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溅射靶材用超高纯铜及铜铝合金微观组织与织构研究
Study on Microstructure and Texture of Ultra-high Purity Copper and Copper-aluminum Alloy for Sputtering Target
【作者】 张静;
【导师】 刘施峰;
【作者基本信息】 重庆大学 , 工程(材料工程)(专业学位), 2021, 硕士
【摘要】 随着集成电路的快速发展,对超高纯铜和铜铝合金溅射靶材的微观组织和织构提出更高的要求,研究不同轧制方式和退火工艺对超高纯铜与铜铝合金微观组织与织构的影响,有助于提高溅射靶材的品质。基于此,本文通过金相显微镜、X射线衍射、电子背散射衍射等技术,系统研究了不同轧制方式和不同形变量的超高纯铜和铜铝合金板材的微观组织,及其在不同退火工艺后的再结晶组织和织构演变规律,通过研究得出如下结论:(1)单向轧制和交叉轧制90%压下量的超高纯铜试样在室温下发生了明显的动态再结晶,前者还发生严重的晶粒异常长大,两者都会有Cube织构生成;两种轧制方式下,变形量90%的Cu-0.1Al合金试样为沿轧制方向的层片状的轧制态组织,Brass织构较为明显。单向轧制54%、70%和90%压下量的超高纯铜在100℃保温1h后开始生成了再结晶晶粒,变形量增加,试样的再结晶晶粒更多,再结晶程度更高;在200℃保温1h,随着变形量增加,试样的平均晶粒尺寸变小,特殊晶界含量增加;在300℃保温1h,随着变形量的增加,晶粒越容易发生异常长大。(2)单向轧制54%、70%和90%压下量的Cu-0.1Al合金在100℃保温1h后仍然保持轧制态组织,Cu-0.1Al合金的再结晶温度高于超高纯铜的再结晶温度;在200℃保温1h,随着变形量增加,试样的再结晶程度提高;在300℃保温1h,Cu-0.1Al合金处于完全再结晶状态,随着变形量的增加,试样的晶粒尺寸越小。交叉轧制54%、70%和90%压下量的超高纯铜和Cu-0.1Al合金在300℃保温1h,随着变形量的增加,晶粒的平均尺寸减小,特殊晶界的含量增高,晶粒的等轴性提高,织构的取向密度值降低。相比于单向轧制,交叉轧制的变形方式更有利于消除各向异性,生成随机织构。(3)在200℃保温不同时间,对交叉轧制70%压下量超高纯铜的平均晶粒尺寸、特殊晶界的含量、晶粒取向的影响较小,但保温2h更有利于消除试样的各向异性,形成弱织构状态。在450℃保温不同时间,对交叉轧制70%压下量Cu-0.1Al合金的平均晶粒尺寸与特殊晶界的含量影响较大,保温15min时晶粒的平均尺寸最小,小于30μm,但保温1h更有利于消除试样的各向异性,形成弱织构状态。
【Abstract】 With the rapid development of integrated circuits,higher requirements are put forward on the microstructure and texture of ultra-high-purity copper and copper-aluminum alloy sputtering targets,and the effects of different rolling methods and annealing processes on ultra-high-purity copper and copper-aluminum alloys are studied.The influence of microstructure and texture helps to improve the quality of sputtering targets.Based on this,this paper systematically studied the microstructure changes of ultra-high-purity copper and copper-aluminum alloy sheets with different rolling methods and different deformations through metallographic microscopy,X-ray diffraction,electron backscatter diffraction and other techniques,and the changes after different annealing processes.The evolution of recrystallized structure and texture after different annealing processes,the following conclusions are drawn through research:(1)The ultra-high purity copper samples with 90% unidirectional rolling deformation and 90% cross-rolling deformation have obvious dynamic recrystallization at room temperature.The former also has serious abnormal growth of grains,and both will have Cube texture formation;In the two rolling methods,the Cu-0.1Al alloy sample with 90% deformation has a lamellar rolled structure along the rolling direction,and the Brass texture is more obvious.The ultra-high purity copper with 54%,70% and90% unidirectional rolling deformations began to form recrystallized grains after holding at 100°C for 1 hour.The amount of deformation increased,the sample had more recrystallized grains,and the degree of recrystallization was higher;holding at 200℃for 1h,with the increase of deformation,the average grain size of the sample becomed smaller,and the content of special grain boundaries increased;holding at 300℃ for 1h,as the deformation increases,the grains were more prone to abnormal growth.(2)The Cu-0.1Al alloys with 54%,70% and 90% unidirectional rolling deformations still maintained the rolled structure after being held at 100°C for 1 hour.The recrystallization temperature of Cu-0.1Al alloy was higher than ultra-high purity copper: holding at 200℃ for 1h,with the increase of deformation,the degree of recrystallization of the sample increased;holding at 300°C for 1 hour,the Cu-0.1Al alloy was in a completely recrystallized state.As the amount of deformation increases,the grain size of the sample becomed smaller.The ultra-high purity copper and Cu-0.1Al alloy with 54%,70% and 90% cross-rolling deformation are kept at 300℃ for1 h,as the amount of deformation increasing,the average grain size decreased,and the content of special grain boundaries increased,The equiaxiality of the crystal grains was improved,and the orientation density value of the texture was reduced.Compared with unidirectional rolling,the deformation method of cross rolling was more conducive to eliminating anisotropy and generating random texture.(3)In the isothermal annealing experiment at 200℃ for the ultra-high purity copper with 70% cross-rolling deformation,different time had little effect on the average grain size,content of special grain boundaries,and grain orientation,but holding for 2 hours was more conducive to eliminating anisotropy of the sample and forming a weak texture state.In the isothermal annealing experiment at 450℃ for the Cu-0.1Al alloy with 70% cross-rolling deformation,different time had a greater influence on the average grain size and the content of special grain boundaries.The average grain size is the smallest when holding for 15 minutes,which is less than 30μm,but it is more important when holding for 1 hour,because it was helpful to eliminate the anisotropy of the sample and form a weak texture state.
【Key words】 Ultra-high purity copper; Copper-aluminum alloy; Rolling; Texture; Recrystallization;
- 【网络出版投稿人】 重庆大学 【网络出版年期】2022年 10期
- 【分类号】TG146.11;TN40
- 【下载频次】154