Overcoat dependence of laser-induced damage threshold of 355 nm HR coatings

A series of HR coatings, with and without overcoat, were prepared by electron beam evaporation using the same deposition process. The laser-induced damage threshold (LIDT) was measured by a 355 nm Nd:YAG laser with a pulse width of 8 ns. Damage morphologies of samples were observed by Leica-DMRXE Microscope. The stress was measured by viewing the substrate deformation before and after coatings deposition using an optical interferometer. Reflectance of the samples was measured by Lambda 900 Spectrometer. The theoretical results of electric field distributions of the samples were calculate by thin film design software (TFCalc). It was found that SiO₂ overcoat had improved the LIDT greatly, while MgF₂ overcoat had little effect on the LIDT because of its high stress in the HR coatings. The damage morphologies were different among HR coatings with and without overcoats.     

Study on the feasibility of double stack high reflector coating at 355 nm

The feasibility of the idea of double stack HR coating was discussed in this paper both in theory and experiment. The theoretical simulation was made by employing optical coating design software. The analysis results showed that the design of double stack HR coating was feasible, which made the HR coating have ascendancy not only at reflectance but also at laser damage resistance. Then, the LaF₃/MgF₂ HR coating, the HfO₂/SiO₂ HR coating and the double stack HR coating were prepared for comparison, respectively. Transmittance spectra, surface morphologies and damage morphologies of these coatings were measured. Measurement of laser-induced damage threshold (LIDT) of S polarized light of the samples was performed at 355 nm, 45° incidence. The measurement results showed that the LIDT value of the LaF₃/MgF₂ HR coating with 30 layers was very high, but the reflectance was low. When the layer number was increased up to 36, lots of cracks appeared on the surface of the LaF₃/MgF₂ HR coating, with the LIDT badly declining. It was thought that the residual stress resulted in the cracks and the decline of the LIDT. The spectra measurement showed the double stack HR coatings could provide higher reflectance and wider reflection band than LaF₃/MgF₂ HR coating with less layer pairs. Any crack was also not found on the surface of the double stack coatings. Meanwhile, the double stack HR coatings possessed greater laser damage resistances than the HfO₂/SiO₂ HR coating. The damage morphologies showed that the damage of the double stack coating was even milder than that of the HfO₂/SiO₂ coating. Therefore, the double stack design was effective to gain high reflectance and great UV laser radiation resistance simultaneously.     

Calculation of temperature fields with a film-substrate interfacial layer model to discuss the layer-pair number effects on the damage thresholds of LaF3/MgF2 high reflectors at 355 nm

Laser induced damage thresholds (LIDT) of LaF₃/MgF₂ high reflectors at 355 nm were measured and investigated as a function of layer-pair number. Generally, LaF₃/MgF₂ coatings with more layer pairs possessed higher LIDT, but coatings with too high layer-pair number crazed because of high tensile stress, so the LIDT of them decreased badly. The temperature rise in the coatings was calculated based on a film-substrate interfacial absorption model, and the depth of the damage in the coatings were measured by a Veeco optical profilograph. The two characterization methods together were used to interpret the effects of layer-pair number on LIDT, and the damage mechanism of coatings at laser wavelength of 355 nm was also discussed.     

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 355 nm 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 LIDT of Al2O3 thin film.     

Influence of substrate temperature on properties of MgF2 coatings

Thermal boat evaporation was employed to prepare MgF₂ single-layer coatings upon both JGS1 and UBK7 substrates at different substrate temperatures. Microstructure, transmittance and residual stress of these coatings were measured by X-ray diffraction, spectrophotometer, and optical interferometer, respectively. Measurement of laser induced damage threshold (LIDT) of the samples was performed at 355 nm, 8 ns pulses. The results showed that high substrate temperature was beneficial to crystallization of the film. Above 244 °C, the refractive index increased gradually with the substrate temperature rising. Whereas, it was exceptional at 210 °C that the refractive index was higher than those deposited at 244 and 277 °C. The tensile residual stresses were exhibited in all MgF₂ films, but not well correlated with the substrate temperature. In addition, the stresses were comparatively smaller upon JGS1 substrates. A tendency could be seen that the LIDTs reached the highest values at about 244 °C, and the films upon JGS1 had higher LIDTs than those upon UBK7 substrates at the same temperature. Meanwhile, the damage morphologies showed that the laser damage of the coating resulted from an absorbing center at the film-substrate interface. The features of the damages were displayed by an absorbing center dominated model. Furthermore, the reason of the difference in LIDT values was discussed in detail.     

