射频磁控反应溅射法制备HfO_2薄膜的研究
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摘要
金刚石具有高红外透过率、低吸收系数、抗热冲击性好、耐磨擦等一系列优异的性能，是用于长波红外波段(8～12μm)理想的窗口和头罩材料。然而金刚石在750℃以上时很容易发生氧化，导致透过率急剧下降。在金刚石表面镀制抗氧化增透涂层可以满足其在高速、高温条件下应用。氧化铪(HfO_2)具有优良的物理、化学性能，抗高温氧化能力强，可用作金刚石抗氧化保护涂层。在国外，HfO_2用作金刚石抗氧化涂层的研究已经展开，并取得进展；在国内，有关HfO_2抗氧化保护涂层的研究还未见报道。本文主要研究射频磁控溅射法制备HfO 2薄膜的工艺对其成分、结构、光学特性及沉积速率的影响规律，为将HfO_2用作金刚石红外增透及抗氧化膜系奠定基础。主要研究工作及结果如下：
利用OPFCAD软件在金刚石衬底上设计了HfO_2//Diamond和HfO_2/a-Si：H//Diamond增透膜系，并对所设计的膜系进行了结构敏感因子及结构偏差分析。膜系设计结果表明，在金刚石双面镀两种膜系后在长波红外波段的红外透过率均大于85％，可满足高速红外窗口和头罩使用要求。
研究了主要工艺参数对HfO_2薄膜沉积速率的影响，对工艺参数进行了优化。试验结果表明，HfO_2薄膜的沉积速率随溅射功率增大而增大，随气体压强和O_2流量增大而减小，衬底温度对沉积速率无明显影响。正交试验结果表明O_2流量对沉积速率的影响最大，并确定了获得薄膜最大沉积速率的工艺参数。
对制备的HfO_2薄膜进行了X射线光电子谱(XPS)、X射线衍射(XRD)和椭圆偏振光谱(SE)分析。结果表明，沉积态薄膜中Hf和O原子结合形成了HfO_2化合物；薄膜中Hf和O元素的原子百分比基本符合HfO_2的化学计量比；沉积态薄膜中HfO_2为单斜相，主要以多晶状态存在；在椭偏光谱分析范围(0.4～1.8μm)，HfO_2薄膜的折射率随波长的增大而快速下降，波长大于1.2μm后趋于稳定值1.95，而且薄膜的吸收很小。
Diamond has excellent properties such as good transmittance in the infrared wave band, low absorption coefficient, high resistance to thermal shock and friction. So diamond is an ideal material for airborne LWIR (8-12μm) windows and domes. However, diamond is easily subject to oxidation in air at temperatures greater than 750℃, and the optical transmittance is degraded greatly. It's useful to prepare anti-oxidation and anti-reflective films on the diamond surface to meet the need for applications of high-speed or high temperature environment. Hafnium oxide (HfO_2) is a promising anti-oxidation material with good physical, chemical properties and good anti-oxidation property. Some progress has been made in the researches about HfO_2 anti-oxidation films overseas. But no domestic work has been done on HfO_2 optical and protective films. Researches of the paper mostly concentrate on preparation of HfO_2 films by magnetron sputtering and the functions of experiment parameters on films components, structure, optical properties and deposition rate. The main contents and results are listed as follows:
HfO_2/Diamond and HfO_2/a-Si:H//Diamond antireflection film systems are designed by OPFCAD, and the sensitive factors and deviation of the films' structure are analyzed. Results show that the average transmittance in LWIR waveband can exceed 85% after both films systems are deposited on the surfaces of diamond, which can meet the requirements high-speed infrared windows and domes.
The influence of main parameters on deposition rate is discussed, and the main parameters are optimized. The results show that deposition rate of films increases with the sputtering power increasing, and decreases with sputtering pressure and O_2 flux increasing, and deposition rate is insensitive to growth temperature. The orthogonal experiment results show that the effect of O_2 flux on the deposition rates is the most significant, and the parameters to get high deposition rate are decided. XPS and XRD analyses as well as SE transmission spectrum tests are carried out.
