智能激光防护材料：氧化钒薄膜的生长及其光电性能研究
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摘要
随着激光武器的迅猛发展,寻找一种适用于激光防护领域的新型材料,有效对抗激光致盲武器,保护单兵及军用装备中的光学探测器及其光学系统不受敌方的毁灭性打击,这对于各国军事技术研究者来说,已成为急需解决的重要问题。
氧化钒作为一种性能优异的功能材料,在一定相变温度附近发生从低温半导体相到高温金属相的突变。基于氧化钒薄膜在相变过程中光电特性的突变,氧化钒薄膜在热电开关、激光防护和温控装置等方面应用前景广阔。但由于钒氧体系的复杂性和纯V02和纯V205薄膜相变温度较高等关键问题尚没有完全解决,严重阻碍了氧化钒薄膜的实际应用。
本文采用直流磁控溅射法在玻璃衬底上生长了非晶态V205薄膜,样品经一定温度区间的O2氛围退火后,开始生成β相V205纳米棒。通过扫描电子显微镜(SEM)、 X射线衍射(XRD)、自制电阻-温度装置、MAYA2000PRO型光谱仪等表征手段,研究了退火温度对生长β相V205纳米棒的晶体结构、光学和电学性质的影响规律。实验表明,在一个狭窄温度范围内,V205纳米棒光电性能呈现出温度敏感特性；室温下,所制样品在紫外及近紫外线波长范围具有很高的吸收率,在近红外线波长范围具有较高的透射率；其中,经500℃热处理的样品,高低温电阻变化了2个数量级,相变温度出现在350℃左右。
同时,综述了氧化钒薄膜多种制备方法的原理,优缺点以及通过元素掺杂调控氧化钒薄膜相变和光电性能方面的最新进展,并重点介绍了氧化钒薄膜在智能激光防护武器上的应用。
With the rapid development of laser weapons, looking for new materials in the field of laser protective effective against blinding laser weapons, to protect the optical detector and optical system of individual soldiers and military equipment from the devastating blow, has becomeplaced in the national military technology researchers in front of the very real problem.
As a high performance intelligent material, Vanadium oxide has a reversible transition from low-temperature semiconductor phase to high-temperature metal phase at certain phase-transition, accompanied by an abrupt change in photoelectric characteristic. Therefore, Vanadium oxide has great potential for the application in laser protection, thermoelectric switch, etc. While its practical application is blocked seriously by the problems like the complication of material system and high phase transition temperature of pure vanadium oxide.
In this paper, amorphous V2O5thin films were deposited on glass substrates by reactive dc magnetron sputtering. After the annealing treatment under certain temperature range of O2atmosphere, the P-phase V2O5nanorods were synthesized. The effect of temperature on crystal structure and optoelectronic properties of β-phase V2O5nanorods was studied by SEM, XRD, self-made resistance-temperature measurement system and so on. The result indicates that V2O5nanorods have high temperature sensitive characteristic within a narrow temperature range. In room temperature, the sample shows high absorptivity in the ultraviolet and the near-ultraviolet region, as well as high transmittance in near infrared region. The sample annealed in500°C caused two orders of magnitude in high and low resistance, and the phase-transition temperature was about350°C.
At the same time, the representative preparation methods and their merit and demerit are reviewed in this paper, with an emphasis on the application prospect of vanadium oxide thin film in intelligent laser protection weapons. The effects of different doping methods and different impurity upon the phase transitions, temperature hysteresis, optical and electrical properties are also summarized.
氧化钒作为一种性能优异的功能材料,在一定相变温度附近发生从低温半导体相到高温金属相的突变。基于氧化钒薄膜在相变过程中光电特性的突变,氧化钒薄膜在热电开关、激光防护和温控装置等方面应用前景广阔。但由于钒氧体系的复杂性和纯V02和纯V205薄膜相变温度较高等关键问题尚没有完全解决,严重阻碍了氧化钒薄膜的实际应用。
本文采用直流磁控溅射法在玻璃衬底上生长了非晶态V205薄膜,样品经一定温度区间的O2氛围退火后,开始生成β相V205纳米棒。通过扫描电子显微镜(SEM)、 X射线衍射(XRD)、自制电阻-温度装置、MAYA2000PRO型光谱仪等表征手段,研究了退火温度对生长β相V205纳米棒的晶体结构、光学和电学性质的影响规律。实验表明,在一个狭窄温度范围内,V205纳米棒光电性能呈现出温度敏感特性；室温下,所制样品在紫外及近紫外线波长范围具有很高的吸收率,在近红外线波长范围具有较高的透射率；其中,经500℃热处理的样品,高低温电阻变化了2个数量级,相变温度出现在350℃左右。
同时,综述了氧化钒薄膜多种制备方法的原理,优缺点以及通过元素掺杂调控氧化钒薄膜相变和光电性能方面的最新进展,并重点介绍了氧化钒薄膜在智能激光防护武器上的应用。
With the rapid development of laser weapons, looking for new materials in the field of laser protective effective against blinding laser weapons, to protect the optical detector and optical system of individual soldiers and military equipment from the devastating blow, has becomeplaced in the national military technology researchers in front of the very real problem.
