直流脉冲磁控溅射铜膜的结构与性能研究
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摘要
采用直流脉冲磁控溅射法制备铜膜,利用X射线衍射法分析薄膜相结构,通过扫描电镜观察薄膜形貌,基于纳米压痕载荷-位移曲线计算薄膜的硬度、弹性模量和接触刚度,同时采用显微硬度法测量薄膜硬度,系统研究了溅射功率和偏压对铜膜结构和力学性能的影响。结果表明,通过纳米压痕载荷-位移曲线计算薄膜力学性能是可靠的。随着溅射功率的增大,铜膜生长取向几乎无变化,均呈无择优生长状态,弹性模量、接触刚度基本不变,硬度略有减小;偏压增大会使铜膜呈现明显的(111)取向生长,接触刚度、弹性模量和硬度呈下降趋势。
Copper films were prepared by DC pulsed magnetron sputtering.The film phase structure was analyzed using X-ray diffraction and the film morphology was observed by scanning electron microscopy.The hardness,elastic modulus,and contact stiffness of Cu films were calculated based on nanoindentation load-displacement curve.The film hardness was also tested by microhardness tester.Thus,effects of sputtering power and bias on the structure and mechanical properties of copper films were investigated systematically.The results show that the mechanical property calculation of thin films through the nanoindentation load-displacement curves is reliable.With the increase of sputtering power the copper film always presents no preferential growth,and the elastic modulus and contact stiffness are almost unchanged,but the hardness decreases slightly.However,the copper film presents obvious preferred orientation of(111)with increasing bias,and all of the contact stiffness,elastic modulus and hardness decrease.
Copper films were prepared by DC pulsed magnetron sputtering.The film phase structure was analyzed using X-ray diffraction and the film morphology was observed by scanning electron microscopy.The hardness,elastic modulus,and contact stiffness of Cu films were calculated based on nanoindentation load-displacement curve.The film hardness was also tested by microhardness tester.Thus,effects of sputtering power and bias on the structure and mechanical properties of copper films were investigated systematically.The results show that the mechanical property calculation of thin films through the nanoindentation load-displacement curves is reliable.With the increase of sputtering power the copper film always presents no preferential growth,and the elastic modulus and contact stiffness are almost unchanged,but the hardness decreases slightly.However,the copper film presents obvious preferred orientation of(111)with increasing bias,and all of the contact stiffness,elastic modulus and hardness decrease.
引文
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[2]Wu Guifang,Shi Shouhua,He Yuping,et al.Influence of annealing temperature on microstructures and stress of sputtered Cu film on Si substrate[J].Chinese Journal of Vacuum Science and Technology,2002,22(2):139-142.吴桂芳,史守华,何玉平,等.退火温度对硅基溅射铜膜应力的影响[J].真空科学与技术,2002,22(2):139-142.
[3]Guo Junting,Xu Yang.Study on the performance of nanocopper film deposited by magnetron sputtering[J].Journal of Functional Materials,2015,46(5):05123-05127.郭俊婷,徐阳.磁控溅射法沉积纳米Cu薄膜的性能研究[J].功能材料,2015,46(5):05123-05127.
[4]Gao Lihua,Zheng Yuying.Effects of sputtering power on Al doped ZnO thin films deposited by RF magnetron sputtering[J].Journal of Functional Materials,2015,46(8):08028-08030.高立华,郑玉婴.溅射功率对磁控溅射ZnO:Al(ZAO)薄膜性能的影响[J].功能材料,2015,46(8):08028-08030.
[5]Zhou Xuyang,Wu Aimin,Ma Yanping,et al.Influence of sputtering power on properties of BCMg thin films prepared by magnetron sputtering[J].Journal of Dalian University of Technology,2014,54(3):298-302.周徐洋,吴爱民,马艳萍,等.磁控溅射工艺中靶材溅射功率对BCMg薄膜性能影响[J].大连理工大学学报,2014,54(3):298-302.
[6]Ding Jianning,Xie guoxin,Fan Zhen,et al.Effects of sputtering power on surface topography and mechanical properties of GeSb2Te4phase change films[J].Journal of Jiangsu University(Natural Science Edition),2005,26(5):372-375.丁建宁,解国新,范真,等.溅射功率对GeSb2Te4膜形貌及力学性能的影响[J].江苏大学学报(自然科学版),2005,26(5):372-375.
