王林青,蒲春林,张艳,王军军.Al含量对TiZrNbMoAlx难熔高熵合金薄膜高温抗氧化的影响[J].表面技术,2025,54(1):53-61, 73.
WANG Linqing,PU Chunlin,ZHANG Yan,WANG Junjun.Effect of Al Content on High-temperature Oxidation Resistance of TiZrNbMoAlx Refractory High Entropy Alloy Thin Films[J].Surface Technology,2025,54(1):53-61, 73 |
| Al含量对TiZrNbMoAlx难熔高熵合金薄膜高温抗氧化的影响 |
| Effect of Al Content on High-temperature Oxidation Resistance of TiZrNbMoAlx Refractory High Entropy Alloy Thin Films |
| 投稿时间：2024-09-18 修订日期：2024-12-31 |
| DOI：10.16490/j.cnki.issn.1001-3660.2025.01.005 |
| 中文关键词: 难熔高熵合金薄膜 高温抗氧化性能 Al含量 相组成 微观结构 |
| 英文关键词:refractory high entropy alloy thin film high temperature oxidation resistance Al content phase composition microstructure |
| 基金项目:国家自然科学基金(52475177);重庆市科技局科技项目/重庆市自然科学基金(CSTB2023NSCQ-MSX0439) |
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| Author | Institution |
| WANG Linqing | School of Science,Chongqing 400054, China |
| PU Chunlin | School of Science,Chongqing 400054, China |
| ZHANG Yan | School of Materials Science and Engineering, Chongqing University of Technology, Chongqing 400054, China |
| WANG Junjun | School of Materials Science and Engineering, Chongqing University of Technology, Chongqing 400054, China |
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| 中文摘要: |
| 目的 探讨Al含量对TiZrNbMoAlx难熔高熵合金(Refractory High-entropy Alloys，RHEAs)薄膜结构和高温抗氧化性能的影响，并讨论TiZrNbMoAlx RHEAs薄膜的氧化机理。方法 利用双靶磁控共溅射技术，以90°扇形的Ti、Zr、Nb、Mo靶拼接而成的靶材和Al靶材作为溅射靶材，通过调节Al靶溅射功率，制备不同Al含量(原子数分数0%、14%、18%、24%、28%)的TiZrNbMoAlx RHEAs薄膜，并将这些薄膜置于600 ℃大气环境中进行氧化试验。采用场发射扫描电子显微镜(FESEM)、能量色散光谱仪(EDS)、X射线衍射仪(XRD)和X射线光电子能谱仪(XPS)等，对氧化前后薄膜的物相组成和微观结构进行分析。对比不同Al含量的TiZrNbMoAlx RHEAs薄膜的抗氧化性能，并分析其氧化机理。结果 薄膜的微观结构和高温抗氧化性能与Al含量密切相关。不含Al时，薄膜呈现出(110)择优取向的BCC单相固溶体结构;Al原子数分数为14%~24%时，薄膜表现为无定形相结构;Al含量较高(原子数分数为28%)时，薄膜中出现了AlZr3二次相。在600 ℃环境退火后，Al氧化生成了Al2O3，这有效提升了TiZrNbMoAlx RHEAs薄膜的抗氧化性能。然而，过量的Al含量(原子数分数为28%)会导致应力集中并产生裂纹，降低薄膜的高温抗氧化性能。结论 Al含量对TiZrNbMoAlx RHEAs薄膜的高温抗氧化性能具有重要影响，适量的Al含量可改善TiZrNbMoAlx RHEAs薄膜的抗氧化性能。 |
| 英文摘要: |
| Refractory high-entropy alloys (RHEAs), which exhibit excellent mechanical properties at high temperature, are being developed for potential applications in high-temperature environments. However, their poor high-temperature oxidation resistance significantly restricts their practical application. This work aims to investigate the oxidation resistance behavior of TiZrNbMoAlx RHEAs films with different Al contents, and provide theoretical supports for improving the oxidation resistance of TiZrNbMoAlx RHEAs films. In this study, TiZrNbMoAlx RHEAs films were prepared using a magnetron co-sputtering system with a spliced target (ϕ76.2 mm×5 mm) composed of 90° fan-shaped Ti, Zr, Nb and Mo (99.95% purity), and an Al target (ϕ76.2 mm×5 mm, 99.95% purity) as the sputtering targets. TiZrNbMoAlx RHEAs films with different Al contents (0at.%, 14at.%, 18at.%, 24at.% and 28at.%) were obtained by adjusting the sputtering power of the Al target. The as-deposited TiZrNbMoAlx RHEAs films were subjected to oxidation tests at 600 ℃ in air. The phase composition and microstructure of the films before and after oxidation were analyzed by field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray Diffraction (XRD). The oxidation resistance of TiZrNbMoAlx RHEAs films with different Al contents was compared, and the oxidation mechanisms of the films were analyzed. It was found that the microstructure and high-temperature oxidation resistance of the films were strongly dependent on the Al content. The TiZrNbMoAlx RHEAs films without Al content presented a (110) preferred orientation BCC single-phase solid solution structure. The TiZrNbMoAlx RHEAs films with low Al contents (14at.%-24at.%) exhibited an amorphous phase structure. When the Al content was high (28at.%), an AlZr3 secondary phases were found in the films. After oxidation at 600 ℃, in the absence of Al content, cellular protrusions appeared on the film surface, accompanied by fissures. Notably, some protrusions detached easily when manipulated with tweezers. Simultaneously, the film thickness increased from an initial 1.20 μm to 2.20 μm, representing an accelerated thickness growth rate of 83%, ultimately leading to complete oxidation of the film. The introduction of Al effectively improved the oxidation resistance characteristics of the TiZrNbMoAlx RHEAs films, attributed to the presence of an oxide layer containing Al2O3 on the film surface. The higher the Al content, the denser the oxide layer containing Al2O3, and the better the oxidation resistance of the film. When the Al content increased from 14at.% to 24at.%, the thickness growth rate decreased from 83% to 28%. However, excessive Al content (28at.%) led to stress concentration, resulting in cracks that worsened the high-temperature oxidation resistance of the films. In conclusion, Al content has a significant influence on the high-temperature oxidation resistance properties of TiZrNbMoAlx RHEAs films. Appropriate Al content can improve the oxidation resistance properties of TiZrNbMoAlx RHEAs films. |
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