ZrO2/ SiO2多层膜的化学法制备研究

 分别以ZrOCl₂·8H₂O 和正硅酸乙酯为原料,采用溶胶-凝胶工艺制备了性能稳定的ZrO₂和SiO₂溶胶。用旋转镀膜法分别在K9玻璃和单晶硅片上制备了ZrO₂/ SiO₂多层膜。采用溶剂替换和紫外光处理等手段,有效地解决了ZrO₂/SiO₂多层膜中膜层开裂和膜间渗透等问题。应用扫描电子显微镜观测了薄膜的表面和剖面微观形貌,并用椭偏仪测得薄膜的厚度和折射率,研究了薄膜厚度、折射率与热处理温度、紫外光处理时间的关系,对所获得薄膜的紫外-可见、红外光谱进行了分析。用输出波长1064nm ,脉宽15ns 的电光调Q光系统产生的强激光进行了单层膜的辐照实验,结果发现溶剂替换后激光损伤阈值有所提高。     

ZrO2/SiO2溶胶-凝胶薄膜膜层间的渗透行为

 分别以丙醇锆和正硅酸乙酯为原料，采用溶胶-凝胶工艺制备了性能稳定的ZrO₂和SiO₂溶胶。用旋转镀膜法在K9玻璃上分别制备了单层SiO₂薄膜、单层ZrO₂薄膜、ZrO₂/ SiO₂双层膜和SiO₂/ZrO₂双层膜。采用原子力显微镜观察了薄膜的表面形貌，用椭偏仪测量薄膜的厚度与折射率，用紫外-可见光分光光度计测量了薄膜的透射率。对薄膜的透射光谱和椭偏仪模拟的数据进行分析，发现SiO₂/ZrO₂双层膜之间的渗透十分明显，而ZrO₂/SiO₂双层膜之间几乎不发生渗透。利用TFCalc模系设计软件,采用三层膜模型对薄膜的透射率进行模拟，得出的透射曲线与用紫外-可见光分光光度计测量的透射曲线十分符合。     

关于热生长SiO2薄膜厚度的测量

在半导体硅器件的研究工作中,需要准确地测量和控制SiO₂薄膜的厚度。由于干涉原理,SiO₂薄膜在白光照射下呈现颜色。但薄膜厚度与颜色相应的单色光的波长并不成简单的函数关系。本文叙述了用干涉显微镜测量热生长SiO₂薄膜厚度的方法。由测量结果得到SiO₂薄膜的折射率以及SiO₂和硅界面及空气和硅界面反射相移之差。并且测量了一组标准样品的薄膜厚度,列出了薄膜厚度与干涉颜色的对应关系。所得结果与从Rollet数据所推算的结果大致符合。样品厚度还包括了Rollet数据中所未包括的范围(3300—4200?)。     

层间热处理对SiO2/ZrO2双层膜的影响

 以正硅酸乙酯和丙醇锆为前驱体,用溶胶-凝胶法在K9基片上提拉镀制SiO₂/ZrO₂双层膜。采用不同实验步骤制备了2个样品,样品1镀完SiO₂后直接镀ZrO₂ ,样品2镀完SiO₂经热处理后再镀ZrO₂。采用原子力显微镜、椭偏仪、紫外-可见分光光度计对薄膜进行表征。针对SiO₂/ZrO₂双层膜,考虑到膜间渗透的影响,采用３层Cauchy模型进行椭偏模拟,椭偏参数的模拟值曲线与椭偏仪的测量值曲线十分吻合,进而发现热处理可以使SiO₂/ZrO₂双层膜之间的渗透减少近23 nm,从而提高其峰值透射率。利用输出波长1.064 mm,脉宽8.1 ns的激光束对样品进行了损伤阈值的测试,用光学显微镜观察损伤形貌,结果发现两者损伤阈值分别为13.6 J/c2和14.18 J/cm²,均为膜的本征损伤。     

