4H-SiC基底Al_2O_3/SiO_2双层减反射膜的设计和制备

在4H-SiC基底上设计并制备了Al2O3/SiO2紫外双层减反射膜,通过扫描电镜(SEM)和实测反射率谱来验证理论设计的正确性。利用编程计算得到Al2O3和SiO2的最优物理膜厚分别为42.0nm和96.1nm以及参考波长λ=280nm处最小反射率为0.09%。由误差分析可知,实际镀膜时保持双层膜厚度之和与理论值一致有利于降低膜系反射率。实验中应当准确控制SiO2折射率并使Al2O3折射率接近1.715。用电子束蒸发法在4H-SiC基底上淀积Al2O3/SiO2双层膜,厚度分别为42nm和96nm。SEM截面图表明淀积的薄膜和基底间具有较强的附着力。实测反射率极小值为0.33%,对应λ=276nm,与理论结果吻合较好。与传统SiO2单层膜相比,Al2O3/SiO2双层膜具有反射率小,波长选择性好等优点,从而论证了其在4H-SiC基紫外光电器件减反射膜上具有较好的应用前景。

基于平板夹具的电子束蒸发沉积薄膜中的挖坑效应分析

电阻加热具有比较好的加热均匀性,可以认为对于非升华性材料,具有比较理想的平面源发射特性n=1。而电子束加热时,通常n=2~3,甚至可以为6,发射特性参数的范围大,没有取值指导理论或规律,具有很大的不确定性,这对分析薄膜均匀性非常不利。采用细分蒸发源为无数个小的面蒸发源的思想,建立了镀膜材料出现挖坑效应时薄膜厚度均匀性的分析模型。分析结果表明电子束蒸发方法很难获得理想的平面蒸发源,不同程度的挖坑效应将使得n值不同程度地偏离n=1,挖坑效应越明显,n值越大。可以从镀膜机结构设计及薄膜沉积工艺选取两方面着手,降低挖坑效应带来的影响。该研究对认识蒸发源材料发射特性的物理含义具有重要意义,对实验工作同样具有指导性意义。

单脉冲飞秒脉冲激光对单层和高反光学薄膜的损伤

用电子柬蒸发的方法在BK7玻璃上制备了ZrO2单层膜和ZrO2／SiO2高反膜，利用掺Ti：sapphire飞秒激光系统输出的中心波长为800nm，脉宽为50fs的激光脉冲对这两种样品进行了激光损伤阈值测试．实验结果表明，ZrO2单层膜的阂值比ZrO2／SiO2高反膜的高；这与传统的纳秒脉冲激光的损伤情况相反．利用光离化和碰撞离化激发电子到导带，形成电子等离子体基本模型并对此现象进行了解释．同时，用显微镜对样品的损伤形貌进行了观测，对损伤的特点进行了表征．

电子束蒸发镀膜速率控制

介绍了电子束蒸发镀膜速率控制的基本原理和方法,选取实际生产中大量使用且蒸发特性较难控制的SiO_2和HfO_2,对两者的电子束蒸发速率控制分别进行了实验研究。采用比例积分微分(PID)闭环反馈控制,通过Ziegler-Nichols工程经验公式进行原始参量整定,并在实验的基础上对控制器的原始参量进行调整以及对积分作用和微分作用进行分区处理,速率控制的实验结果表明,采用该参量整定方法并结合工艺流程的改进,能获得良好的速率控制。针对速率控制中存在的难点问题进行了分析,并提出改进措施:将速率控制和电子枪扫描控制相结合能进一步改善速率控制。

Investigation of damage threshold to TiO2 coatings at different laser wavelength and pulse duration

Laser-induced damages to TiO2 single layers and TiO2/SiO2 high reflectors at laser wavelength of 1064 nm, 800 run, 532 urn, and pulse width of 12 ns, 220 ps, 50 fs, 8 ns are investigated. All films are prepared by electron beam evaporation. The relations among microstructure, chemical composition, optical properties and laser-induced damage threshold (LIDT), have been researched. The dependence of damage mechanism on laser wavelength and pulse width is discussed. It is found that from 1064 nm to 532 nm, LIDT is mainly absorption related, which is determined by film's extinction coefficient and stoichiometric defects. The rapid decrease of LIDT at 800 nm is due to the pulse width factor. TiO2 coatings are mainly thermally by damaged at long pulse (tau >= 220 ps). The damage shows ablation feature at 50 fs. (C) 2007 Elsevier B.V. All rights reserved.

