基于透射光谱确定溶胶凝胶ZrO2薄膜的光学常数

基于溶胶凝胶ZrO2薄膜的紫外/可见/近红外透射实验光谱,采用Swanepoel方法结合Wemple-DiDomenico色散模型,方便地导出了ZrO2薄膜在200-1200 nm波长范围内的光学常数,包括折射率、色散常数、膜层厚度、吸收系数及能量带隙.研究发现,溶胶凝胶ZrO2薄膜具有高折射率(1.63-1.93,测试波长为632.8 nm)、低吸收和直接能量带隙(4.97-5.63 eV) 等光学特性,而且其光学常数对薄膜制备过程中的重要工艺参数--膜层后处理温度表现出强烈的依赖性.此外,在膜层的弱吸收和中等吸收光谱区域内,计算得到的折射率色散曲线与分光光度法的测试结果基本符合,说明本实验中所建立的计算方法在确定溶胶凝胶ZrO2薄膜光学常数方面的可靠性.     

基于透射光谱确定溅射Al2O3薄膜的光学（已撤稿）

基于反应磁控溅射Al₂O₃薄膜的紫外—可见—近红外透射实验光谱,采用Swanepoel方法结合Wemple-DiDomenico色散模型,方便地导出了Al₂O₃薄膜在200—1100 nm波长范围内的光学常数,包括折射率、色散常数、膜层厚度、吸收系数及能量带隙.研究发现反应磁控溅射Al₂O₃薄膜具有高折射率(1.556— 1.76,测试波长为550 nm)、低吸收和直接能量带隙(3.91—4.20 eV)等光学特性,而且其光学常数对薄膜制备过程中的重要工艺参数——膜层后处理温度表现出强烈的依赖性.此外,在膜层的弱吸收和中等吸收光谱区域内,计算得到的折射率色散曲线与分光光度法的测试结果基本符合,说明本实验中所建立的计算方法在确定反应磁控溅射Al₂O₃薄膜光学常数方面的可靠性. 关键词： 光学常数 Swanepoel方法 2O₃薄膜')" href="#">Al₂O₃薄膜 热处理     

椭偏光谱法研究溶胶-凝胶TiO2薄膜的光学常数

以钛酸丁酯为前驱体,采用溶胶-凝胶工艺成功制备了TiO₂薄膜.利用反射式椭圆偏振光谱仪测量了薄膜的椭偏参量Ψ和Δ,并用Cauchy模型对椭偏参数进行数据拟合,得到了薄膜的厚度和光学常数在380—800 nm的色散关系.用分光光度计测量了薄膜的反射率,并用干涉法计算薄膜的厚度;使用原子力显微镜观测了薄膜的表面微结构,分析讨论了不同退火温度处理的薄膜微结构与光学常数之间的关系.研究结果表明,Cauchy模型能较好地符合溶胶-凝胶TiO₂薄 关键词： 光学常数 2薄膜')" href="#">TiO₂薄膜 溶胶-凝胶 椭圆偏振     

利用透射光谱与X射线反射谱精确测量溶胶-凝胶TiO2薄膜厚度和光学常数

在洁净K9玻璃基底上沉积TiO2薄膜,将透射光谱和X射线反射光谱相结合分析获得膜层的厚度和光学常数。X射线反射谱拟合能精确得到膜层的厚度、电子密度及表面和界面粗糙度,其中膜层厚度的数值为透射光谱的分析提供了重要参考。基于Forouhi-Bloomer色散模型拟合膜层透射光谱,得到薄膜折射率和消光系数,理论曲线和实验曲线吻合良好。对于同一样品,两种光谱拟合分析得到的厚度数值非常接近,差值最大为4.9nm,说明两种方法的结合能够提高光学分析结果的可靠性。     

溶胶-凝胶ZrO2-TiO2高折射率光学膜层的抗激光损伤性能研究

采用溶胶-凝胶方法制备了ZrO₂-TiO₂(Ti含量为0—100mol%)高折射率光学薄膜. 借助激光动态光散射技术研究溶胶微结构. 采用傅里叶变换红外光谱、原子力显微镜、薄膜光学常数分析仪、漫反射吸收光谱及强激光辐照实验，对膜层的结构、光学性能及抗激光损伤性能进行了系统表征. 结果显示，溶胶-凝胶工艺可以在部分牺牲折射率的情况下，使膜层的抗激光损伤性能得到大幅度提升. 随Ti含量从0mol%增加至100mol%，膜层的平均损伤阈值呈下降趋势，当Ti含量从0mol%增加至60mol%时，平均损伤阈值从57.1J/cm²下降到21.1J/cm²(辐照激光波长为1053nm，脉冲宽度为10ns，“R/1”测试模式)，当Ti含量从60mol%增加至100mol%时，平均损伤阈值变化很小. 综合溶胶微结构、膜层光学性能和损伤实验结果可以推断，强激光诱导多光子吸收是引起膜层损伤的主要原因. 不同配比的复合膜之间光学带隙的显著差异导致相同辐照激光情况下多光子吸收的概率发生变化，从而导致损伤阈值的规律性变化. 关键词： 2-TiO₂薄膜')" href="#">ZrO₂-TiO₂薄膜 溶胶-凝胶 激光诱导损伤 光学带隙     