真空退火对355nm Al2O3/MgF2高反射薄膜性能的影响

 采用电子束蒸发沉积技术制备了355nm Al₂O₃/MgF₂ 高反射薄膜，并在真空中进行不同温度梯度的退火，用X射线衍射（XRD）观察了薄膜微结构的变化，用355nm Nd：YAG脉冲激光测试了薄膜的激光损伤阈值，用Lambda 900光谱仪测试了薄膜的透过和反射光谱。结果表明在工艺条件相同的条件下真空退火过程对薄膜的性能有很大的影响，退火温度梯度越小的样品，吸收越小，阈值越大，并且是非晶结构。选择合适的真空退火过程可以减少355nm Al₂O₃/MgF₂ 高反射膜的膜层吸收，提高薄膜的激光损伤阈值。     

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.     

Microstructure and mechanical properties of Al2O3-Al composite coatings deposited by plasma spraying

Al₂O₃ and Al₂O₃-Al composite coatings were prepared by plasma spraying. Phase composition of powders and as-sprayed coatings was determined by X-ray diffraction (XRD), while optical microscopy (OM) and scanning electron microscopy (SEM) were employed to investigate the morphology of impacted droplets, polished and fractured surface, and the element distribution in terms of wavelength-dispersive spectrometer (WDS). Mechanical properties including microhardness, adhesion and bending strength, fracture toughness and sliding wear rate were evaluated. The results indicated that the addition of Al into Al₂O₃ was beneficial to decrease the splashing of impinging droplets and to increase the deposition efficiency. The Al₂O₃-Al composite coating exhibited homogeneously dispersed pores and the co-sprayed Al particles were considered to be distributed in the splat boundary. Compared with Al₂O₃ coating, the composite coating showed slightly lower hardness, whereas the coexistence of metal Al phase and Al₂O₃ ceramic phase effectively improved the toughness, strength and wear resistance of coatings.     

Effect of the deposition parameters on the structure and physicochemical properties of protective Al2O3 coatings

Three series of Al₂O₃ coating samples are fabricated by microarc oxidation under various deposition conditions and are studied by scanning electron microscopy (SEM) in combination with energy-dispersive x-ray spectroscopy (EDXS), Rutherford backscattering, and X-ray diffraction. Defects and pores in the coatings are analyzed by positron annihilation spectroscopy at room temperature without vacuum. No nanometer pores are detected in the coatings. When changing the electrolyte-plasma oxidation conditions, one can change the concentration and the ratio of the types of vacancy defects in these Al₂O₃ coatings.     

Optimization of facet coating for highly strained InGaAs quantum well lasers operating at 1200 nm

The optical output power of a laser diode can be enhanced by anti-reflection (AR) and high-reflection (HR) facet coatings, respectively, at the front and back facet. AR and HR coatings also serve the purpose of protection and passivation of laser diode facets. In this work, we have designed and optimized a single layer λ/4 thick Al₂O₃ film for the AR coating and a stack of λ/4 thick Al₂O₃/λ/4 thick Si bi-layers for the HR coating for highly strained InGaAs quantum-well edge emitting broad area (BA) laser diodes. Effect of the front and back facet reflectivities on output power of the laser diodes has been studied. The light output versus injected current (L–I characteristics) measurements were carried out on selected devices before and after the facet coatings. We have also carried out the numerical simulation and analysis of L–I characteristics for this particular diode structure. The experimental results have been compared and verified with the numerical simulation.     

Preparation and characterization of the electrodeposited Cr-Al2O3/SiC composite coating

To increase the SiC content in Cr-based coatings, Cr-Al₂O₃/SiC composite coatings were plated in Cr(VI) baths which contained Al₂O₃-coated SiC powders. The Al₂O₃-coated SiC composite particles were synthesized by calcining the precursor prepared by heterogeneous deposition method. The transmission electron microscopy analysis of the particles showed that the nano-SiC particle was packaged by alumina. The zeta potential of the particles collected from the bath was up to +23 mV, a favorable condition for the co-deposition of the particles and chromium. Pulse current was used during the electrodeposition. Scanning Electron Microscopy (SEM) indicated that the coating was compact and combined well with the substrate. Energy dispersive X-ray analysis of Cr-Al₂O₃/SiC coatings demonstrated that the concentration of SiC in the coating reached about 2.5 wt.%. The corrosion behavior of the composite coating was studied by potentiodynamic polarization and electrochemical impedance spectroscopy techniques. The data obtained suggested that the Al₂O₃/SiC particles significantly enhanced the corrosion resistance of the composite coating in 0.05 M HCl solution.     

