VNbMoTaWCo高熵合金氮化物扩散阻挡层的制备及其热稳定性

doi:10.13251/j.issn.0254-6051.2022.06.037

金属热处理 ›› 2022, Vol. 47 ›› Issue (6): 196-201.DOI: 10.13251/j.issn.0254-6051.2022.06.037

VNbMoTaWCo高熵合金氮化物扩散阻挡层的制备及其热稳定性

李荣斌^1,2, 张霞¹, 蒋春霞²

1.上海理工大学材料与化学学院, 上海 200093;
2.上海电机学院材料学院, 上海 201306

收稿日期:2022-01-23 修回日期:2022-04-18 出版日期:2022-06-25 发布日期:2022-07-05
作者简介:李荣斌(1969—),男,教授,博士,主要研究方向为高温合金结构与性能,E-mail: lirb@sdju.edu.cn
基金资助:
上海市地方院校能力建设项目(21010500900);上海大件热制造工程技术研究中心(18DZ2253400)

Preparation and thermal stability of VNbMoTaWCo-nitride diffusion barrier layer

Li Rongbin^1,2, Zhang Xia¹, Jiang Chunxia²

1. School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China;
2. School of Materials, Shanghai Dianji University, Shanghai 201306, China

Received:2022-01-23 Revised:2022-04-18 Online:2022-06-25 Published:2022-07-05

摘要/Abstract

摘要： 利用直流磁控溅射镀膜机设置不同氮气流量参数,制备VNbMoTaWCoN_x薄膜,氮气流量为20%时,在洁净的硅基底上沉积厚度约为15 nm的VNbMoTaWCoN₂₀高熵合金氮化物薄膜,并在其上面再溅镀一层厚度约为50 nm的Cu膜,最终形成Cu/VNbMoTaWCoN₂₀/Si 三层复合结构。采用四点探针电阻测试仪(FPP)、X射线衍射仪(XRD)、原子力显微镜(AFM)、场发射扫描电镜(SEM)对三层复合结构500 ℃退火前后的方块电阻、物相结构、粗糙度以及表面形貌进行了分析表征,研究了VNbMoTaWCoN₂₀高熵合金氮化物薄膜作为扩散阻挡层的热稳定性。研究结果表明,当氮气流量占比为20%时,VNbMoTaWCo₂₀高熵合金氮化物薄膜为非晶态,且出现了微量纳米晶;此氮气流量占比下制备的薄膜表面平整光滑、致密度最佳、粗糙度数值最小。Cu/VNbMoTaWCoN₂₀/Si三层复合结构进行500 ℃退火8 h后,Cu膜的方块电阻仍然维持在较低的数值,即0.065 Ω/sq,虽然Cu膜发生团聚,但是并未检测到高阻态Cu-Si化合物。VNbMoTaWCoN₂₀高熵合金氮化物薄膜作为扩散阻挡层在500 ℃温度下退火8 h后,表现出了优异的热稳定性。

关键词: 高熵合金氮化物薄膜, 热稳定性, 扩散阻挡层, 退火, 直流磁控溅射

Abstract: VNbMoTaWCoN_x films (x=N₂ flow rate) were prepared by DC magnetron sputtering in different N₂ flow parameter. At N₂ flow ratio of 20%, a Cu/VNbMoTaWCoN₂₀/Si triple-layer stack structure was prepared by depositing a 15 nm thick VNbMoTaWCoN₂₀ film on the cleaned silicon substrate and depositing a 50 nm thick Cu film on the top. The sheet resistance, phase structure, roughness and surface morphology of the Cu/VNbMoTaWCoN₂₀/Si structure samples before and after annealing at 500 ℃ were analyzed and characterized by four probe resistance tester (FPP), X-ray diffractometer (XRD), atomic force microscope (AFM), field emission scanning electron microscope (SEM), and then the thermal stability and diffusion barrier properties of the VNbMoTaWCoN₂₀ film were studied. The results indicate that when the N₂ flow ratio is 20%, the VNbMoTaWCoN₂₀ film before annealing is amorphous with some locally dispersed nanocrystals, and with flat and smooth film surface, with the best density and the smallest roughness. After the Cu/VNbMoTaWCoN₂₀/Si triple-layer stack structure is annealed at 500 ℃ for 8 h, though agglomeration occurs on the surface of the Cu film, but no Cu-Si compound is found, and the sheet resistance of the film is still maintained at a low value 0.065 Ω/sq. The amorphous structured VNbMoTaWCoN₂₀ film as diffusion barrier layer annealed at 500 ℃ for 8 h showes excellent thermal stability and diffusion barrier properties.

Key words: high-entropy alloy nitride film, thermal stability, diffusion barrier layer, annealing, DC magnetron sputtering

中图分类号:

TG174.4

李荣斌, 张霞, 蒋春霞. VNbMoTaWCo高熵合金氮化物扩散阻挡层的制备及其热稳定性[J]. 金属热处理, 2022, 47(6): 196-201.

Li Rongbin, Zhang Xia, Jiang Chunxia. Preparation and thermal stability of VNbMoTaWCo-nitride diffusion barrier layer[J]. Heat Treatment of Metals, 2022, 47(6): 196-201.

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VNbMoTaWCo高熵合金氮化物扩散阻挡层的制备及其热稳定性

Preparation and thermal stability of VNbMoTaWCo-nitride diffusion barrier layer

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