酸碱分步催化对溶胶-凝胶ZrO2膜光学性能的影响

以丙醇锆作为前驱体,利用酸碱分步催化法制备了ZrO2溶胶,用粒度仪检测胶体粒度;用N2吸脱附表征凝胶的结构;采用旋转镀膜法在K9基片上镀制单层ZrO2薄膜;用分光光度计和椭偏仪检测膜层的透过率、折射率及膜层厚度;用红外光谱仪检测胶体内部粒子间化学键状态。实验结果发现,在脉宽1 nm,波长1 064 nm时,采用此种胶体镀制的单层ZrO2膜层折射率达到1.74,单层膜损伤阈值为9.0 J/cm2,表明该方法集中了酸与碱两种催化方式的优点,一定程度上提高了膜层的光学性能。     

氧分压对ZrO2薄膜激光损伤阈值的影响

在不同的氧分压下用电子束热蒸发的方法制备了ZrO2薄膜。分别通过X射线衍射、光学光谱、热透镜技术、抗激光辐照等测试,对所制备样品的微结构、折射率、吸收率及激光损伤阈值进行了测量。实验结果表明,薄膜中晶粒主要是四方相为主的多晶结构,并且随着氧分压的增加,结晶度、折射率以及弱吸收均逐渐降低。薄膜的激光损伤阈值开始随着氧分压增加从18.5J/cm2逐渐增加,氧分压为9×10-3Pa时达到最大,值为26.7 J/cm2,氧分压再增加时则又降低到17.5 J/cm2。由此可见,氧分压引起的薄膜微结构变化是ZrO2薄膜激光损伤阈值变化的主要原因。     

溶胶凝胶ZrO2/SiO2宽带减反膜的制备与性能

采用溶胶凝胶法制备得到以正丙醇锆和正硅酸乙酯为前驱体的ZrO₂和SiO₂溶胶,通过TFCalc光学薄膜软件模拟了ZrO₂/SiO₂三层“宽M型”基频二倍频减反膜,并使用提拉法制备得到了该均匀膜层。三层减反膜在527 nm和1053 nm处的透过率约为99.5%,且透过率大于99%的波长范围均超过150 nm。经热处理后的膜层表面均方根粗糙度为1.34 nm,表面平整性良好;并运用1-on-1激光损伤阈值测试方法测得该减反膜的零几率激光损伤阈值达到36.8 J·cm^-2(1064 nm,10.7 ns)。     

ZrO2薄膜的改性与抗激光损伤研究

采用水热合成技术,制备了ZrO2胶体,用旋涂法镀制了单层ZrO2介质膜以及添加了有机粘合剂PVP的复合ZrO2-PVP薄膜。采用X射线衍射(XRD)、椭偏仪、红外分光光度计（FTIR）、原子力显微镜（AFM）等仪器对干凝胶及薄膜进行了性能测试和表征,并用输出波长为1.064 μm、脉宽为10 ns的电光调Q激光系统产生的强激光测试其激光损伤阈值。测得ZrO2和ZrO2-PVP薄膜在300 ℃热处理60 min后的激光损伤阈值分别为24.5 J/cm2和37.8 J/cm2。研究表明：添加有机粘合剂后的复合薄膜具有平整的表面结构;有机粘合剂的添加有助于提高薄膜的折射率和激光损伤阈值,其中,ZrO2-PVP 复合薄膜的折射率可高达1.75,激光损伤阈值达到37.8 J/cm2,比ZrO2单层膜的激光损伤阈值提高50%。     

光谱法确定离子束溅射Ta_2O_5/SiO_2薄膜的光学常数及其性能

采用双离子溅射的方法,在硅、石英基底上制备了单层Ta2O5、SiO2及双层Ta2O5/SiO2光学薄膜。结合Cauchy色散模型,利用石英基底上单层Ta2O5及双层Ta2O5/SiO2薄膜透射光谱曲线,采用改进的遗传单纯形混合算法,获得了Ta2O5和SiO2薄膜材料在400~700nm波段的光学常数。结果表明,理论分析值与实验测量值取得了很好的一致性,拟合出的单层Ta2O5薄膜折射率误差小于0.001,膜层厚度误差不超过1nm;双层Ta2O5/SiO2薄膜最大折射率误差小于0.004,最大厚度误差小于2.5nm。此外,还对400℃高温环境下双层Ta2O5/SiO2薄膜的微观结构、应力、表面形貌及光学性能变化进行了研究。     

XPS investigation of diffusion of two-layer ZrO2/SiO2 and SiO2/ZrO2 sol–gel films

Two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were deposited on K9 glass substrates by sol–gel dip coating method. X-ray photoelectron spectroscopy (XPS) technique was used to investigate the diffusion of ZrO₂/SiO₂ and SiO₂/ZrO₂ films. To explain the difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films, porous ratio and surface morphology of monolayer SiO₂ and ZrO₂ films were analyzed by using ellipsometry and atomic force microscopy (AFM). We found that for the ZrO₂/SiO₂ films there was a diffusion layer with a certain thickness and the atomic concentrations of Si and Zr changed rapidly; for the SiO₂/ZrO₂ films, the atomic concentrations of Si and Zr changed relatively slowly, and the ZrO₂ layer had diffused through the entire SiO₂ layer. The difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films was influenced by the microstructure of SiO₂ and ZrO₂.     