[7]Zhang Ling,He Zhibing,Li Jun,et al.Influence of sputtering power on components and mechanical properties of boron carbide films[J].High Power Laser and Particle Beams,2013,25(9):2317-2323.张玲,何智兵,李俊,等.溅射功率对碳化硼薄膜组分与力学性能的影响[J].强激光与粒子束,2013,25(9):2317-2323.
[8]Wang Q M,Kim K H.Effect of negative bias voltage on CrN films deposited by arc ion plating.Ⅱ.Film composition,structure,and properties[J].Journal of Vacuum Science and Technology A,2008,26(5):1268-1276.
[9]Liu Xing,Ma Guojia,Sun Gang,et al.Growth and property characterization of magnetron sputtered TaN[J].Chinese Journal of Vacuum Science and Technology,2013,33(1):54-60.刘星,马国佳,孙刚,等.气压及偏压对磁控溅射TaN薄膜力学性能影响[J].真空科学与技术,2013,33(1):54-60.
[10]Zhu Shengfa,Wu Yanping,Liu Tianwei,et al.Effect of pulse bias voltage on microstructure and properties of CrNxfilm prepared by magnetron sputtering on uranium[J].Transactions of Materials and Heat Treatment,2012,33(5):116-120.朱生发,吴艳萍,刘天伟,等.脉冲偏压对贫铀表面磁控溅射CrNx薄膜结构与性能的影响[J].材料热处理学报,2012,33(5):116-120.
[11]Gu Wencui,Li Shoude,Wang Huaiyong,et al.Influence of bias voltage on microstructure and properties of magnetron sputtering TiB2coating[J].Journal of Aeronautical Materials,2014,34(5):37-42.谷文翠,李寿德,王怀勇,等.基片偏压对磁控溅射制备TiB2涂层结构及性能的影响[J].航空材料学报,2014,34(5):37-42.
[12]Xue Yaping,Cao Jun,Yu Lihua,et al.Effects of bias voltage on microstructure and properties of magnetron sputtering TaN films[J].The Chinese Journal of Nonferrous Metals,2013,23(7):1923-1970.薛雅平,曹峻,喻利花,等.负偏压对磁控溅射TaN薄膜微观结构和性能的影响[J].中国有色金属学报,2013,23(7):1923-1970.
[13]Wu Xiaojing,Wu Zijing,Jiang Bin.Application of nanoindentation tests in research of nanomaterials[J].Journal of Fudan University(Natural Science)2008,47(1):1-7.吴晓京,吴子景,蒋宾.纳米压痕试验在纳米材料研究中的应用[J].复旦学报(自然科学版),2008,47(1):1-7.
[14]Oliver W C,Pharr G M.An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments[J].Journal of Materials Research,1992,7:1564-1583.
[15]Oliver W C,Pharr G M.Measurement of Hardness and Elastic Modulus by Instrumented indentation:Advances in Understanding and Refinements to Methodology[J].Journal of Materials Research,2004,19(I):3-20.
[16]Yin Chuan.Study on copper thin films prepared by magnetron sputtering and its super hydrophobic surface modification[D].Nanjing:Nanjing University of Science and Technology,2013.殷川.磁控溅射法制备铜薄膜及其超疏水表面改性研究[D].南京:南京理工大学,2013.
[17]Tan Shuyong,Zhang Xuhai,Wu Xiangjun,et al.Comparison of chromium nitride coatings deposited by DC and RF magnetron sputtering[J].Thin Solid Films,2011,519:2116-2120.
[18]Duan Linglong.Studies on the structure and properties of Ti films fabricated by magnetron sputtering[D].Lanzhou:Lanzhou University,2008.段玲珑.磁控溅射制备Ti膜的结构与性能研究[D].兰州:兰州大学,2008.
[19]Liu Zhaozheng,Liu Yaohui,Tong Yuling,et al.Influence of bias on microstructures and properties of CrAlTi(Ce)N coatings[J].Chinese Journal of Vacuum Science and Technology,2011,31(1):80-84.刘兆政,刘耀辉,佟玉玲,等.偏压对CrAlTi(Ce)N薄膜的制备和性能的影响[J].真空科学与技术,2011,31(1):80-84.
[20]Tang Dapei,Gao Qing,Jiang Xiaoyu.Properties of TiN and TiC and Ti(C,N)coatings and the factors affecting the properties[J].Materials protection,2005,38(3):42-46.唐达培,高庆,江晓禹.TiN,TiC和Ti(C,N)涂层的性能及影响因素研究[J].材料保护,2005,38(3):42-46.