Y2O3 stabilized ZrO2 thin films deposited by electron beam evaporation: Structural, morphological characterization and laser induced damage threshold

Four kinds of Y2O3 stabilized ZrO2 (YSZ) thin films with different Y2O3 content have been prepared on BK7 substrates by electron-beam evaporation method. Structural properties and surface morphology of thin films were investigated by X-ray diffraction (XRD) spectra and scanning probe microscope. Laser induced damage threshold (LIDT) was determined. It was found that crystalline phase and microstructure of YSZ thin films was dependent on Y2O3 molar content. YSZ thin films changed from monoclinic phase to high temperature phase (tetragonal and cubic) with the increase of Y2O3 content. The LIDT of stabilized thin film is more than that of unstabilized thin films. The reason is that ZrO2 material undergoes phase transition during the course of e-beam evaporation resulting in more numbers of defects compared to that of YSZ thin films. These defects act as absorptive center and the original breakdown points. (c) 2006 Elsevier B.V. All rights reserved.

High laser-induced damage threshold HfO2 films prepared by ion-assisted electron beam evaporation

HfO2 films were deposited by electron beam evaporation with different deposition parameters. The properties such as refractive index, weak absorption, and laser induced damage thresholds (LIDTs) of these films have been investigated. It was found that when pulsed Nd:YAG 1064 nm laser is used to investigate LIDT of films: Metallic character is the main factor that influences LIDTs of films obtained from Hf starting material by ion-assisted reaction, and films prepared with higher momentum transfer parameter P have fewer metallic character; The ion-assisted reaction parameters are key points for preparing high LIDT films and if the parameters are chose properly, high LIDT films can be obtained. (c) 2004 Elsevier B.V. All rights reserved.

真空中有机污染物对TiO2/SiO2介质膜损伤阈值的影响

本文主要研究了真空中有机污染物对薄膜阈值的影响。采用电子枪蒸镀的方式制备了由TiO2/SiO2两种材料组合而成的1064nm高反膜，分别在大气和真空中对其损伤阈值进行了测量。发现在真空中污染物易黏附于光学元件表面，导致损伤；真空中的氧分子会加速损伤过程，根据破斑形貌的分析认为是由于在激光作用下氧分子与有机污染物发生反应造成的；真空中的有机污染物被去除后，真空和大气中的损伤阈值差别不大，破斑形貌相似。结果表明有机污染物是真空中损伤阈值降低的主要原因。

Comparison of TiO2 and ZrO2 films deposited by electron-beam evaporation and by sol-gel process

TiO2 and ZrO2 films are deposited by electron-beam (EB) evaporation and by sol-gel process. The film properties are characterized by visible and Fourier-transform infrared spectrometry, x-ray diffraction analysis, surface roughness measure, absorption and laser-induced damage threshold (LIDT) test. It is found that the sol-gel Elms have lower refractive index, packing density and roughness than EB deposited films due to their amorphous structure and high OH group concentration in the film. The high LIDT of sol-gel films is mainly due to their amorphous and porous structure, and low absorption. LIDT of EB deposited film is considerably affected by defects in the Elm, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.

Influences of oxygen partial pressure on structure and related properties of ZrO2 thin films prepared by electron beam evaporation deposition

ZrO2 thin films were prepared by electron beam evaporation at different oxygen partial pressures. The influences of oxygen partial pressure on structure and related properties of ZrO2 thin films were studied. Transmittance, thermal absorption, structure and residual stress of ZrO2 thin films were measured by spectrophotometer, surface thermal lensing technique (STL), X-ray diffraction and optical interferometer, respectively. The results showed that the structure and related properties varied progressively with the increase of oxygen partial pressure. The refractive indices and the packing densities of the thin films decreased when the oxygen partial pressure increased. The tetragonal phase fraction in the thin films decreased gradually as oxygen partial pressure increased. The residual stress of film deposited at base pressure was high compressive stress, the value decreased with the increase of oxygen partial pressure, and the residual stress became tensile with the further increase of oxygen pressure, which was corresponding to the evolution of packing densities and variation of interplanar distances. (c) 2007 Elsevier B.V. All rights reserved.

Optical and electrical properties of TiOx thin films deposited by electron beam evaporation

The TiOx thin films were prepared by electron beam evaporation using TiO as the starting material. The effect of the annealing temperature on the optical and electrical properties was investigated. The spectra of X-ray photoelectron spectroscopy reveal that Ti in the films mainly exist in the forms of Ti2+ and Ti3+ below 400 degrees C 24h annealing. The charge transfer between different titanium ion contribute greatly to the color, absorption, and electrical resistance of the films. (c) 2006 Elsevier Ltd. All rights reserved.

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。

Influence of oxygen plasma treatment on properties of ZrO2 films prepared by e-beam evaporation techniques

Zirconia films were prepared by e-beam evaporation, and oxygen plasma treatment was used to modify film properties. Spectrophotometry, x-ray diffractometry (XRD), and atomic force microscopy were used to characterize refractive index, extinction coefficient, rnicrostructure, and surface roughness, respectively. The experimental results indicate that both refractive index and extinction coefficient of the films were reduced slightly after oxygen plasma treatment, with the decrease of intrinsic stress and surface roughness. From XRD spectra, the intensity decrease of the T(110) diffraction peak was clearly observed after the treatment, which was caused by the restructuring of the film atoms. (C) 2008 Elsevier Ltd. All rights reserved.