Preparation of sol-gel ZrO2-SiO2 highly reflective multilayer films and laser-induced damage threshold characteristic

Sol-gel (ZrO₂/SiO₂)¹² ZrO₂ films were prepared by spin coating method. The reflectivity spectrum of the films was measured with a Lambda 900 spectrometer. In order to investigate laser-induced damage threshold (LIDT) characteristic of highly reflective films, one-layer ZrO₂ and SiO₂ films, two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were also prepared by spin coating method. LIDT of each film was measured. Damage morphology after laser irradiation was characterized by optical microscopy (Nikon E600K). The experimental results showed that the reflectivity of (ZrO₂/SiO₂)¹² ZrO₂ film at 1064 nm and 355 nm wavelength is 99.7%. The LIDT results decreases as the number of layer of films increases. All the films have similar damage morphology. The experimental results are explained by the different temperature profiles of the films.     

Intrinsic defect related luminescence in ZrO2

The studies of ZrO₂ and yttrium stabilized ZrO₂ nanocrystals luminescence as well as yttrium stabilized single crystal luminescence and induced absorption showed that the intrinsic defects are responsible for luminescence at room temperature. These defects form a quasi-continuum of states in ZrO₂ band gap and are the origin of the luminescence spectrum dependence on the excitation energy. Luminescence centers are oxygen vacancies related but not the vacancies themselves. At room temperature, in ZrO₂, deep traps for electrons and holes exist. The oxygen vacancies are proposed to be the traps for electrons.     

Morphology and natural wettability properties of sol-gel derived TiO2-SiO2 composite thin films

Previous studies suggest that granular interfaces induce a natural and persistent super-hydrophilicity in TiO₂-SiO₂ composite thin films deposited by sol-gel route. This effect enables to consider self-cleaning applications that do not require a permanent UV exposure, whereas such a permanent exposure is necessary for pure TiO₂ films. In this study, TiO₂-SiO₂ composite thin films have been deposited from a TiO₂ anatase crystalline suspension and different SiO₂ polymeric sols. Wettability studies show that a suitable control of the TiO₂-SiO₂ mixed sol formulations noticeably enhances persistence of the natural super-hydrophilicity in composite films. It is shown that, beside granular interface effects, modifications in the composite film morphologies can noticeably influence wettability properties.     

Effect of O2 gas partial pressure on structures and dielectric characteristics of rf sputtered ZrO2 thin films

Amorphous and polycrystalline zirconium oxide thin films have been deposited by reactive rf magnetron sputtering in a mixed argon/oxygen or pure oxygen atmosphere with no intentional heating of the substrate. The films were characterized by high-resolution transmission electron microscopy (HR-TEM), atomic force microscopy (AFM), spectroscopic ellipsometry (SE), and capacitance versus voltage (C-V) measurements to investigate the variation of structure, surface morphology, thickness of SiO₂-like interfacial layer as well as dielectric characteristics with different oxygen partial pressures. The films deposited at low oxygen partial pressures (less than 15%) are amorphous and dense with a smooth surface. In contrast, the films prepared at an oxygen partial pressure higher than 73% are crystallized with the microstructure changing from the mixture of monoclinic and tetragonal phases to a single monoclinic structure. The film structural transition is believed to be consequences of decrease in the oxygen vacancy concentration in the film and of increase of the energetically neutral particles in the plasma due to an increased oxygen partial pressure. SE measurements showed that significant interfacial SiO₂ growth has taken place above approximately 51%. The best C-V results in terms of relative dielectric constant values are obtained for thin films prepared at an oxygen partial pressure of 15%.     

Extraction of optical constants and thickness of nanometre scale TiO2 film

TiOTiO2 薄膜 沉积物 磁电管喷射系统 X射线 发射光谱TiO₂ thin films, pointwise constrained optimization approach, constrained nonlinear programming, optical constants, parameters extractionProject supported by Shanghai Municipal Commission for Science and Technology (Grant No 03DZ14025) and National Basic Research Program of China (Grant No 2006CB300406).3/4/2005 12:00:00 AM2005-03-042005-07-28TiO2 thin films were deposited on glass substrates by sputtering in a conventional rf magnetron sputtering system. X-ray diffraction pattern and transmission spectrum were measured. The curves of refraction index and extinction coefficient distributions as well as the thickness of films calculated from transmission spectrum were obtained. The optimization problem was also solved using a method based on a constrained nonlinear programming algorithm.