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。

SiO_2薄膜折射率的准确拟合分析

精确的光学常数对于设计和制备高品质的光学薄膜非常重要,尤其是那些光学性能对折射率变化敏感的薄膜。SiO_2是一种常用的低折射率材料,因与常用基底折射率相近使其准确拟合有一定难度。实验通过离子束溅射制备了SiO_2单层膜。考虑测量时的误差和基底折射率的影响,采用透射率包络和反射率包络得到了SiO_2的折射率,并用所得折射率进行反演来对这两种途径在实际测量拟合过程中的准确性进行比对。分析表明,剩余反射率在实际的测量过程中误差更小,直接用测量镀膜前后基片的剩余反射率值可以更简便更准确地得到SiO_2的折射率,能达到10~(-2)的精度。

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.

吸收杂质热辐射诱导光学薄膜破坏的热力机制

光学元件的破坏是限制高功率激光系统发展的主要问题,理解光学元件的破坏机制对于高功率激光系统的设计、运行参量选择以及器件技术发展有重要影响。以热辐射模型为基础研究了杂质吸收诱导光学薄膜破坏的热力过程。研究发现薄膜发生初始破坏所需时间很短,脉冲的大部分时间是引起薄膜发生更大的破坏。在考虑吸收杂质发生相变的情况下,计算了吸收杂质汽化对薄膜产生的蒸汽压力,论证了薄膜发生宏观破坏的可能性。此模型能很好地解释光学薄膜的平底坑破坏形貌。

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.

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.

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。

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。

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.

Occupational exposure to nano-TiO2 in the life cycle steps of new depollutant mortars used in construction

The present work is focused on the measurement of workers exposure to nano-TiO2 in the life cycle steps of depollutant mortars. It has been done in the framework of the SCAFFOLD project, which aims at the management of potential risks arising from the use of manufactured nanomaterials in construction. Main findings can be summarized as follows: (1) The occupational exposure to nano-TiO2 is below 0.3 mg/m(3) for all measured scenarios. The highest concentrations were measured during the cleaning task (in the nano-TiO2 manufacturing process) and during the application (spraying) of depollutant coatings on a wall. (2) It was found a high release of particles above the background in several tasks as expected due to the nature of the activities performed. The maximum concentration was measured during drilling and during adding powder materials (mean total particle concentration up to 5.591E+04 particles/cm(3) and 5.69E+04 particles/cm(3)). However, considering data on total particle concentration released, no striking differences have been observed when tasks have been performed using conventional materials in the sector (control) and when using materials doped with nano-objects.

Eletrodeposição de ligas Zn-Co por corrente contínua e pulsada simples, a partir de banhos ambientalmente não agressivos

Revestimentos produzidos a partir de ligas de Zn-Co são comumente utilizados em indústrias (aeronáutica, de isoladores elétricos e automobilística, por exemplo) devido à sua ótima resistência à corrosão, principalmente quando comparados aos tradicionais revestimentos de Zn puro. Na co-deposição de zinco com metais, como o ferro, cobalto e níquel, ocorre o que se chama de deposição anômala, onde o metal menos nobre (zinco) é preferencialmente depositado, independente do modo de corrente aplicada (contínua ou pulsada). Recentemente, diversos trabalhos relacionam a produção de eletrodepósitos de liga Zn-Co a partir de banhos ambientalmente não agressivos, a fim de substituir os banhos alcalinos extremamente tóxicos, a base de cianeto. Na presente dissertação foram produzidos revestimentos de ligas de Zn-Co sobre substrato de aço carbono, empregando corrente contínua ou corrente pulsada simples, a partir de banhos contendo diferentes concentrações de Co2+ (0,05 mol/L e 0,10mol/L), 0,05 mol/l de Zn2+ e citrato de sódio (0,10 mol/L) como agente complexante, sob condições agitadas. Quatro diferentes valores de densidade de corrente (10 A/m2, 20 A/m2, 40 A/m2 e 80 A/m2) e de frequência de pulso (100 Hz, 500 Hz, 1000 Hz, 2000 Hz) foram aplicados para a produção da liga a partir dos dois banhos, tendo como objetivo avaliar a influência dos parâmetros de deposição(concentração de Co (II), densidade de corrente aplicada e, no caso de deposição por corrente pulsada simples, também da frequência de pulso), nas variáveis eficiência de corrente catódica, composição da liga, densidade de corrente de corrosão, microestrutura e morfologia dos depósitos de liga Zn-Co. As cores das camadas obtidas variaram do cinza claro ao escuro, quase sempre sem brilho, independente do modo de corrente empregado. Foi verificado que o processo normal de eletrodeposição foi prevalente na produção de revestimentos por corrente contínua, enquanto que apenas deposição anômala foi observada quando do uso de corrente pulsada. A maior eficiência de corrente catódica (60%) foi obtida, para corrente contínua, nas condições de menor concentração de Co2+ (0,05 mol/L) e maior densidade de corrente (80 A/m2). Nestas mesmas condições foi determinada uma eficiência de corrente catódica de 98% para corrente pulsada simples na freqüência de 2000 Hz. Maiores teores do metal mais nobre (cobalto) foram alcançados em maiores densidades de corrente para todas as condições empregadas. Os revestimentos assim obtidos apresentavam os menores valores de tamanho de grão, para cada uma das soluções estudadas. Os demais parâmetros estudados também influenciaram na granulometria e na morfologia das ligas obtidas. Revestimentos com melhor resistência à corrosão, contendo teores de cobalto entre aproximadamente 8 e 10% m/m, foram produzidos a partir do banho com maior concentração de Co2+, sob corrente pulsada simples