Laser conditioning and multi-shot laser damage accumulation effects of HfO2/SiO2 antireflective coatings

Laser conditioning effects of the HfO2/SiO2 antireflective (AR) coatings at 1064 nm and the accumulation effects of multishot laser radiation were investigated. The HfO2/SiO2 AR coatings were prepared by E-beam evaporation (EBE). The singleshot and multi-shot laser induced damage threshold was detected following ISO standard 11254-1.2, and the laser conditioning was conducted by three-step raster scanning method. It was found that the single-shot LIDT and multi-shot LIDT was almost the same. The damage mostly > 80% occurred in the first shot under multi-shot laser radiation, and after that the damage occurring probability plummeted to < 5%. There was no obvious enhancement of the laser damage resistance for both the single-shot and multi-shot laser radiation of the AR coatings after laser conditioning. A Nomarski microscope was employed to map the damage morphology, and it found that the damage behavior is defect-initiated for both unconditioned and conditioned samples. © 2004 Elsevier B.V. All rights reserved.

HfO2 膜料中的杂质对薄膜损伤及性能的影响

By analysis of impurity elements in HfO2 coating material, the influence of main impurity elements on the characteristic of coatings were studied. The results indicate that the metal elements and absorptive dielectric elements damage the HfO2 coatings. The more the Zr element content is, the more the absorption is for the coatings in ultraviolet wave. The negative ion element will become the gas source center and form an ejection in the process of evaporation of coating material, so decrease the damage threshold of the coatings.

Influence of negative ion element impurities on laser induced damage threshold of HfO2 thin film

Negative ion element impurities breakdown model in HfO2 thin film was reported in this paper. The content of negative ion elements were detected by glow discharge mass spectrum analysis (GDMS); HfO2 thin films were deposited by the electron-beam evaporation method. The weak absorption and laser induced damage threshold (LIDT) of HfO2 thin films were measured to testify the negative ion element impurity breakdown model. It was found that the LIDT would decrease and the absorption would increase with increasing the content of negative ion element. These results indicated that negative ion elements were harmful impurities and would speed up the damage of thin film. (c) 2006 Elsevier B.V. All rights reserved.

Optical, structural and laser-induced damage threshold properties of HfO2 thin films prepared by electron beam evaporation

We prepare HfO2 thin films by electron beam evaporation technology. The samples are annealed in air after deposition. With increasing annealing temperature, it is found that the absorption of the samples decreases firstly and then increases. Also, the laser-induced damage threshold (LIDT) increases firstly and then decreases. When annealing temperature is 473K, the sample has the highest LIDT of 2.17J/cm(2), and the lowest absorption of 18 ppm. By investigating the optical and structural characteristics and their relations to LIDT, it is shown that the principal factor dominating the LIDT is absorption.

沉积温度对电子束蒸发HfO2薄膜残余应力的影响

采用电子束蒸发沉积方法在BK7玻璃基底和熔融石英基底上沉积了HfO2薄膜，研究了不同沉积温度下的应力变化规律。利用ZYGO干涉仪测量了基片镀膜前后曲率半径的变化，计算了薄膜应力。结果发现在所考察的实验条件下HfO2薄膜的残余应力均为张应力，应力值随沉积温度的升高先增大后减小。两种基底上薄膜的残余应力的主要产生机制不同。对于BK7玻璃基底HfO2薄膜的残余应力起决定作用的是内应力，熔融石英基底上HfO2薄膜的残余应力在较低沉积温度下制备的薄膜起决定作用的是热应力，在沉积温度进一步升高后内应力开始起决定作用。

Damage on HfO2/SiO2 high-reflecting coatings under single and multiple Nd:YAG laser pulse irradiation

The single- and multi-shot damage behaviors of HfO2/SiO2 high-reflecting (HR) coatings under Nd:YAG laser exposure were investigated. Fundamental aspects of multi-shot laser damage, such as the instability due to pulse-to-pulse accumulation of absorption defect and structural defect effect, and the mechanism of laser induced defect generation, are considered. It was found in multi-shot damage, the main factors influencing laser-induced damage threshold (LIDT) are accumulation of irreversible changes of structural defects and thermal stress that induced by thermal density fluctuations.

HfO2薄膜的结构对抗激光损伤阈值的影响

利用蒸发氧化铪和离子辅助蒸发金属铪反应沉积氧化铪薄膜，对两种工艺下制备的氧化铪薄膜进行光学和结构以及激光损伤特性的研究，实验结果表明，用金属铪反应沉积的氧化铪薄膜不仅结构均匀，并且具有较高的激光损伤阈值．文章对损伤阈值和薄膜的结构及光学特性之间的关系进行了讨论。

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.

