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.

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．

LBO晶体上1064，532nm倍频增透膜的镀制及性能分析

用电子束蒸发沉积方法在X切LBO（X-LBO）晶体上镀制了两种不同膜系结构的1064和532nm倍频增透膜，其中一种膜系结构为基底／ZrO2／Y2O3／A12O3／SiO2／空气，另一种为基底／0．5Al2O3／ZrO2／Y2O3／A12O3／SiO2／空气，两种膜系结构的主要差别在于有无氧化铝过渡层。测量了薄膜的反射率光谱曲线，发现两种增透膜在1064和532nm处的反射率均小于0．5％，实际镀制结果与理论设计曲线的差异主要是由材料折射率的变化引起的。且对样品在空气环境中进行了温度为473K的退火处理，

沉积速率对热舟蒸发LaF3薄膜性能的影响

用热舟蒸发方法在不同的沉积速率下制备了LaF3单层膜,并对部分单层膜进行了真空退火。分别采用X射线衍射(XRD),Lambda 900 光谱仪和355 nm Nd∶YAG脉冲激光测试了薄膜的晶体结构、透射光谱和激光损伤阈值(LIDT),并通过透射光谱计算得到样品的折射率和消光系数。实验结果表明,增大沉积速率有利于LaF3薄膜的结晶和择优生长,可以提高薄膜的致密性和折射率,但薄膜的抗激光损伤能力有所下降;沉积速率太大,又会恶化薄膜的结晶性能,同时薄膜中产生大量孔洞,薄膜的机械强度降低,导致薄膜的折射率减小和

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。

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。

355nm增透膜的设计、制备与性能

用热舟蒸发法结合修正挡板技术制备了355 nm LaF3/MgF2增透膜,并对部分样品进行了真空退火。采用Lambda 900光谱仪测试了增透膜的低反光谱和透射光谱,并考察了其光谱稳定性;使用脉冲8 ns的355 nm激光测试了增透膜的激光损伤阈值(LIDT);采用Normarski显微镜对增透膜的表面缺陷密度和破斑形貌进行了观察。实验结果表明,制备得到的增透膜的剩余反射率较低,光谱稳定性好;真空退火对增透膜的激光损伤阈值没有改善;增透膜的破环形貌为散点形式,结合破斑深度测试表明薄膜的破坏源于薄膜和基底界面的缺陷点。JGS1熔石英基底由于有好的表面状况、固有的高激光损伤阈值和以其为基底的增透膜具有更低的表面场强,使得其上的增透膜有更高的抗激光损伤能力。

Influence of laser preconditioning on the capacity of optical films to resist laser-induced damage

As a technique to improve the ability of optical films to resist laser-induced damage (ARLID), laser preconditioning has been investigated broadly. In this paper, the laser preconditioning effect has been analyzed based on the defect-initialized damage mechanism that the author had put forward previously. Theoretical results show that an energy density scope (PEDS) exists in which the preconditioning laser can effectively improve the ARLID of optical films. In addition, when the energy density of the testing laser pulse is altered, the boundary of PEDS will change accordingly. Experimental results have verified these theoretical assumptions. PEDS will also become wider if the critical energy density of the preconditioning laser that can induce films' micro-damage increases, or the critical energy density of the preconditioning laser that can cause laser annealing decreases. In these cases, it is relatively easy to improve the ARLID of optical films. Results of the current work show great significance in enhancing the ARLID of optical films through the laser preconditioning technique. (C) 2008 Elsevier B.V. All rights reserved.

Influence of substoichiometer on the laser-induced damage characters of HfO2 thin films

HfO2 is one of the most important high refractive index materials for depositing high power optical mirrors. In this research, HfO2 thin films were prepared by dual-ion beam reactive sputtering method, and the laser-induced damage thresholds (LIDT) of the sample were measured in 1-on-1 mode for laser with 1064 nm wavelength. The results indicate that the LIDT of the as-grown sample is only 3.96 J/cm(2), but it is increased to 8.98 J/cm(2) after annealing under temperature of 200 degrees C in atmosphere. By measuring the laser weak absorption and SIMS of the samples, we deduced that substoichiometer is the main reason for the low LIDT of the as-grown sample, and the experiment results were well explained with the theory of electronic-avalanche ionization. (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.

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.

Síntese e caracterização de TiO2 puro e modificado para aplicações ambientais

Fotocatalisadores baseados em nanopartículas de dióxido de titânio modificados fornecem soluções em potencial para a mineralização de poluentes orgânicos em meio aquoso. Agentes modificadores têm sido amplamente investigados com o objetivo de promover a fotoativação pela luz visível. Foram estudadas a nível fundamental até aqui, as modificações estruturais, texturais e óticas causadas pela introdução de silício e nitrogênio na rede da titânia. Titânias puras (TiO2) e modificadas nanoestruturadas, particularmente titânias modificadas com silício (TiO2-SiO2), com razões atômicas Si/Ti de 0,1, 0,2 e 0,3 foram sintetizadas pelo método sol-gel a partir da hidrólise ácida de isopropóxido de titânio(IV) e tetraetoxisilano. As metodolo-gias sintéticas desenvolvidas tentaram aderir aos princípios da Química Verde, dispensando o uso de atmosfera inerte e temperatura e pressão elevadas, o que foi alcançado utilizando-se, principalmente, a agitação ultrassônica. Titânias modificadas com silício e dopadas com ni-trogênio (TiO2-SiO2-N) foram obtidas a partir do pré-tratamento de TiO2-SiO2 a 500 C ao ar e então submetidas ao fluxo de amônia (NH3) a 600 C por 1-3 h e, após resfriamento, foram recozidas a 400 C ao ar. Amostras distintas foram caracterizadas, na forma de pó seco e após calcinação entre 400600 C, por difração de raios X, adsorção de nitrogênio, microscopia eletrônica de varredura e espectroscopia de refletância difusa no UV-Visível. As titânias pu-ras, obtidas principalmente variando-se a razão de hidrólise, foram cristalizadas na forma de anatásio como fase predominante até 600 C, além de traços de brookita presente até 500 C. O rutilo foi identificado a partir de 600 C como fase minoritária, embora apresentando tama-nhos de cristal significativamente maiores que os estimados para o cristal de anatásio. As titâ-nias modificadas com até 20% de silício apresentaram notável estabilidade térmica, evidenci-ada pela presença exclusiva de anatásio até 900 C. Foi também observado o aparecimento de macroporos com diâmetro médio em torno de 55 nm após calcinação a 400 C, diferentemente do que se observou nas amostras em geral. A introdução de baixo teor de silício assegurou às titânias calcinadas valores elevados de área específica, atribuído ao efeito de contenção acentuada na taxa de crescimento do cristal. As titânias modificadas com silício e as titânias puras obtidas com taxa de hidrólise 25:1 para a razão H2O : Ti apresentaram mesoporos com diâmetros médios de mesma dimensão do cristal. As titânias modificadas com silício e dopa-das com nitrogênio apresentaram absorção na região visível entre 400-480 nm, com discreta redução da energia de band gap para as transições eletrônicas consideradas. Titânias calcina-das a 300−400 C apresentaram desempenho fotocatalítico semelhante ao TiO2 P25 da De-gussa sob irradiação UV, na degradação do azo corante Reactive Yellow 145 em soluções a-quosas em pH 5 a 20 1C