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.

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.

HfO2的纯度对紫外多层膜反射率的影响

用辉光放电质谱法和二次离子质谱仪测定了两种HfO2材料及它们相应的单层膜中的杂质含量，结果发现，无论是在体材料中还是在用电子束蒸发技术沉积的材料单层薄膜中，ZrO2都是这两种HfO2材料中最主要的杂质。而且，这两种HfO2材料中Zr含量的差别远远大于Ti、Fe含量的差别，这说明Zr含量的差别正是引起两种HfO2膜层光学性能差别的原因。用这两种不同纯度的HfO2材料与同一纯度的SiO2材料组合，沉积形成266nm的紫外反射镜，实验结果表明这两种反射镜的反射率分别在99.85% 和 99.15%左右。这个结果与依据单层膜得出的光学常数所设计的结果符合的很好。

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.

Investigation of annealing effects on the laser-induced damage threshold of amorphous Ta2O5 films

Ta2O5 films were deposited using the conventional electron beam evaporation method and then annealed at temperatures in the range 373-673 K. Chemical composition, scattering and absorption were examined by X-ray photoelectron spectroscopy (XPS), total integrated scattering (TIS) measurement and the surface thermal lensing (m) technique, respectively. The laser-induced damage threshold (LIDT) was assessed using the output from an Nd:YAG laser with a pulse length of 12 ns. The results showed that the improvement of the LIDT after annealing was due to the reduced substoichiometric and structural defects present in the film. The LIDT increased slightly below 573K and then increased significantly with increase in annealing temperature, which could be attributed to different dominant defects. Moreover, the root mean square (RMS) roughness and scattering had little effect on the LIDT, while the absorption and the LIDT were in accord with a general relation. (c) 2008 Elsevier Ltd. All rights reserved.

Effects of deposition rates on laser damage threshold of TiO2/SiO2 high reflectors

TiO2 single layers and TiO2/SiO2 high reflectors (HR) are prepared by electron beam evaporation at different TiO2 deposition rates. It is found that the changes of properties of TiO2 films with the increase of rate, such as the increase of refractive index and extinction coefficient and the decrease of physical thickness, lead to the spectrum shift and reflectivity bandwidth broadening of HR together with the increase of absorption and decrease of laser-induced damage threshold. The damages are found of different morphologies: a shallow pit to a seriously delaminated and deep crater, and the different amorphous-to-anatase-to-rutile phase transition processes detected by Raman study. The frequency shift of Raman vibration mode correlates with the strain in. film. Energy dispersive X-ray analysis reveals that impurities and non-stoichiometric defects are two absorption initiations resulting to the laser-induced transformation. (C) 2008 Elsevier B. V. All rights reserved.

Investigation on thermal stability of TiO2 films for application at high temperature

The thermal stability of electron beam deposited TiO2 monolayers and TiO2/SiO2 high reflectors (HR) during 300 to 1100 degrees C annealing is studied. It is found that the optical loss of film increases with the increase in annealing temperature, due to the phase change, crystallisation and deoxidising of film. Scattering loss dominates the optical property degradation of film below 900 degrees C, while the absorption is another factor at 1100 degrees C. The increase in refractive index and decrease in physical thickness of TiO2 layer shift the spectra of HR above 900 degrees C. The possible crack mechanism on the surface of HR during annealing is discussed. Guidance for application on high temperature stable optical coatings is given.