沉积温度对HfO2薄膜残余应力的影响

用电子柬蒸发方法制备了HfO2薄膜，根据镀膜前后基片曲率半径的变化，用Stoney公式计算了薄膜应力。讨论了沉积温度对薄膜残余应力的影响。结果发现，HfO2薄膜的残余应力均为张应力，应力值随沉积温度的升高先增大后减小，在280℃左右出现极大值。对样品进行了XRD测试，从微观结构上对实验结果进行了分析，发现微结构演变引起的内应力变化是引起薄膜残余应力改变的主要因素，HfO2薄膜在所选沉积温度60～350℃内出现了晶态转变，堆积密度随温度升高而增大。

高真空室中的水蒸气对HfO2薄膜性能的影响

本文研究了在镀膜过程中真空室内水蒸气的含量对HfO2薄膜物理性能的影响。用电子束蒸发和光电极值监控的方法在BK7基底上制备HfO2薄膜。利用残余气体分析仪在线监测了真空室内的残余气氛组成。分别用Lambda 900光谱仪、X射线衍射方法、表面热透镜技术和1064nm的激光器测试了薄膜的光学性能、微结构、吸收和激光损伤阈值。实验发现，附加冷阱装置有助于我们有效控制镀膜过程中的水汽含量，且在水蒸气含量较少的真空室内镀制的薄膜具有较高的折射率，较小的晶粒尺寸，较低的弱吸收值和较高的损伤阈值。

Influences of annealing on residual stress and structure of HfO2 films

HfO2 Elms are deposited on BK7 glass substrates by electron beam evaporation. The influences of annealing between 100 degrees C and 400 degrees C on residual stresses and structures of HfO2 films are studied. It is found that little differences of spectra, residual stresses and structures are obtained after annealing at lower temperatures. After annealing at higher temperatures, the spectra shift to short wavelength, the residual stress increases with the increasing annealing temperature. At the same time, the crystallite size increases and interplanar distance decreases. The variations of optical spectra and residual stress correspond to the evolutions of structures induced by annealing.

Comparison of femtosecond and nanosecond laser-induced damage in HfO2 single-layer film and HfO2-SiO2 high reflector

HfO2 single layers, 800 run high-reflective (HR) coating, and 1064 ran HR coating were prepared by electron-beam evaporation. The laser-induced damage thresholds (LIDTs) and damage morphologies of these samples were investigated with single-pulse femtosecond and nanosecond lasers. It is found that the LIDT of the HfO2 single layer is higher than the HfO2-SiO2 HR coating in the femtosecond regime, while the situation is opposite in the nanosecond regime. Different damage mechanisms are applied to study this phenomenon. Damage morphologies of all samples due to different laser irradiations are displayed. (c) 2007 Optical Society of America.

Effect of SiO2 protective layer on the femtosecond laser-induced damage of HfO2/SiO2 multilayer high-reflective coatings

Two kinds of HfO2/SiO2 800 nm high-reflective (HR) coatings, with and without SiO2 protective layer were deposited by electron beam evaporation. Laser-induced damage thresholds (LIDT) were measured for all samples with femtosecond laser pulses. The surface morphologies and the depth information of all samples were observed by Leica optical microscopy and WYKO surface profiler, respectively. It is found that SiO2 protective layer had no positive effect on improving the LIDT of HR coating. A simple model including the conduction band electron production via multiphoton ionization and impact ionization is used to explain this phenomenon. Theoretical calculations show that the damage occurs first in the SiO2 protective layer for HfO2/SiO2 HR coating with SiO2 protective layer. The relation of LIDT for two kinds of HfO2/SiO2 HR coatings in calculation agrees with the experiment result. (c) 2006 Elsevier B.V. All rights reserved.

两种后处理方法对HfO2薄膜性能的影响

利用电子束蒸发和光电极值监控技术制备了氧化铪薄膜，并分别用两种后处理方法（空气中退火和氧等离子体轰击）对样品进行了处理．然后，对样品的透过率、吸收和抗激光损伤阈值进行了测试分析．实验结果表明，两种后处理方法都能不同程度地降低了氧化铪薄膜的吸收损耗、提高了抗激光损伤阈值．实验结果还表明，氧等离子体轰击的后处理效果明显优于热退火，样品的吸收平均值在氧等离子体后处理前后分别为34．8ppm和9．0ppm，而基频（1 064nm）激光损伤阈值分别为10．0J／cm^2和21．4J／cm^2．

薄膜厚度对HfO2薄膜残余应力的影响

HfO2薄膜是用电子束蒸发方法制备的，利用ZYGO干涉仪测量了基片镀膜前后曲率半径的变化，计算了薄膜应力。对样品进行了XRD测试，讨论了膜厚对薄膜残余应力的影响。结果发现不同厚度HfO2薄膜的残余应力均为张应力，应力值随薄膜厚度的增加而减小，当薄膜厚度达到一定值后，应力值趋于稳定。从微观结构变化对实验结果进行了分析，发现微结构演变引起的本征应力变化是引起薄膜残余应力改变的主要因素。