涂层部件应用于2 000 ℃以上保温150 h以上的SiC单晶的生长制备后，涂层部件总体形貌保持完整，部件边缘棱角区域出现了脱落，但其他部位的TaC涂层仍和基体结合良好，涂层在长晶过程中的质量损失率约为0.41 g/(m2.h)，表现出良好的抗腐蚀性能。结论 熔盐法制备石墨表面TaC涂层的工艺简单、成本低、效率高，可制备曲面等不规则的构件。制备的TaC涂层晶粒堆积紧密，没有发生择优取向，与石墨基体的结合强度高，在侵蚀性的环境中，能减弱侵蚀性气体对石墨基体的侵蚀，有望在第三代半导体的制备中得到应用。本研究不仅提供了一种在石墨基体上制备TaC抗腐蚀涂层的方法，也提供了一种在其他碳材料上制备TaC涂层的方法。 |
| 英文摘要: |
| The work aims to prepare the TaC coating on the surface of graphite material with K2TaF7 and Ta powder as the main raw materials, which is of great value for reducing the preparation cost and improving the quality of third-generation semiconductors such as SiC, Gan, and AlN. TaC coating was synthesized on the surface of the graphite substrate by chemical reactions in molten salt at 1 200 ℃ for 3 h followed by high-temperature heat treatment of vacuum at 2 300 ℃ for 1 h. The phase composition and microstructure of the coating were characterized by XRD and SEM. The interface bonding strength between the TaC coating and the graphite substrate was measured by the pull-off method. The hardness and elastic modulus of the coating were characterized by nanoindentation. Finally, the corrosion resistance of the TaC coating was evaluated under simulated conditions and the TaC coated graphite was applied to the SiC crystal growth. The TaC coating prepared via molten salt method continuously covered the surface of the graphite and the surface morphology of the TaC coating was consistent with that of the original graphite substrate, with a bright yellow color. The phase composition of the coating was TaC and the thickness of the coating was about 20-40 μm. The TaC coating had a non-textured granular structure without preferred orientation growth. The interface bonding strength between the TaC coating and the graphite substrate was 9.49 MPa. The hardness and elastic modulus of the TaC coating were 14.42 GPa and 123.32 GPa, respectively. The mass loss rate was only 0.01 g/(m2.h) after the TaC coated graphite sample was kept at 2 300 ℃ for 3 h in SiC corrosion environment, which was much lower than that of uncoated graphite sample of 4.67 g/(m2.h) under the same test conditions. In the contact corrosion experiment with TaC coated graphite embedded by SiC powder at 2 300 ℃ argon for 3 h, the interface between SiC and TaC coating was clear and there was no mutual diffusion. After the TaC coated graphite was applied to the growth of SiC single crystal held at a temperature above 2 000 ℃ for more than 150 h, the overall morphology of the TaC coated graphite remained intact, and the edge corners of the TaC coated graphite peeled off. However, the TaC coating was still well combined with the graphite substrate elsewhere, and the mass loss rate of the TaC coated graphite was about 0.41 g/(m2.h), showing good corrosion resistance. The preparation process of TaC coating prepared on graphite surface by molten salt method is simple with low cost and high efficiency, and the TaC coating can be prepared on the surface of irregular components with complex shapes. The TaC coating grains are densely packed without preferential orientation, and the bonding strength with the graphite matrix is high, which can weaken the erosion of graphite substrate by aggressive gas in a corrosion environment. The TaC coated graphite prepared by molten salt method is expected to be applied in the preparation of the third generation semiconductor. This study provides a method for preparing TaC coating on not only the graphite substrate, but also other carbon materials. |
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