SR-FEL宽带腔镜与双带腔镜光学膜系实验研究与研制

利用“电子束蒸发沉积薄膜生长技术+离子束溅射沉积薄膜生长技术”、“HfO₂/SiO₂+Al₂O₃/SiO₂+M-SiO₂”复合光学膜系设计技术、400°C4h高温处理技术, 研制的SR-FEL宽带腔镜光学膜系在355nm中心波长的绝对光学反射率测量值为R(355nm)=99.45%, 反射光谱带宽测量值为Δλ(R≥99.00%)=75nm; 研制的355nm/248nm双带腔镜光学膜系, 在355nm中心波长, 其绝对光学反射率测量值为R(355nm)=99.69%, 反射光谱带宽测量值为Δλ(R≥99.00%)=59nm; 在248nm中心波长, R(248nm)=98.21%, 绝对光学反射率光谱带宽测量值Δλ(R≥99.00)=9mm, Δλ(R≥98.00%)=33nm.     

SiO2半波覆盖层对HfO2/SiO2高反膜激光损伤的影响

 研究了SiO₂半波覆盖层对HfO₂/SiO₂高反射膜1064nm激光损伤的影响,分析薄膜的激光损伤特性及图貌得出, 对于单脉冲（1-ON-1）激光损伤,SiO₂半波覆盖层能提高HfO₂/SiO₂高反膜的激光损伤阈值;可显著降低激光损伤程度,减小灾难性损伤发生的概率;可大幅度提高HfO₂/SiO₂高反膜膜的抗激光损伤能力。     

波长1064nm脉冲激光高阈值反射膜的研制

 研究HfO₂/SiO₂高反射膜的制备工艺及其激光诱导损伤阈值的比较测试,分别采用了反应蒸镀HfO₂、反应离子辅助蒸镀HfO₂、反应离子辅助蒸镀金属Hf的源材料形成HfO₂薄膜。采用这三种工艺制备了HfO₂/SiO₂高反射膜,在中心波长1064nm处,反射率 R≥99.5%,其中反应蒸镀HfO₂/SiO₂高反射膜损伤阈值最高,可达60J/cm²(1064nm,5ns)。     

LBO晶体上1 064，532 nm倍频增透膜的镀制及性能分析

 用电子束蒸发沉积方法在X切LBO（X-LBO）晶体上镀制了两种不同膜系结构的1 064和532 nm倍频增透膜，其中一种膜系结构为基底/ZrO₂/Y₂O₃/Al₂O₃/SiO₂/空气，另一种为基底/0.5Al₂O₃/ZrO₂/Y₂O₃/Al₂O₃/SiO₂/空气，两种膜系结构的主要差别在于有无氧化铝过渡层。测量了薄膜的反射率光谱曲线，发现两种增透膜在1 064和532 nm处的反射率均小于0.5％，实际镀制结果与理论设计曲线的差异主要是由材料折射率的变化引起的。且对样品在空气环境中进行了温度为473 K的退火处理，结果发现两种膜系结构均表现了较优异的光学性能，氧化铝过渡层的加入使薄膜具有强的热应力性能。     

氧化物激光薄膜的离子束溅射制备技术

 研究了由Ta₂O₅和SiO₂组成的多层氧化物激光薄膜的双离子束溅射制备工艺。简要介绍了离子束溅射技术的基本工作原理和应用，着重分析了薄膜厚度均匀性的调控方法。先后得到了Ta₂O₅和SiO₂单层薄膜厚度均匀性调控结果以及不同波长处薄膜折射率，并定性地分析比较了离子束溅射和电子束蒸发制备的薄膜结构；制备并测试了633nm,1 315nm反射薄膜以及增透膜。结果表明：采用离子束溅射技术能够制备出优良的、满足需要的激光高反射薄膜元件。     

多孔TiO2/Al/SiO2纳米复合结构的紫外光吸收特性研究

在SiO₂玻璃衬底上用脉冲激光沉积(PLD)技术，分别沉积Ti和Ti/Al膜，经电化学阳极氧化成功制备了多孔TiO₂/SiO₂和TiO₂/Al/SiO₂纳米复合结构. 其中TiO₂薄膜上的微孔阵列高度有序，分布均匀. 实验研究了Al过渡层对多孔TiO₂薄膜光吸收特性的影响. 结果表明：无Al过渡层的多孔TiO₂薄膜其紫外吸收峰在27     

