高功率脉冲磁控溅射制备的TiN薄膜应力释放及其结合稳定性研究  

Stress Release and Adhesion Stability of TiN Films Deposited by High Power Pulsed Magnetron Sputtering

作　　者：唐鑫 马东林 陈畅子[2] 冷永祥[1] 黄楠[1] TANG Xin;MA Dong-lin;CHEN Chang-zi;LENG Yong-xiang;HUANG Nan(School of Materials Science and Engineering,Southwest Jiaotong University,Chengdu 610031,China;Jingchu University of Technology,Jingmen 448000,China)

机构地区：[1]西南交通大学材料科学与工程学院,成都610031 [2]荆楚理工学院,湖北荆门448000

出　　处：《表面技术》2019年第9期245-251,共7页Surface Technology

基　　金：国家自然科学基金(31570958,U1330113)~~

摘　　要：目的探究高功率脉冲磁控溅射(HPPMS)制备的氮化钛(TiN)薄膜在自然时效过程中,应力、薄膜/基体结合性能随时间的变化规律。方法采用高功率脉冲磁控溅射(HPPMS)技术,通过调控基体偏压(-50、-150V),制备出具有不同残余压应力(3.18、7.46GPa)的TiN薄膜,并采用基片曲率法、X射线衍射法、划痕法和超显微硬度计评价了薄膜的应力、薄膜/基体结合性能、硬度随时间的变化规律。结果在沉积完成后1h内,-50V和-150V基体偏压下制备的TiN薄膜压应力分别在3.12~3.39GPa和7.40~7.55GPa范围内波动,薄膜压应力没有发生明显变化;沉积完成后1~7天,平均每天分别下降28.57MPa和35.71MPa;7~30天,平均每天分别下降2.08MPa和2.50MPa;30~60天内,平均每天分别下降1.67MPa和7.00MPa。其压应力连续下降,且均表现出前期下降速率快,后期下降逐渐放缓的趋势。自然放置60天后,应力基本释放完毕,薄膜性质基本保持稳定。同时,薄膜/基体结合性能随时间逐渐变差,薄膜硬度下降。结论HPPMS制备的TiN薄膜在自然时效过程中,其残余应力会随时间增加,连续下降,进而影响薄膜的力学性能。The work aims to investigate the time-dependent variation of stress and film/substrate bonding properties of TiN films prepared by high power pulsed magnetron sputtering (HPPMS) during natural aging.TiN thin films with different residual compressive stresses (3.18 and 7.46 GPa) were prepared with high power pulsed magnetron sputtering (HPPMS) by adjusting substrate bias (-50 and -150 V).The time-dependent variation of stress,film/substrate bonding and hardness of the films was evaluated by substrate curvature method,X-ray diffraction method,scratch method and ultra-microhardness tester.Within 1 hour after deposition,the compressive stresses of TiN films prepared under -50 V and -150 V substrate bias pressure fluctuated from 3.12 GPa to 3.39 GPa and 7.40 GPa to 7.5 GPa,respectively.The compressive stresses of TiN films did not change significantly. The average daily decrease was 28.57 MPa and 35.71 MPa for 1~7 days after deposition,2.08 MPa and 2.50 MPa for 7~30 days and 1.67 MPa and 7.00 MPa for 30~60 days,respectively.The compressive stress decreased continuously,and showed a rapid decline rate in the early stage and a gradual slowdown trend in the later stage.After 60 days of natural placement,the stress was basically released and the film properties remained stable.At the same time,the bonding property of the film/substrate became poor with time and the hardness of the film decreased.The residual stress of TiN films prepared by HPPMS will increase with time and decrease continuously during natural aging,which will affect the mechanical properties of the films.

关 键 词：高功率磁控溅射 氮化钛薄膜 薄膜应力 膜基结合力 自然时效 

分 类 号：TG174.4[金属学及工艺—金属表面处理]