Annealing effects on the optical and structural properties of Al2O3/SiO2 films as UV antireflection coatings on 4H-SiC substrates

Al2O3/SiO2 films have been prepared by electron-beam evaporation as ultraviolet (UV) antireflection coatings on 4H-SiC substrates and annealed at different temperatures. The films were characterized by reflection spectra, ellipsometer system, atomic force microscopy (AFM), X-ray diffraction (XRD) and Xray photoelectron spectroscopy (XPS), respectively. As the annealing temperature increased, the minimum reflectance of the films moved to the shorter wavelength for the variation of refractive indices and the reduction of film thicknesses. The surface grains appeared to get larger in size and the root mean square (RMS) roughness of the annealed films increased with the annealing temperature but was less than that of the as-deposited. The Al2O3/SiO2 films maintained amorphous in microstructure with the increase of the temperature. Meanwhile, the transition and diffusion in film component were found in XPS measurement. These results provided the important references for Al2O3/SiO2 films annealed at reasonable temperatures and prepared as fine anti-reflection coatings on 4H-SiC-based UV optoelectronic devices. (c) 2008 Elsevier B.V. All rights reserved.

退火对HfO2/SiO2多层膜残余应力的影响

用电子束蒸发方法在BK7基底上沉积了HfO2/SiO2多层膜。研究了200℃到400℃的退火对残余应力的影响。结果表明退火前的薄膜残余应力为压应力，在200℃退火后发展为张应力，然后张应力值随着退火温度的升高而增大。在400℃退火后，由于张应力太大，薄膜表面出现了裂纹。同时，随着退火温度的升高，晶粒尺寸长大，晶面间距降低。残余应力的变化与结构的演变相对应。

Investigation on properties of TiO2 thin films deposited at different oxygen pressures

TiO2 thin films were prepared by electron beam evaporation at different oxygen partial pressures. The influences of oxygen partial pressure on optical, mechanical and structural properties of TiO2 thin films were studied. The results showed that with the increase of oxygen partial pressure, the optical transmittance gradually increased, the transmittance edge gradually shifted to short wavelength, and the corresponding refractive index decreased. The residual stresses of all samples were tensile, and the value increased as oxygen partial pressure increasing, which corresponded to the evolutions of the packing densities. The structures of TiO2 thin films all were amorphous because deposition particles did not possess enough energy to crystallize. (C) 2007 Elsevier Ltd. All rights reserved.

三种不同后处理方式对ZrO_2薄膜性能的影响

采用有氧热处理、激光预处理和离子后处理三种方式对电子束蒸发(EBE)制备的单层ZrO_2薄膜进行了后处理,并分别对样品的光学性能和抗激光损伤阈值(LIDT)特性进行了研究。实验结果表明,热处理方式可以有效排除膜层内吸附的水气,弥补薄膜制备过程中的氧损失,使得光谱短移、吸收减小、损伤阈值增高;激光预处理过程可以在一定程度上减少缺陷、提高损伤阈值,但对膜层的光谱和吸收情况没有明显的改善作用;而离子后处理能够提高膜层的堆积密度、减少缺陷、降低吸收从而提高损伤阈值。由于三种方式处理机制不同,在实际应用中应根据膜层的性能选择合适的处理方式。

Influences of CO2 laser annealing on mechanical and laser-induced damage properties of ZrO2 thin films

Zirconium dioxide (ZrO2) thin films were deposited on BK7 glass substrates by the electron beam evaporation method. A continuous wave CO2 laser was used to anneal the ZrO2 thin films to investigate whether beneficial changes could be produced. After annealing at different laser scanning speeds by CO2 laser, weak absorption of the coatings was measured by the surface thermal lensing (STL) technique, and then laser-induced damage threshold (LIDT) was also determined. It was found that the weak absorption decreased first, while the laser scanning speed is below some value, then increased. The LIDT of the ZrO2 coatings decreased greatly when the laser scanning speeds were below some value. A Nomarski microscope was employed to map the damage morphology, and it was found that the damage behavior was defect-initiated both for annealed and as-deposited samples. The influences of post-deposition CO2 laser annealing on the structural and mechanical properties of the films have also been investigated by X-ray diffraction and ZYGO interferometer. It was found that the microstructure of the ZrO2 films did not change. The residual stress in ZrO2 films showed a tendency from tensile to compressive after CO, laser annealing, and the variation quantity of the residual stress increased with decreasing laser scanning speed. The residual stress may be mitigated to some extent at proper treatment parameters. (c) 2007 Elsevier GmbH. All rights reserved.

