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.

SiO2保护层和退火对Ta2O5薄膜激光损伤阈值影响的对比研究

Ta2O5薄膜采用传统的电子束蒸发方法沉积在BK7基底上。文中对SiO2保护层和退火对Ta2O5薄膜的激光损伤阈值的不同影响进行了研究。结果表明，SiO2保护层不会影响薄膜内的电场分布，薄膜微结构和微缺陷密度，但是会使薄膜的吸收稍微增大；而退火对降低薄膜的微缺陷密度和吸收较有效。SiO2保护层和退火都有利于提高Ta2O5薄膜的抗激光损伤能力，并且退火对提高阈值的影响更为明显。此外，采用SiO2保护层和退火结合的方法，获得了具有最大激光损伤阈值的薄膜。

Influence of different substrates on laser induced damage thresholds at 1064 nm of Ta2O5 films

Ta2O5 films are prepared on Si, BK7, fused silica, antireflection (AR) and high reflector (HR) substrates by electron beam evaporation method, respectively. Both the optical property and laser induced damage thresholds (LIDTs) at 1064 nm of Ta2O5 films on different substrates are investigated before and after annealing at 673 K for 12h. It is shown that annealing increases the refractive index and decreases the extinction index, and improves the O/Ta ratio of the Ta2O5 films from 2.42 to 2.50. Moreover, the results show that the LIDTs of the Ta2O5 films are mainly correlated with three parameters: substrate property, substoichiometry defect in the films and impurity defect at the interface between the substrate and the films. Details of the laser induced damage models in different cases are discussed.

Laser induced damage threshold at 355 and 1064 nm of Ta2O5 films of different phases

Ta2O5 films are deposited on fused silica substrates by conventional electron beam evaporation method. By annealing at different temperatures, Ta2O5 films of amorphous, hexagonal and orthorhombic phases are obtained and confirmed by x-ray diffractometer ( XRD) results. X-ray photoelectron spectroscopy ( XPS) analysis shows that chemical composition of all the films is stoichiometry. It is found that the amorphous Ta2O5 film achieves the highest laser induced damage threshold ( LIDT) either at 355 or 1064 nm, followed by hexagonal phase and finally orthorhombic phase. The damage morphologies at 355 and 1064 nm are different as the former shows a uniform fused area while the latter is centred on one or more defect points, which is induced by different damage mechanisms. The decrease of the LIDT at 1064nm is attributed to the increasing structural defect, while at 355nm is due to the combination effect of the increasing structural defect and decreasing band gap energy.

不同方法制备的Ta_2O_5薄膜光学性能和激光损伤阈值的对比分析

采用电子束蒸发(EBE)和离子束溅射(IBS)制备了不同的Ta_2O_5薄膜,同时对电子束蒸发制备的薄膜进行了退火处理。研究了制备的Ta_2O_5薄膜的光学性能、激光损伤阈值(LIDT)、吸收、散射、粗糙度、微缺陷密度和杂质含量。结果表明,退火可使电子束蒸发制备的薄膜的光学性能得到改善,接近离子束溅射的薄膜的光学性能。电子束蒸发制备的薄膜的损伤阈值较低的主要原因在于吸收大,微缺陷密度和杂质含量高,而与薄膜的散射和粗糙度关系不大。退火后薄膜的吸收和微缺陷密度都明显降低,损伤阈值得到提高。退火后的薄膜损伤阈值仍然低于溅射得到的薄膜损伤阈值是因为退火并不能降低膜内的杂质含量,因此选用高纯度的蒸发膜料和减少电子束蒸发过程中的污染有可能进一步提高薄膜的损伤阈值。

Structure and optical properties of Nb2O5 sculptured thin films by glancing angle deposition

Nb2O5 sculptured thin. films deposited by electron beam evaporation with glancing angle deposition were prepared. Nb2O5 sculptured thin. films with tilted columns are optical anisotropy. XRD, SEM, UV-vis-NIR spectra are employed to characterize the microstructure and optical properties. The maximum of birefringence (Delta n) is up to 0.045 at alpha = 70 degrees with packing density of 0.487. With increasing the deposition angle, refractive index and packing density of Nb2O5 STF are decreasing. The relationship among deposition parameter, microstructure and optical properties was investigated in detail. (C) 2008 Elsevier B. V. All rights reserved.