利用OPFCAD软件在金刚石衬底上设计了HfO_2//Diamond和HfO_2/a-Si：H//Diamond增透膜系，并对所设计的膜系进行了结构敏感因子及结构偏差分析。膜系设计结果表明，在金刚石双面镀两种膜系后在长波红外波段的红外透过率均大于85％，可满足高速红外窗口和头罩使用要求。
研究了主要工艺参数对HfO_2薄膜沉积速率的影响，对工艺参数进行了优化。试验结果表明，HfO_2薄膜的沉积速率随溅射功率增大而增大，随气体压强和O_2流量增大而减小，衬底温度对沉积速率无明显影响。正交试验结果表明O_2流量对沉积速率的影响最大，并确定了获得薄膜最大沉积速率的工艺参数。
对制备的HfO_2薄膜进行了X射线光电子谱(XPS)、X射线衍射(XRD)和椭圆偏振光谱(SE)分析。结果表明，沉积态薄膜中Hf和O原子结合形成了HfO_2化合物；薄膜中Hf和O元素的原子百分比基本符合HfO_2的化学计量比；沉积态薄膜中HfO_2为单斜相，主要以多晶状态存在；在椭偏光谱分析范围(0.4～1.8μm)，HfO_2薄膜的折射率随波长的增大而快速下降，波长大于1.2μm后趋于稳定值1.95，而且薄膜的吸收很小。
Diamond has excellent properties such as good transmittance in the infrared wave band, low absorption coefficient, high resistance to thermal shock and friction. So diamond is an ideal material for airborne LWIR (8-12μm) windows and domes. However, diamond is easily subject to oxidation in air at temperatures greater than 750℃, and the optical transmittance is degraded greatly. It's useful to prepare anti-oxidation and anti-reflective films on the diamond surface to meet the need for applications of high-speed or high temperature environment. Hafnium oxide (HfO_2) is a promising anti-oxidation material with good physical, chemical properties and good anti-oxidation property. Some progress has been made in the researches about HfO_2 anti-oxidation films overseas. But no domestic work has been done on HfO_2 optical and protective films. Researches of the paper mostly concentrate on preparation of HfO_2 films by magnetron sputtering and the functions of experiment parameters on films components, structure, optical properties and deposition rate. The main contents and results are listed as follows:
HfO_2/Diamond and HfO_2/a-Si:H//Diamond antireflection film systems are designed by OPFCAD, and the sensitive factors and deviation of the films' structure are analyzed. Results show that the average transmittance in LWIR waveband can exceed 85% after both films systems are deposited on the surfaces of diamond, which can meet the requirements high-speed infrared windows and domes.
The influence of main parameters on deposition rate is discussed, and the main parameters are optimized. The results show that deposition rate of films increases with the sputtering power increasing, and decreases with sputtering pressure and O_2 flux increasing, and deposition rate is insensitive to growth temperature. The orthogonal experiment results show that the effect of O_2 flux on the deposition rates is the most significant, and the parameters to get high deposition rate are decided. XPS and XRD analyses as well as SE transmission spectrum tests are carried out.
