夏天,黄珂,郑宇亭,陈良贤,刘金龙,魏俊俊,李成明.磁控溅射铱薄膜的表面形态与取向演变的控制优化[J].表面技术,2023,52(3):338-344, 369.
XIA Tian,HAUNG Ke,ZHENG Yu-ting,CHEN Liang-xian,LIU Jin-long,WEI Jun-jun,LI Cheng-ming.Control and Optimization of Surface Morphology and Orientation Evolution of Iridium Films Prepared by Magnetron Sputtering[J].Surface Technology,2023,52(3):338-344, 369
磁控溅射铱薄膜的表面形态与取向演变的控制优化
Control and Optimization of Surface Morphology and Orientation Evolution of Iridium Films Prepared by Magnetron Sputtering
  
DOI:10.16490/j.cnki.issn.1001-3660.2023.03.031
中文关键词:  磁控溅射  功率  厚度  Ir膜  表面微结构  晶体质量
英文关键词:magnetronsputtering  power  thickness  Ir films  surface microstructure  crystal quality
基金项目:国家自然科学基金(11291211);北京市自然科学基金(08910109)
作者单位
夏天 北京科技大学 新材料技术研究院,北京 100083 
黄珂 北京科技大学 新材料技术研究院,北京 100083 
郑宇亭 北京科技大学 新材料技术研究院,北京 100083 
陈良贤 北京科技大学 新材料技术研究院,北京 100083 
刘金龙 北京科技大学 新材料技术研究院,北京 100083 
魏俊俊 北京科技大学 新材料技术研究院,北京 100083 
李成明 北京科技大学 新材料技术研究院,北京 100083 
AuthorInstitution
XIA Tian Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
HAUNG Ke Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
ZHENG Yu-ting Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
CHEN Liang-xian Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
LIU Jin-long Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
WEI Jun-jun Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
LI Cheng-ming Institute of Advanced Materials Technology, University of Science and Technology Beijing, Beijing 100083, China 
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中文摘要:
      目的 研究磁控溅射制备金属Ir膜的过程中溅射参数对Ir膜表面微结构和晶体质量的影响,制备高质量(100)取向的外延Ir膜,为单晶金刚石的异质外延生长奠定重要基础。方法 通过磁控溅射技术在单一改变参数(溅射功率、溅射厚度)的条件下制备金属Ir膜,通过分析原子力显微镜、扫描电子显微镜、X射线衍射、电子背散射衍射等测试结果,研究了各条件对所制备Ir膜粗糙度、表面形貌、晶体结构和取向的影响,并通过摇摆曲线衡量真空退火对薄膜晶体质量的优化效果。结果 在(100)MgO衬底上外延生长的Ir膜具有均匀的微结构,该结构由规则且紧密的矩形颗粒排列而成。薄膜表面微结构特征尺寸随溅射功率升高而逐渐减小;当功率为45 W时,Ir(200)X射线衍射峰强度最大、半高宽最宽;而随着厚度的增大,Ir(200)X射线衍射峰的半高宽及强度均增大。经优化的Ir膜表面光滑(Ra<0.5 nm)、薄膜晶体质量高(θFWHM<0.5°)。结论 功率、厚度和退火处理都会影响薄膜晶体质量和表面微结构尺寸,合适的功率和厚度结合退火处理能获得具有特定表面微结构的高质量Ir膜。
英文摘要:
      The preparation of high-quality Iridium films is an important step in the heteroepitaxy growth of single crystal diamond, it is self-evident that the irreplaceable role of Ir films in this area. To establish a solid foundation for the heteroepitaxy growth of single crystal diamond and prepare high quality (100) oriented Ir films, it is necessary to figure out the influence of sputtering parameters and annealing process on the quality of Ir films. The preparation of Ir films was based on RF magnetron sputtering, and single crystal (100) MgO with high crystal quality (θFWHM=0.045°) and smooth surface (Ra=0.016 nm) was used as substrate. This research was carried out as a single factor (power and thickness) experiment, when the power was studied, the range was set as 25 W, 45 W, 65 W, 85 W and 105 W, and when the thickness was studied, the range was set as 36 min, 48 min, 60 min, 72 min and 84 min, corresponding to the Ir films thickness of 150 nm, 200 nm, 250 nm, 300 nm and 350 nm, respectively. And the samples were characterized by atomic force microscopy, scanning electron microscopy, X-ray diffraction and electron back scattering diffraction, the influence of parameters on roughness, surface morphology, crystal structure and orientation was analyzed. The annealing experiment was based on vacuum annealing furnace, this experiment was carried out as a before-after experiment in the same sample. The Ir films 200 nm and 350 nm thick were used as blank space group in this experiment, and the films were set as experimental group after the characterization step. And then the Ir films of experimental group were adopted vacuum annealing treatment at 950 ℃ for 1 h. The effect of vacuum annealing treatment on the crystal quality of Ir films was analyzed by rocking curve. The Ir films grown on (100) MgO substrate had a uniform microstructure, which was composed of regular and closely arranged rectangular particles. As the power increased, the characteristic size of microstructure on the surface of Ir films gradually decreased. The films with narrowest FWHM and strongest Ir(200) peak were obtained at 45 W,too high or too low power would degrade the crystalline quality of the Ir films; the FWHM and intensity of Ir films increased with the increasement of thickness, the main reason for this phenomenon was the enhanced crystallinity of the Ir films, although the upper Ir films shielding substrate signals also contributed, but this part was eliminated by normalization of XRD patterns, the effect of Ir films thickness on the roughness and grain size was very limited. After annealing process, as was shown in the rocking curve patterns, the Ir(200) peak strength of rocking curve was enhanced and the FWHM was reduced, the crystal quality is obviously optimized. Eventually the high quality (θFWHM<0.5°) Ir films obtain smooth surface (Ra<0.5 nm) and highly preferred orientation. Power、thickness and annealing treatment can affect crystal quality and the size of microstructure. High quality Ir films with specific surface microstructure can be obtained by appropriate power and thickness combined with annealing treatment.
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