二氧化钒薄膜制备及掺Au对其相变性能影响的研究
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摘要
摘要：二氧化钒是一种典型的热致相变化合物。随着温度的升高,在68℃时,二氧化钒会由低温半导体态转变为高温金属态(可逆),伴随着这一相变的发生,二氧化钒的电学,光学性质也发生突变。这一特殊的性质使得二氧化钒在很多领域有着重要的应用价值,如热敏电阻材料,光致开关材料,智能玻璃窗涂层,太阳能温控装置等；最重要的是通过掺杂可以改变它的相变温度。二氧化钒作为一种功能型材料,具有很高的研究价值。本文主要探索了用射频磁控溅射制备二氧化钒薄膜的条件以及掺杂Au阵列后对二氧化钒薄膜性质的影响。
本文用射频磁控溅射在玻璃和蓝宝石衬底上制备二氧化钒薄膜。用四探针法测得相变前后电阻变化均达到两个数量级以上；用高紫外灵敏度光谱仪进行透射率-温度的研究,在1100nm波长处,测得玻璃衬底上的透射率随着温度升高由35%减小到15%,降幅到达了20%,总结得出红外波段透射率随温度变化远远大于可见光波段,接近文献报道的最好水平。
本文还对二氧化钒薄膜进行Au掺杂：采用直接溅射掺杂和纳米刻蚀掺杂两种方法。其中刻蚀法的过程：利用滴点法制备出了聚苯乙烯胶体球掩膜板,在掩膜板上溅射Au,再除去聚苯乙烯小球后得到纳米Au六方点阵列,在Au阵列上沉积二氧化钒薄膜。两种方法掺Au都降低了二氧化钒的相变温度,尤其是刻蚀掺Au法,使得二氧化钒的相变温度降低至37-45℃之间,最大的降幅达到30度；光学透过率降幅达10%。
此外,对制备出的薄膜还进行了XRD, AFM和SEM表征,分析不同生长条件对二氧化钒的影响。
ABSTRACT:Vanadium dioxide (VO2)is a typical thermochromical compound. With the rise of temperature, it has Low temperature semiconductor-to-high temperature metal transition at 68℃(reversible), the phase-transition is accompanied with abrupt changes in its electrical and optical properties. This special properties make VO2 in many fields has important application value, for example, it can use as thermistor materials, optical switches, smart windows, solar temperature-control devices and so on, the important is that its transition temperature can be adjusted through doping. As a special function material, it has high value for study. This paper reported that the VO2 thin films were prepared by radio frequency reactive magnetron sputtering and optical and electrical properties of which VO2 thin films doped with Au and Au array were studied.
In this paper, VO2 thin films were fabricated on the plain glass substrates and sapphire substrates by magnetron sputtering method. The curve of resistance-temperature were determined using four-point probe method; the film's resistance changed about two orders of magnitude at the transition temperature on both of glass substrates and sapphire substrates. Transmittance spectrums were measured by high UV sensitivity spectrometer in varied temperature. At 1100nm wavelengths, with the temperature rise the transmittance reduces from 35% to 15%, 20% off on the glass substrates. We found that the variation of the rate in the infrared is more obviously than in the visible light, this result approaches with the best in references.
Other work of this paper, Au was doped into VO2 thin films using direct sputtering and nanosphere lithography (NSL) method, respectively. In the nano-etching method:Firstly, polystyrene colloid ball mask was prepared using drop point method; secondly, Au was sputtered on the mask board; thirdly, hexagonal Au nano-point array was obtained after removing polystyrene ball; finally, VO2 thin films was sputtered on the Au hexagonal nano-point array and Au:VO2 composite films was obtained. Both of methods reduced the phase-transition temperature, especially nano-etching method, using this method the film's phase-transition temperature has reduced from 68℃to between 37-45℃, the largest decreasing amplitude to 30℃The transmittance amplitude decreases 10%.
Synchronously, we analysis the films by XRD, AFM and SEM, learn the film's physical properties under different growth conditions.