Working pressure dependence of properties of Al2O3 thin films prepared by electron beam evaporation

The effects of working pressure on properties of Al2O3 thin films are investigated. Transmittance of the Al2O3 thin film is measured by a Lambda 900 spectrometer. Laser-induced damage threshold (LIDT) is measured by a Nd:YAG laser at 355nm with a pulse width of 7ns. Microdefects were observed under a Nomarski microscope. The samples are characterized by optical properties and defect, as well as LIDT under the 355 nm Nd: YAG laser radiation. It is found that the working pressure has fundamental effect on the LIDT. It is the absorption rather than the microdefect that plays an important role on the LID T of Al2O3 thin film.

Al2O3/SiO2 films prepared by electron-beam evaporation as UV antireflection coatings on 4H-SiC

Al2O3/SiO2 films have been deposited as UV antireflection coatings on 4H-SiC by electron-beam evaporation and characterized by reflection spectrum, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The reflectance of the Al2O3/SiO2 films is 0.33% and 10 times lower than that of a thermally grown SiO2 single layer at 276 nm. The films are amorphous in microstructure and characterize good adhesion to 4H-SiC substrate. XPS results indicate an abrupt interface between evaporated SiO2 and 4H-SiC substrate free of Si-suboxides. These results make the possibility for 4H-SiC based high performance UV optoelectronic devices with Al2O3/SiO2 films as antireflection coatings. (C) 2007 Elsevier B.V. All rights reserved.

Y2O3 stabilized ZrO2 thin films deposited by electron-beam evaporation: Optical properties, structure and residual stresses

This paper describes the preparation and the characterization Of Y2O3 stabilized ZrO2 thin films produced by electric-beam evaporation method. The optical properties, microstructure, surface morphology and the residual stress of the deposited films were investigated by optical spectroscopy, X-ray diffraction (XRD), scanning probe microscope and optical interferometer. It is shown that the optical transmission spectra of all the YSZ thin films are similar with those of ZrO2 thin film, possessing high transparency in the visible and near-infrared regions. The refractive index of the samples decreases with increasing of Y2O3 content. The crystalline structure of pure ZrO2 films is a mixture of tetragonal phase and monoclinic phase, however, Y2O3 stabilized ZrO2 thin films only exhibit the cubic phase independently of how much the added Y2O3 content is. The surface morphology spectrum indicates that all thin films present a crystalline columnar texture with columnar grains perpendicular to the substrate and with a predominantly open microporosity. The residual stress of films transforms tensile from compressive with the increasing Of Y2O3 molar content, which corresponds to the evolutions of the structure and packing densities. (C) 2008 Elsevier Ltd. All rights reserved.

Influence of ZrO2 in HfO2 on reflectance of HfO2/SiO2 multilayer at 248 nm prepared by electron-beam evaporation

Influence of ZrO2 in HfO2 on the reflectance of HfO2/SiO2 multilayer at 248 nm was investigated. Two kinds of HfO2 with different ZrO2 content were chosen as high refractive index material and the same kind of SiO2 as low refractive index material to prepare the mirrors by electron-beam evaporation. The impurities in two kinds of HfO2 starting coating materials and in their corresponding single layer thin films were determined through glow discharge mass spectrum (GDMS) technology and secondary ion mass spectrometry (SIMS) equipment, respectively. It showed that between the two kinds of HfO2, either the bulk materials or their corresponding films, the difference of ZrO2 was much larger than that of the other impurities such as Ti and Fe. It is the Zr element that affects the property of thin films. Both in theoretical and in experimental, the mirror prepared with the HfO2 starting material containing more Zr content has a lower reflectance. Because the extinction coefficient of zirconia is relatively high in UV region, it can be treated as one kind of absorbing defects to influence the optical property of the mirrors. (C) 2008 Elsevier B.V. All rights reserved.

Influence of oxygen post-treatment on laser-induced damage of antireflection coatings prepared by electron-beam evaporation and ion beam assisted deposition

Antireflection coatings at the center wavelength of 1053 nm were prepared on BK7 glasses by electron-beam evaporation deposition (EBD) and ion beam assisted deposition (IBAD). Parts of the two kinds of samples were post-treated with oxygen plasma at the environment temperature after deposition. Absorption at 1064 nm was characterized based on surface thermal lensing (STL) technique. The laser-induced damage threshold (LIDT) was measured by a 1064-nm Nd:YAG laser with a pulse width of 38 ps. Leica-DMRXE Microscope was applied to gain damage morphologies of samples. The results revealed that oxygen post-treatment could lower the absorption and increase the damage thresholds for both kinds of as-grown samples. However, the improving effects are not the same. (c) 2008 Elsevier B.V. All rights reserved.

High refractive index TiO2 film deposited by electron beam evaporation

The well known 'crystal seed' theory is first applied in this work to prepare TiO2 film: a high refractive index rutile TiO2 film is grown by electron beam evaporation on the rutile seed formed by 1100 degrees C annealing. The average n is larger than 2.4, by far the highest in all the authors' TiO2 films. The films are characterised by optical properties, microstructure and surface morphologies. It is found that the refractive index shows positive relation with the crystal structure, grain size, and packing density and roughness of the film. The film has lower density of granularity and nodule defects on the surface than those of the film deposited by magnetron sputtering. The result shows attractive application in complex filter and laser coatings.