李岩,张伟强.磁控溅射工艺对FeCrCoNiMn氧化物薄膜质量的影响[J].表面技术,2023,52(1):56-62, 92.
LI Yan,ZAHNG Wei-qiang.Effects of Magnetron Sputtering Process on Quality of FeCrCoNiMn Oxide Films[J].Surface Technology,2023,52(1):56-62, 92 |
| 磁控溅射工艺对FeCrCoNiMn氧化物薄膜质量的影响 |
| Effects of Magnetron Sputtering Process on Quality of FeCrCoNiMn Oxide Films |
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| DOI：10.16490/j.cnki.issn.1001-3660.2023.01.006 |
| 中文关键词: 磁控溅射 高熵合金 氧化物 膜基结合力 硬度 弹性模量 |
| 英文关键词:magnetron sputtering high entropy alloy oxide film-substrate adhesion hardness elastic modulus |
| 基金项目:装备预先研究领域基金(61409230111) |
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| 中文摘要: |
| 目的 探究氧气浓度、基底温度和溅射功率对高熵合金氧化物薄膜成分、膜基结合力和硬度的影响，分别找出某一工艺参数的改变对性能的影响趋势，并总结影响因素和规律。方法 采用射频磁控溅射方法在Si(100)基体上制备不同工艺参数下的(FeCrCoNiMn)Ox薄膜，结合X射线衍射仪(XRD)、能谱仪(EDS)、划痕仪、纳米压痕仪分析薄膜的物相结构、成分组成、膜基结合力、硬度和弹性模量。结果 薄膜为FCC结构。膜基结合力、硬度和弹性模量随着氧气浓度的增加，分别由4.85 N、6.06 GPa、137.8 GPa提高至6.56 N、14.51 GPa、189.4 GPa，最后降至3.75 N、7.52 GPa、144.9 GPa。薄膜的膜基结合力、硬度和弹性模量随着基底温度的升高而升高，分别由3.6 N、12.58 GPa、164.2 GPa升高到5.05 N、14.51 GPa、189.4 GPa。随着溅射功率的提高，膜基结合力由5.05 N提高至8.25 N，硬度和弹性模量呈先升高后降低的趋势。结论 与普通FeCrCoNiMn合金薄膜相比，氧原子的引入使(FeCrCoNiMn)Ox薄膜拥有更大的混合熵，增强了其固溶强化效应。氧气浓度和溅射功率对薄膜成分的影响较大，基底温度对成分无明显影响。适当提高氧气浓度和溅射功率可以有效提高薄膜的力学性能，在温度为350 ℃时膜基结合力和硬度均最好。 |
| 英文摘要: |
| The work aims to explore the effects of oxygen concentration, substrate temperature and sputtering power on the film components, film-substrate adhesion and hardness of high-entropy alloy oxides, find out the influence trend of a certain process parameter change on the performance, and summarize the influencing factors and rules. In this experiment, the (FeCrCoNiMn)Ox films under different process parameters were prepared on the Si(100) matrix by RF magnetron sputtering, and the phase structure, composition, film-substrate adhesion, hardness and elastic modulus of the films were analyzed with X-ray diffractometer (XRD), energy spectrometer (EDS), scratch meter and nanoindenterometer. The results showed that the film had an FCC structure and did not form a metal-oxide mixture. The grain size and crystallinity of the films decreased with the increase of oxygen concentration; The increase of substrate temperature led to the increase of grain size and the thickening of films. With the increase of oxygen concentration , the oxygen atoms in the film were close to saturation, and the oxygen content in the films increased rapidly when the oxygen concentration was 0%-10%; When it exceeded 10%, the rising trend of oxygen element in the film slowed down. The film composition was the closest to the equiatomic ratio when the sputtering power was 150 W, and the mixing entropy was the highest. The substrate temperature had little effect on the film composition and mixing entropy. As oxygen concentration increased, the film-substrate adhesion, hardness, and elastic modulus increased and then decreased, from 4.85 N, 6.06 GPa, and 137.8 GPa at 0 percent to 6.56 N, 14.51 GPa, and 189.4 GPa at 5 percent, and then it dropped to 3.75 N, 7.52 GPa, and 144.9 GPa at 20 percent. The film-substrate adhesion, hardness and elastic modulus increased with the increase of the substrate temperature, from 3.6 N, 12.58 GPa and 164.2 GPa to 5.05 N, 14.51 GPa, and 189.4 GPa, respectively. With the increase of sputtering power, the film-substrate adhesion increased from 5.05 N to 8.25 N, and the hardness and elastic modulus increased from 9.5 GPa and 170.3 GPa to 14.51 GPa and 189.4 GPa respectively and then decreased to 11.38 GPa and 172.6 GPa, respectively. Compared with ordinary FeCrCoNiMn alloy films, the introduction of oxygen atoms makes (FeCrCoNiMn) Ox films have greater mixed entropy, which enhances its solution strengthening effect; but when the oxygen concentration is too high, the oxygen atoms in the film are saturated, and the quality of the film decreases. Therefore, it is very important to select the correct process parameters for the quality of the film. The oxygen concentration and sputtering power have a great influence on the composition of the film, but the substrate temperature has no significant effect on the composition. The mechanical properties of the films can be effectively improved by properly increasing the oxygen concentration and sputtering power. When the substrate temperature is 350 ℃, the film-substrate adhesion and hardness are the highest. The performance is best when the oxygen concentration is 5%. |
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