本文用射频磁控溅射在玻璃和蓝宝石衬底上制备二氧化钒薄膜。用四探针法测得相变前后电阻变化均达到两个数量级以上；用高紫外灵敏度光谱仪进行透射率-温度的研究,在1100nm波长处,测得玻璃衬底上的透射率随着温度升高由35%减小到15%,降幅到达了20%,总结得出红外波段透射率随温度变化远远大于可见光波段,接近文献报道的最好水平。
本文还对二氧化钒薄膜进行Au掺杂：采用直接溅射掺杂和纳米刻蚀掺杂两种方法。其中刻蚀法的过程：利用滴点法制备出了聚苯乙烯胶体球掩膜板,在掩膜板上溅射Au,再除去聚苯乙烯小球后得到纳米Au六方点阵列,在Au阵列上沉积二氧化钒薄膜。两种方法掺Au都降低了二氧化钒的相变温度,尤其是刻蚀掺Au法,使得二氧化钒的相变温度降低至37-45℃之间,最大的降幅达到30度；光学透过率降幅达10%。
此外,对制备出的薄膜还进行了XRD, AFM和SEM表征,分析不同生长条件对二氧化钒的影响。
ABSTRACT:Vanadium dioxide (VO2)is a typical thermochromical compound. With the rise of temperature, it has Low temperature semiconductor-to-high temperature metal transition at 68℃(reversible), the phase-transition is accompanied with abrupt changes in its electrical and optical properties. This special properties make VO2 in many fields has important application value, for example, it can use as thermistor materials, optical switches, smart windows, solar temperature-control devices and so on, the important is that its transition temperature can be adjusted through doping. As a special function material, it has high value for study. This paper reported that the VO2 thin films were prepared by radio frequency reactive magnetron sputtering and optical and electrical properties of which VO2 thin films doped with Au and Au array were studied.
In this paper, VO2 thin films were fabricated on the plain glass substrates and sapphire substrates by magnetron sputtering method. The curve of resistance-temperature were determined using four-point probe method; the film's resistance changed about two orders of magnitude at the transition temperature on both of glass substrates and sapphire substrates. Transmittance spectrums were measured by high UV sensitivity spectrometer in varied temperature. At 1100nm wavelengths, with the temperature rise the transmittance reduces from 35% to 15%, 20% off on the glass substrates. We found that the variation of the rate in the infrared is more obviously than in the visible light, this result approaches with the best in references.
Other work of this paper, Au was doped into VO2 thin films using direct sputtering and nanosphere lithography (NSL) method, respectively. In the nano-etching method:Firstly, polystyrene colloid ball mask was prepared using drop point method; secondly, Au was sputtered on the mask board; thirdly, hexagonal Au nano-point array was obtained after removing polystyrene ball; finally, VO2 thin films was sputtered on the Au hexagonal nano-point array and Au:VO2 composite films was obtained. Both of methods reduced the phase-transition temperature, especially nano-etching method, using this method the film's phase-transition temperature has reduced from 68℃to between 37-45℃, the largest decreasing amplitude to 30℃The transmittance amplitude decreases 10%.
Synchronously, we analysis the films by XRD, AFM and SEM, learn the film's physical properties under different growth conditions.
引文
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[10]P.哈森,材料的相变[M].,北京：科学出版社,1998.
[11]Christrmann T.,Felde B.,Niessner W.,et al,Themachromic VO2 thin films studied by photoelectron spectroscopy[J],Thin solid films,1996,287:134-138.
[12]Michael F.Becker,A.Bruce Buckman, Rodger M. Walser.Femtosecond laser excitation of the semiconductor-metal phase transition in VO2 [J].Appl. Phys. Lett.1994,65(12):1507-1512
[13]Y Muraoka.Y Ueda.Z Hiroi.Large modification of the metal-insulator transition temperature in strained VO2 films grown on TiO2 substrates[J].Journal of Physics and Chemistry of Solids.2002.63:965-967.
[14]Mark Borek.F Qian.V Nagabushman and R K Singh.Pulsed laser deposition of oriented VO2 thin films on R-cut sapphire substrates[J].Appl.Phys.Lett..1993.63(24):3288-3290.
