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

作　　者：李荣斌 陈童童 蒋春霞 张如林 LI Rong-bin;CHEN Tong-tong;JIANG Chun-xia;ZHANG Ru-lin(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)

机构地区：[1]上海理工大学材料科学与工程学院,上海200093 [2]上海电机学院材料学院,上海201306

出　　处：《表面技术》2020年第11期161-167,共7页Surface Technology

基　　金：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)。

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0.070Ω/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。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.

关 键 词：高熵合金 非晶结构 磁控溅射 扩散阻挡性 退火 

分 类 号：TG156[金属学及工艺—热处理]