李忠盛,陈大军,莫非,黄安畏,付扬帆,刘正涛,吴厦,丛大龙.高密度C/C表层TaC改性及其高温抗氧化性[J].表面技术,2023,52(8):255-262.
LI Zhong-sheng,CHEN Da-jun,MO Fei,HUANG An-wei,FU Yang-fan,LIU Zheng-tao,WU Xia,CONG Da-long.TaC Modification of High-density C/C Surface and Its High Temperature Oxidation Resistance[J].Surface Technology,2023,52(8):255-262 |
| 高密度C/C表层TaC改性及其高温抗氧化性 |
| TaC Modification of High-density C/C Surface and Its High Temperature Oxidation Resistance |
| 投稿时间：2022-08-18 修订日期：2022-11-23 |
| DOI：10.16490/j.cnki.issn.1001-3660.2023.08.020 |
| 中文关键词: 浸渍 TaC改性层 物相组成 体积密度 高温抗氧化性 |
| 英文关键词:impregnation TaC modified layer phase composition volume density high temperature oxidation resistance |
| 基金项目: |
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| Author | Institution |
| LI Zhong-sheng | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| CHEN Da-jun | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| MO Fei | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| HUANG An-wei | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| FU Yang-fan | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| LIU Zheng-tao | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| WU Xia | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
| CONG Da-long | Southwest Institute of Technology and Engineering, Chongqing 401329, China |
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| 中文摘要: |
| 目的 研究高密度C/C表层TaC改性层的制备工艺及微观结构，分析TaC改性层的高温抗氧化性能。方法 采用真空加压浸渍和高温原位反应法生成TaC改性层，采用X射线衍射仪(XRD)分析TaC改性层的物相组成，采用体积密度来表征不同浸渍时间、浸渍次数等浸渍工艺下C/C基体的密度，采用带能谱仪的环境扫描电子显微镜(SEM)对TaC改性层的截面形貌、元素组成进行表征，采用氧-乙炔焰测试TaC改性层的高温抗氧化性能。结果 XRD分析表明，改性层由C和TaC组成。密度测试结果表明，体积密度随浸渍次数和浸渍时间的增加先迅速增大后趋缓，在浸渍15 min、循环浸渍11次后，C/C基体的体积密度达到1.88 g/cm3。SEM观测结果表明，改性层中TaC颗粒呈液滴状或团簇状，尺寸为1~3 μm，不均匀分布在TaC改性层中。高温氧-乙炔试验结果表明，试验后，TaC改性层表面生成厚度约30~40 μm且结构较为完整的黏滞状Ta2O5层，在氧化50 s时，其质量损失率仅1.9%。结论 采用真空加压浸渍和高温原位反应法能在高密度C/C表层生成TaC改性层，提高了C/C复合材料的高温抗氧化性能。 |
| 英文摘要: |
| The work aims to study the preparation process and microstructure of TaC modified layers on the high-density C/C surface, and to analyze the high-temperature oxidation resistance of the TaC modified layers.In this paper, 2.5 D puncture C/C composites with high density of 1.8 g/cm3 were used as matrix, and its size was φ15 mm×10 mm, the mixed solution of TaCl5 and anhydrous ethanol was selected as the impregnation solvent, and the mass percentage concentration of Tacl5 was 6%. Firstly, the C/C matrix was impregnated by a self-developed vacuum pressurized impregnation system, and the impregnation process parameters were designed as follows:the impregnation time was 5 min, 15 min, 25 min and 35 min respectively; the impregnation times was 5, 7, 9, 11, 13, 15 respectively; the vacuum for impregnation was 8×10–1 Pa and the impregnation pressure was 2 MPa. Secondly, the C/C matrix after impregnation was reduced in hydrogen environment to reduce TaCl5 to Ta, and the process parameters were designed as follows:the reduction temperature was 800 ℃; the reduction time was 5 min. Finally, the C/C matrix after hydrogen reduction was heated at high-temperature to make Ta in-situ reaction with C in C/C matrix to form TaC, and the process parameters were designed as follows:the heating temperature of in-situ reaction was 1 900 ℃; the reduction time was 8 min. According to the TaC modified layer prepared by the above processes, the phase composition of the TaC modified layer was analyzed by an X-ray diffractometer (XRD), the volume density was used to characterize the density of C/C matrix under different impregnation processes such as impregnation time and impregnation times, the cross-sectional morphology and elemental composition of the TaC modified layer were characterized by an environmental scanning electron microscope and an energy dispersive spectrometer (SEM). The oxygen-acetylene flame was used to test the high-temperature oxidation resistance of the TaC modified layer. XRD analysis showed that the modified layer consisted of C and TaC. The results of volume density test showed that the volume density of C/C matrix increased rapidly and then slowed down with the increase of impregnation time and impregnation times. The volume density of the C/C matrix reached 1.88 g/cm3 under the conditions of impregnation time of 15 min and impregnation times of 11. The results of high power SEM observations showed that TaC particles in the TaC modified layer were droplet-shaped or cluster-shaped, 1-3 μm in size, unevenly and discontinuity distributed in the C/C matrix. The results of high-temperature oxygen-acetylene test showed that the surface of the TaC modified layer after the test was formed with a thickness of about 30 μm to 40 μm and a relatively complete structure of the viscous Ta2O5 layer, and the quality loss rate was only 1.9% when the oxidation time was 50 s. It is only 1/6 of the mass loss rate of pure C/C composite material. In conclusion, vacuum pressure impregnation and high temperature in situ reaction method can generate TaC modified layers on the high-density C/C surface, which improves the high temperature oxidation resistance of C/C composites. |
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