As a high performance intelligent material, Vanadium oxide has a reversible transition from low-temperature semiconductor phase to high-temperature metal phase at certain phase-transition, accompanied by an abrupt change in photoelectric characteristic. Therefore, Vanadium oxide has great potential for the application in laser protection, thermoelectric switch, etc. While its practical application is blocked seriously by the problems like the complication of material system and high phase transition temperature of pure vanadium oxide.
In this paper, amorphous V2O5thin films were deposited on glass substrates by reactive dc magnetron sputtering. After the annealing treatment under certain temperature range of O2atmosphere, the P-phase V2O5nanorods were synthesized. The effect of temperature on crystal structure and optoelectronic properties of β-phase V2O5nanorods was studied by SEM, XRD, self-made resistance-temperature measurement system and so on. The result indicates that V2O5nanorods have high temperature sensitive characteristic within a narrow temperature range. In room temperature, the sample shows high absorptivity in the ultraviolet and the near-ultraviolet region, as well as high transmittance in near infrared region. The sample annealed in500°C caused two orders of magnitude in high and low resistance, and the phase-transition temperature was about350°C.
At the same time, the representative preparation methods and their merit and demerit are reviewed in this paper, with an emphasis on the application prospect of vanadium oxide thin film in intelligent laser protection weapons. The effects of different doping methods and different impurity upon the phase transitions, temperature hysteresis, optical and electrical properties are also summarized.
引文
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[4]Cui J Z,Da D,et al. Structure characterization of vanadium oxide thin films prepared by magnetronsputtering methods [J]. Applied Structure Science,1998,133:225-229.
[5]Morin F J. Oxides which show a metal-toinsulator transition at the neel temperature[J]. Phy. Rev. Lett.,1959,3 (1):34-36.
[6]Gui Z, Chen X H, et al.A new metastable phase of needle-like nanocrystalline VO2 ? H20 and phase transf ormat ion [J]. Journal of Solid State Chemistry,2001,157:250-254.
[7]Schlag H J, Scherber W. New sputter process for V02 thin films and examination with MIS-elements and C-V-measurements [J]. Thin Solid Films,2000,366:28-31.
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[9]陈长琦,朱武,等.二氧化钒薄膜制备及其相变机理研究分析[J].真空科学与技术,2001,21(6)：452-456.
[10]刘金城,鲁建业,等.磁控溅射法制备二氧化钒薄膜最佳参量的研究[J].光子学报,2003,23(1)：65-67.
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[12]Lampert C M. Large-area smart glass and integrated photovoltaics[J]. Solar Energy Materials and Solar Cells,2003,76 (4):489-499.
[13]骆永全,王伟平,罗飞V2O5薄膜在连续激光防护中的应用研究[J].应用激光,2005,25(6)：381-383.
[14]Su Q, Pan X J, Xie E Q,et al.Influence of Temperature on the Microstructure of V2O5 Film Prepared By DC Magnetron Sputtering[J]. RareMaters,2006,25 (6):82-87.
[l5]Gui Z, Chen X H, Chen X H, et al. A new metastable phase of needle-like nanocrystalline VO2 ? H2O and phase transformation[J]. Journal of Solid State Chemistry,2001,157:250-254.
[16]Schlag H J,Scherber W. New sputter process for V02 thin films and examination with MIS-elements and C-V-measurements [J]. Thin Solid Films,2000,366:28-31.
[17]Zou C W, Yan X D.Patterson D A, et al. Temperature sensitive crystallization of V2O5: from amorphous film to β-V2O5 nanorods[J]. Crystal Engineering Communications,2010,12,691-693.
[18]Chain E E. Optical Properties of Vanadium Dioxide and Vanadium Pentoxide Thin Films[J]. Applied Optics,1991,30 (19):2782-2787.
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