引文
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2．梅遂生，杨家德．光电子技术．北京：国防工业出版社，1999，85
3．张贵峰．新型红外增透膜与保护膜．红外技术，1995．17(5)：23
4．阎锋：射频磁控反应溅射法制备Y_2O_3薄膜的研究．硕士学位论文，西北工业大学，2006
5. Tim P Mollart, The development of CVD infrared optics from planar windows to missile domes. Proc. SPIE, Vol. 5078, 2003: 127～136
6．彭鸿雁，赵立新．类金刚石膜的制备、性能与应用．北京：科学出版社，2004
7. R . Korenstein, P. Cremin, T. E. Varitimos, et al. Optical Properties of Durable Oxide Coatings for Infrared Applications. SPIE, 2003, 5078: 169～178
8．陈光华，张阳等．金刚石薄膜的制备与应用．北京：化学工业出版社，2004
9. T.P. Mollart, K. L. Lewis. Transition metal oxide anti-reflection coatings for airborne diamond optics. Diamond and Related Materials. 2001, (10): 536～541
10. K. Tankala et al. Oxidation of diamond films synthesized by hot filament assisted chemical vapour deposition. J. Mater. Res, 1990, 5: 2483～2489
11. M. Alam et al. The kinetics of chemical vapour deposited diamond-oxygen reaction. J. Mater. Res ,1993, 8:2870～2878
12. C A Klein et al. Critical-point phonon frequencies of diamond. Phys Rev B45,1992, 22:12854～12862
13. Chang Q Sun et al. Preferential oxidation of diamond {111}. J. Phys. D: Appl. Phys, 2000, 33:2196～2199
14. Jane Yuan Howe. The Oxidation of Diamond.Thesis for Doctor Degree. New York: Alfred university, 2001
15. Sun C Q. A model of bonding and band-forming for oxides and nitrides. Appl. Phys. Lett,1998,72:1706～1708
16. P. John et al. The Oxidation of (100) Textured Diamond. Diamond and Related Materials, 2002, 11:861～866
17. K. P. Loh et al. Surface oxygenation studies on (100)-oriented diamond using an atom beam source and local anodic oxidation. Surface Science, 2002, 505:93～114
18. Chen J et al. Graphitization of nano diamond powder annealed in argon ambient. Appl. Phys. Lett, 1999, 74:3651～3653
19. A.B.Harker and J.F.DeNatale, "Diamond Gradient Index 'Moth-Eye' Antireflection Surfaces for LWIR Windows, "proc. SPIE, 1992: 1760, 261-267
20. Douglas S. Hobbs, Bruce D. MacLeod. Design, Fabrication, and Measured Performance of Anti-Reflecting Surface Textures in Infrared Transmitting Materials. SPIE, 2005, 5786: 349-364
21. GrANNEN K J, TSU D V, MELIUNAS R J, et al. Oxidation studies of fluorine containing diamond films. Applied Physics Letters, 1991, 59(6): 745-747
22. Miyata K, Kobashi K. Air oxidation of undoped and B-doped polycrystalline diamond films at high temperature. Journal of Material Research, 1996, 11: 296-305
23. Kirkpatrick et al. Method of Protective Surfaces on Diamond, Diamondlike Carbon or Carbon .US patent. No. 5855967. Jan.5,1999
24. S.P.McGeoch E.M.Waddell et al. Aluminum Nitride Coatings for Protection of Diamond at High Temperature in Air. Proc. SPIE 1999, 3705: 163—169
25. 乔保卫,刘正堂.金刚石抗氧化光学涂层的研究进展.材料工程, 2004,8: 54-56
26. T P Mollart, K L lewis, CJK Wort and CSJ Pickles. Coating Technology for CVD diamond Optics. Window and Dome Technologies and Materials VII.SPIE, 2001: 4375: 199-205
27. T P Mollart, K L Lewis. Transition metal oxide anti-reflection coatings for airborne diamond optics. Diamond and Related Materials, 2001, 10:536-541
28. http://www.webelements.com/webelements/elements/text/Hf/key.html
29. C.T. Kuo, R. Kwor. Study of sputtered HfO_2 thin films on silicon. Thin Solid Films. 1992,213:257-264
30. Hei Wong, Hiroshi Iwai. On the scaling issues and high-j replacement of ultrathin gate dielectrics for nanoscale MOS transistors. Microelectronic Engineering, 83(2006): 1867-1904
31. Yongjin Wang, Zhilang Lin, Xinli Cheng et al. Study of HfO_2 thin films prepared by electron beam evaporation. Applied Surface Science 228(2004):93-99
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