基于时间控厚离子束溅射技术的宽带减反膜制备

 为了制备满足设计要求的宽角度、宽波段减反膜,利用离子束溅射沉积技术,在时间-功率控厚的模式下,对膜层沉积速率进行了精确修正。在实验中,利用时间-功率控厚的离子束溅射沉积技术,选择HfO₂和SiO₂作为高低折射率组合,在超抛ZF6玻璃基底上制备了宽角度、宽带减反膜,通过对实验后的透过率光谱曲线的数值反演计算,获得膜层厚度修正系数,初步得到了沉积速率随沉积时间变化的规律。利用修正后的沉积参数制备设计的膜系,在0°~30°入射角度下,600~1 200 nm波段的平均透过率达到99%以上。     

The refractive index of homogeneous SiO<Subscript>2</Subscript> thin films

The effect of the through-thickness inhomogeneity of SiO₂ films on their refractive index is studied. The SiO₂ films, deposited by tetraethoxysilane pyrolysis on plane-parallel oriented crystalline quartz substrates and on silicon plates, were etched layer-by-layer in Pliskin’s solution. The refractive index and the geometric thickness of films were calculated from the measured ellipsometric angles after each etching. The determination errors of the refractive indices as functions of the film thickness, which result from the measurement errors of the polarization angles and substrate parameters, are numerically analyzed. For SiO₂ films thicker than 20nm, no effect of inhomogeneity is found. The refractive indices of thinner films were observed to depend on the thickness. The reasons for such dependences are discussed.     

宽带膜厚实时监控过程中膜层折射率的确定方法

为了准确计算出镀膜过程中每层膜的折射率，介绍了实时监控过程中确定膜层折射率的2种方法：一种是由实测的透射比光谱直接反算出膜层的折射率；另一种是用最小二乘法的优化算法实时拟合折射率。试验结果表明：在线反算适合单点监控，所得折射率误差小于2%。然而在实际镀膜过程中,由于宽带内膜层参数误差较大,一般大于25%。为此，采用最小二乘法拟合，即在整个宽光谱范围内采集每个波长点的信息，所得结果误差很小，一般都在2％～5%之间,有时可达到10%,在很大程度上提高了实际镀膜时膜厚监控的精度。     

自适应模拟退火遗传算法在薄膜厚度及光学常数反演中的应用

准确的测量薄膜的厚度和光学常数,在薄膜的制备、研究和应用中都是十分重要的。借助Cauchy色散模型,通过薄膜透过率测量曲线,用改进的自适应模拟退火遗传算法对透过率曲线进行全光谱拟合,从而反演得到薄膜的厚度和光学常数。对由电子束蒸发制备的TiO2单层膜和SiO2/TiO2双层膜的厚度和光学常数进行了测量计算。实验结果表明,计算得到的光学参数与实测结果相一致,厚度误差小于2nm,在560nm波长处折射率误差小于0.03。     

Optical parameters of epitaxial GaN thin film on Si substrate from the reflection spectrum

A method has been proposed for determining the optical properties of a thin film layer on absorbing substrates. The film optical parameters such as thickness, refractive index, absorption coefficient, extinction coefficient and the optical energy gap of an absorbing film are retrieved from the interference fringes of the reflection spectrum at normal incidence. The envelopes of the maxima of the spectrum E_M and of the minima E_m are introduced in analytical forms to find the reflectance amplitudes at the interfaces and approximate values of the thin film refractive index. Then, the interference orders and film thickness are calculated to get accurate values of the needed optical parameters. There are no complex fitting procedures or assumed theoretical refractive index dispersion relations. The method is applied to calculate the optical properties of an epitaxial gallium nitride thin film on a silicon (1 1 1) substrate. Good agreement between our results and the published data are obtained.     