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[16]卢勇.林理彬.真空还原制备的V02热致相变薄膜Raman光谱和红外光谱研究[J].功能材料.2001.32(6)：657-659.
[17]袁宁一.李金华.林成鲁.氧化钒薄膜的结构、性能及制备技术的相关性[J].功能材料.2001.32(6)：572-575.
[18]JIN Ping. A NoveL Multifunctional Smart Window with VO2 and TiO2 Coatings[J]. Journal of Shaanxi University of Science & Technology,2004,22(5):1-7.
[19]P Jin. S Nakao. S Tanemura. T Bell. Characterization of mechanical properties of VO2 thin films on sapphire and silicon by ultra-microindentation [J]. Thin Solid Films.1999. (343-344):134-137.
[20]Fabien Beteille,Leo Mazerolles.Microstructure and metal2insulation transition of VO2 thin films.[J].Materials Research Bulletin,1999,34:2177-2184.
[21]Fulong Tang, Fuxi Gan, Congshan Zhu. Dye-doped optical storage films prepared by the sol-gel process[]. SPIE,1994,2288:350-355.
[22]A. S. Grenishin, V. M. Kiselev, L. I. Krutova et al. Crystalline passive shutter for iodine lasers [J]. SPIE,1994,2095:180-183
[23]David W. Blodgett, Michael J. Elko, Philip J. McNally. Improved vanadium-dioxide-based infrared spatial light modulator[J]. SPIE,1994,2223:63-74.
[24]SoltaniM,ChakerM,HaddadE,etal.1×2opticalswitch devicesbased on semiconductor-to-Metallicphasertransition characteristics of VO2 smart coatings[J].Measurement Science and Technology,2006,(17):1052.
[25]Chen S,etal.A novelstructural VO2 micro-optical switch[J].Optical and Quantum Electronics,2003,(35):1351.
[26]宁永刚,孙晓泉.二氧化钒薄膜在激光防护上的应用研究[J].红外与激光工程,2005,34(5)：53.
[27]李世涛,乔学亮,陈建国等.卫星多功能激光防护膜层的研究[J].激光杂志,2005,26(4)：9-10.
[28]孟献丰,陆春华,张其土等.激光防护材料的研究进展[J].激光与红外,2005,35(2)：71-73.
[29]刘大军,何兴权,段潜,等.激光防护材料的研究现状[J].激光杂志,2002,23(6)：5-6.
[30]Sihai Chen, Hong Ma, Xinjian Yi,et al.Smart VO2 thin film for protection of sensitive infrared detectors from strong laser radiation[J].Sensors and Actuators A:Physical,2004, 115(1):28-31.
[31]付伟.激光防护技术及其发展现状[J].航天电子对抗,2002(1)：43.
[32]Lee M H.[J].Solar Energy Mater and Solar Cells,2002,71:537-540.
[33]Michael A. Todd, Paul P. Donohue, Rex Watton et al. High-performance ferroelectric and magnetoresistive materials for next-generation thennal detector arrays[J]. SPIE,2002,4795: 88-99.
[34]R. T. Rajendra Kumar, B. Karunagaran, D. Mangalaraj et al. Room-temperature IR detection using pulsed laser deposited vanadium oxide bolometer[J]. SPIE,2003,5092:425-432.
[35]VERKELIS J, BLIZNIKAS Z, BREIVE K. Vanadium oxides thin films and fixed temperature heat sensor with memory [J].Sensors and Actuators,1998, A68:338-343.
[36]HERRING R J, HOWARD P E. Design and performance of the ultra 320×240 uncooled focal plane array and sensor [J]. SPIE,1996,2746:2-12.
[37]陈长琦,方应翠,朱武,等.二氧化钒相变分析及应用[J].真空,2001,6：9.
[38]KannanA M, M anthiram A. etal. Synthesisand electro—chemicalevaluation ofhigh capacity nanostructured VO2 cathodes[J].SlidStateIonies,2003,159(3-4):265.
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