李荣斌,陈童童,蒋春霞,张如林.高熵合金AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7扩散阻挡层的制备与性能研究[J].表面技术,2020,49(11):161-167.
LI Rong-bin,CHEN Tong-tong,JIANG Chun-xia,ZHANG Ru-lin.Preparation and Properties of High-entropy Alloy AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7 Diffusion Barrier Layers[J].Surface Technology,2020,49(11):161-167
高熵合金AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7扩散阻挡层的制备与性能研究
Preparation and Properties of High-entropy Alloy AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7 Diffusion Barrier Layers
投稿时间:2020-01-10  修订日期:2020-04-23
DOI:10.16490/j.cnki.issn.1001-3660.2020.11.017
中文关键词:  高熵合金  非晶结构  磁控溅射  扩散阻挡性  退火
英文关键词:high-entropy alloy  amorphous structure  magnetron sputtering  diffusion barrier  annealing
基金项目:国家自然科学基金面上项目(51671125);上海大件热制造工程技术研究中心(18DZ2253400)
作者单位
李荣斌 上海理工大学 材料科学与工程学院,上海 200093;上海电机学院 材料学院,上海 201306 
陈童童 上海理工大学 材料科学与工程学院,上海 200093 
蒋春霞 上海电机学院 材料学院,上海 201306 
张如林 上海电机学院 材料学院,上海 201306 
AuthorInstitution
LI Rong-bin School of Materials Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China;School of Materials, Shanghai DianJi University, Shanghai 201306, China 
CHEN Tong-tong School of Materials Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China 
JIANG Chun-xia School of Materials, Shanghai DianJi University, Shanghai 201306, China 
ZHANG Ru-lin School of Materials, Shanghai DianJi University, Shanghai 201306, China 
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中文摘要:
      目的 验证15 nm厚度AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7的势垒层热稳定性和扩散阻挡性能。方法 采用直流磁控溅射技术在n型Si(111)基片上真空溅射沉积15 nm的AlCrTaTiZrRu(3 nm)/(AlCrTaTiZrRu)N0.7 (12 nm)双层阻挡层,随后在双层AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7薄膜的顶部沉积50 nm厚的Cu膜,最终制得Cu/AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7/Si复合薄膜试样。将样品在真空退火炉中分别进行600~900 ℃高温退火30 min,以模拟最恶劣的应用环境。用场发射扫描电镜(FE-SEM)、X射线衍射仪(XRD)、能谱分析仪(EDS)、四探针电阻测试仪(FPP)以及原子力显微镜(AFM)对试样的表面形貌、物相组成、化学成分、方块电阻和粗糙度进行表征分析。结果 沉积态AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7薄膜呈现非晶结构,与Cu膜和Si衬底的结合良好。在800 ℃退火后,Cu/AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7/Si薄膜系统结构完整,膜层结构界面之间未出现分层现象,表面Cu颗粒团聚现象加剧,Si衬底和Cu膜表面未发现Cu-Si化合物生成,薄膜方阻保持在较低的0.070 Ω/sq;900 ℃退火后,薄膜系统未出现层间分离和空洞现象,Cu膜表面形成孤立的大颗粒Cu-Si化合物,薄膜电阻率大幅上升。结论AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7双层结构在800 ℃退火后仍能有效抑制Cu与Si相互扩散,其非晶结构增强了Cu/HEA/HEAN0.7/Si体系的热稳定性和扩散阻挡性。
英文摘要:
      The work aims to verify the thermal stability and diffusion-barrier performance of the 15-nm-thick AlCrTaTiZrRu/ (AlCrTaTiZrRu)N0.7 barrier layers. The 15-nm AlCrTaTiZrRu (3 nm)/(AlCrTaTiZrRu)N0.7 (12 nm) double-layer barrier layers were deposited on n-type Si (111) substrate by a DC magnetron-sputtering technology. Subsequently, a 50-nm-thick of Cu film was deposited on the top of the AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7 composite film, to obtain the Cu/AlCrTaTiZrRu/ (AlCrTaTiZrRu)N0.7/Si composite thin film samples. The samples were annealed in a vacuum-annealing furnace at 600-900 ℃ for 30 minutes to simulate the worst application environment. Field emission scanning electron microscopy (FE-SEM), X-ray diffractometer (XRD), energy spectrum analyzer (EDS), four-probe resistance tester (FPP), and atomic force microscope (AFM) were applied to characterize and analyze the surface morphology, phase composition, chemical composition, square resistance and roughness of the samples. The results indicated that the as-deposited AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7 films exhibited amorphous structure and were well bonded to Cu film and Si substrate. After annealing at 800 ℃, the Cu/AlCrTaTiZrRu/ (AlCrTaTiZrRu)N0.7/Si films system still exhibited a complete structure, no delamination occurred between the interface of the film structure, and the agglomeration of Cu particles on the surface was intensified. However, no Cu-Si compound was found on the surface of the Si substrate and Cu film, and the square resistance of the films was kept at a low value of 0.070Ω/sq. After annealing at 900 ℃, there was no interlayer separation and void phenomenon in the thin films system. Isolated large particles of Cu-Si compounds were formed on the surface of the Cu film, and the resistivity of the films increased significantly. The AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7 double-layer structure can still effectively inhibit the interdiffusion of Cu and Si after annealing at 800 ℃. Its amorphous structure enhances the thermal stability and diffusion-barrier of the Cu/HEA/HEAN0.7/Si system.
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