Influence of ytterbia content on residual stress and microstructure of Y2O3-ZrO2 thin films prepared by EB-PVD

Y2O3 stabilized ZrO2 (YSZ) thin films with different Y2O3 molar contents (0, 3, 7, and 12 mol%) are deposited on BK7 substrates by electron-beam evaporation technique. The effects of different Y2O3 contents on residual stresses and structures of YSZ thin films are studied. Residual stresses are investigated by means of two different techniques: the curvature measurement and x- ray diffraction method. It is found that the evolution of residual stresses of YSZ thin films by the two different methods is consistent. Residual stresses of films transform from compressive stress into tensile stress and the tensile stress increases monotonically with the increase of Y2O3 content. At the same time, the structures of these films change from the mixture of amorphous and monoclinic phases into high temperature cubic phase. The variations of residual stress correspond to the evolution of structures induced by adding of Y2O3 content.

沉积温度对氧化钇稳定氧化锆薄膜残余应力的影响

采用自制掺摩尔分数12%的Y2O3的ZrO2混合颗粒料为原料,在不同的沉积温度下用电子束蒸发方法沉积氧化钇稳定氧化锆(YSZ)薄膜样品。利用ZYGOMarkⅢ-GPI数字波面干涉仪对氧化钇稳定氧化锆薄膜的残余应力进行了研究,讨论了沉积温度对残余应力的影响。实验结果表明:随沉积温度升高,氧化钇稳定氧化锆薄膜中残余应力状态由张应力变为压应力,且压应力值随着沉积温度升高而增大;用X射线衍射仪表征了不同沉积温度下氧化钇稳定氧化锆薄膜的微观结构,探讨了薄膜微观结构与其应力的对应关系,并对比了纯ZrO2薄膜表现出的应力状态。

High temperature annealing effect on structure, optical property and laser-induced damage threshold of Ta2O5 films

Ta2O5 films were deposited by conventional electron beam evaporation method and then annealed in air at different temperature from 873 to 1273 K. It was found that the film structure changed from amorphous phase to hexagonal phase when annealed at 1073 K, then transformed to orthorhombic phase after annealed at 1273 K. The transmittance was improved after annealed at 873 K, and it decreased as the annealing temperature increased further. The total integrated scattering (TIS) tests and AFM results showed that both scattering and root mean square (RMS) roughness of films increased with the annealing temperature increasing. X-ray photoelectron spectroscopy (XPS) analysis showed that the film obtained better stoichiometry and the O/Ta ratio increased to 2.50 after annealing. It was found that the laser-induced damage threshold (LIDT) increased to the maximum when annealed at 873 K, while it decreased when the annealing temperature increased further. Detailed damaged models dominated by different parameters during annealing were discussed. (C) 2008 Elsevier B. V. All rights reserved.

Influence of SiO2 additional layers on the laser induced damage threshold of Ta2O5 films

A series or Ta2O5 films with different SiO2 additional layers including overcoat, undercoat and interlayer was prepared by electron beam evaporation under the same deposition process. Absorption of samples was measured using the surface thermal lensing (STL) technique. The electric field distributions of the samples were theoretical predicted using thin film design software (TFCalc). The laser induced damage threshold (LIDT) was assessed using an Nd:YAG laser operating at 1064 nm with a pulse length of 12 ns. It was found that SiO2 additional layers resulted in a slight increase of the absorption, whereas they exerted little influence on the microdefects. The electric field distribution among the samples was unchanged by adding an SiO2 overcoat and undercoat, yet was changed by adding an interlayer. SiO2 undercoat. The interlayer improved the LIDT greatly, whereas the SiO2 overcoat had little effect on the LIDT. (C) 2007 Elsevier Ltd. All rights reserved.

Impact of organic contamination on laser-induced damage threshold of high reflectance coatings in vacuum

The influence of organic contamination in vacuum on the laser-induced damage threshold (LIDT) of coatings is studied. TiO2/SiO2 dielectric mirrors with high reflection at 1064 nm are deposited by the electron beam evaporation method. The LIDTs of mirrors are measured in vacuum and atmosphere, respectively. It is found that the contamination in vacuum is easily attracted to optical surfaces because of the low pressure and becomes the source of damage. LIDTs of mirrors have a little change in vacuum compared with in atmosphere when the organic contamination is wiped off. The results indicate that organic contamination is a significant reason to decrease the LIDT. N-2 molecules in vacuum can reduce the influence of the organic contaminations and prtectect high reflectance coatings. (C) 2008 Elsevier B.V. All rights reserved.