基于等离子体增强化学气相沉积技术的光电子器件多层抗反膜的设计和制作

针对光电子器件端面抗反镀膜的要求,研究了基于等离子体增强化学气相沉积(PECVD)技术的多层抗反膜的设计和制作.首先,对影响SiN_x折射率的因素进行了实验研究,确定了具有大折射率差的SiO₂/SiN_x材料的PECVD沉积条件.根据理论计算分析,设计了四层SiO₂/SiN_x抗反膜结构,能够在70 nm的波长范围内实现低于10^-4的反射率     

Calculation of optical constant of amorphous germanium arsenoselenide wedge-shaped thin films from their shrunk transmittance and reflectance spectra

The optical transmittance spectrum is influenced by inhomogeneities in germanium arsenoselenide thin films. The non-uniformity of thickness, found under the present deposition conditions, gives rise to a clear shrinking of the interference fringes of the transmittance spectrum at normal incidence. Inaccuracies and even serious errors occur if the refractive index and film thickness are calculated from such a shrunken transmittance spectrum, under the unrealistic assumption that the film is uniform. The analytical expressions proposed by Swanepoel [J. Phys. E. Sci. Instrum. 17 (1984) 896] enabled derivation of the refractive index and film thickness of a wedge-shaped thin film from its shrunk transmittance spectrum. This method was applied in this study making it possible to derive the refractive index and average thickness to an accuracy better than 1%. Dispersion of the refractive index is discussed in terms of the single-oscillator Wemple–DiDomenico model [Phys. Rev. B 3 (1971) 1338]. The absorption coefficient and, thus the extinction coefficient, can be calculated from transmittance and reflectance spectra in the strong absorption region. The optical energy gap is derived from Tauc's extrapolation [Amorphous and Liquid Semiconductor (Plenum Press, New York, 1974)]. The relationship between the optical gap and chemical composition in the Ge _x As_{30– x} Se₇₀ (with 0 ≤ x ≤ 30) amorphous system is discussed in terms of the chemical bond approach and cohesive energy.     

Design and Fabrication of Chirped Mirror

Chirped mirrors （CMs） are designed and manufactured. The optimized CM provides a group delay dispersion （ODD） of around -60fs^2 and average reflectivity of 99.4% with bandwidth 200 nm at a central wavelength of 800nm. The CM structure consists of 52 layers of alternating high refractive index Ta2O5 and low refractive index SiO2. Measurement results show that the control of CM manufacturing accuracy can meet our requirement through time control with ion beam sputtering. Because the ODD of CMs is highly sensitive to small discrepancies between the layer thickness of calculated design and those of the manufactured mirror, we analyze the error sources which result in thickness errors and refractive index inhomogeneities in film manufacture.     

Microstructure parameters and optical properties of cadmium ferrite thin films of variable thickness

CdFe₂O₄ thin films of different thicknesses were deposited onto glass substrates by the thermal evaporation technique. Their structural characteristics were studied by X-ray diffraction (XRD). The microstructure parameters, crystallite size, and microstrain were calculated. It is observed that both the crystallite size increases and microstrain increase with increasing with the film thickness. The fundamental optical parameters like absorption coefficient and optical band gap are calculated in the strong absorption region of transmittance and reflectance spectrum. The refractive indices have been evaluated in terms of the envelope method, which has been suggested by Swanepoel in the transparent region. The refractive index can be extrapolated by the Cauchy dispersion relationship over the whole spectra range, which extended from 400 to 2500 nm. The refractive index, n, increases on increasing the film thickness up to 733 nm and the variation of n with higher thickness lies within the experimental errors.     

TiO2/SiO2 multilayer as an antireflective and protective coating deposited by microwave assisted magnetron sputtering

In this paper designing, preparation and characterization of multifunctional coatings based on TiO₂/SiO₂ has been described. TiO₂ was used as a high index material, whereas SiO₂ was used as a low index material. Multilayers were deposited on microscope slide substrates by microwave assisted reactive magnetron sputtering process. Multilayer design was optimized for residual reflection of about 3% in visible spectrum (450–800 nm). As a top layer, TiO₂ with a fixed thickness of 10 nm as a protective film was deposited. Based on transmittance and reflectance spectra, refractive indexes of TiO₂ and SiO₂ single layers were calculated. Ultra high vacuum atomic force microscope was used to characterize the surface properties of TiO₂/SiO₂ multilayer. Surface morphology revealed densely packed structure with grains of about 30 nm in size. Prepared samples were also investigated by nanoindentation to evaluate their protective performance against external hazards. Therefore, the hardness of the thin films was measured and it was equal to 9.34 GPa. Additionally, contact angle of prepared coatings has been measured to assess the wetting properties of the multilayer surface.