退火对电子束热蒸发193nm Al2O3/MgF2反射膜性能的影响

设计并镀制了193nm Al₂O₃/MgF₂反射膜，对它们在空气中分别进行了250—400℃的高温退火，测量了样品的透射率光谱曲线和绝对反射率光谱曲线.发现样品在高反射区的总的光学损耗随退火温度的升高而下降，而后趋于饱和.采用总积分散射的方法对样品在不同退火温度下的散射损耗进行了分析，发现随着退火温度的升高散射损耗有所增加.因此，总的光学损耗的下降是由于吸收损耗而不是散射损耗起主导作用.对Al₂O₃材料的单层膜进行了同等条件的退火处理，由它们光学性能的变化推导出它们的折射率和消光系数的变化，从而解释了相应的多层膜光学性能变化的原因.反射膜的反射率在优化联系、镀膜工艺与退火工艺的基础上达98％以上. 关键词： 193nm 反射膜 退火 光学损耗 吸收     

Microstructure and properties of Ni-Co/nano-Al2O3 composite coatings by pulse reversal current electrodeposition

Ni-Co/nano-Al₂O₃ (Ni-Co/Al₂O₃) composite coatings were prepared under pulse reversal current (PRC) and direct current (dc) methods respectively. The microstructure of coatings was characterized by means of XRD, SEM and TEM. Both the Ni-Co alloy and composite coatings exhibit single phase of Ni matrix with face-centered cubic (fcc) crystal structure, and the crystal orientation of the Ni-Co/Al₂O₃ composite coating was transformed from crystal face (2 0 0) to (1 1 1) compared with alloy coatings. The hardness, anti-wear property and macro-residual stress were also investigated. The results showed that the microstructure and performance of the coatings were greatly affected by Al₂O₃ content and the electrodeposition methods. With the increasing of Al₂O₃ content, the hardness and wear resistance of the composite coatings enhanced. The PRC composite coatings exhibited compact surface, high hardness, better wear resistance and lower macro-residual stress compared with that of the dc composite coatings.     

Deep UV laser induced luminescence in oxide thin films

Time-resolved luminescence experiments have been set up in order to study the interaction of 193-nm laser radiation with dielectric thin films. At room temperature, Al₂O₃ coatings show photoluminescence upon ArF excimer laser irradiation, with significant intensity contributions besides the known substrate emission. Time- and energy-resolved measurements indicate the presence of oxygen-defect centers in Al₂O₃ coatings, which suggests a strong single-photon interaction at 193 nm by F⁺ and F center absorption. Measurements on highly reflective thin-film stacks, consisting of quarter-wave Al₂O₃ and SiO₂ layers, indicate similar UV excitations, mainly from color centers of Al₂O₃. Received: 20 February 2002 / Accepted: 11 April 2002 / Published online: 5 July 2002     

Far ultraviolet optical properties of MgF2 films deposited by ion-beam sputtering and their application as protective coatings for Al

Thin films of MgF₂ deposited by evaporation is a material widely used for its transparency in the far ultraviolet (FUV) down to ∼115 nm. In this paper the optical properties of ion-beam sputtered (IBS) MgF₂ in the FUV are investigated and compared with MgF₂ films deposited by evaporation. A slightly higher transparency at the 121.6-nm, H Lyman α line was obtained for IBS MgF₂ films compared to films deposited by evaporation, which makes IBS MgF₂ a promising protective material for Al reflective coatings. Experimental work on Al films that were protected with a thin evaporated MgF₂ film followed by an IBS MgF₂ film to produce a protective coating with optimum thickness showed a reflectance at 121.6 nm that was higher by about 3% compared to an Al film protected with an all-evaporated MgF₂ film.     

Effects of duty ratio at low frequency on growth mechanism of micro-plasma oxidation ceramic coatings on Ti alloy

The aim of this work is to study the effects of duty ratio on the growth mechanism of the ceramic coatings on Ti-6Al-4V alloy prepared by pulsed single-polar MPO at 50 Hz in NaAlO₂ solution. The phase composition of the coatings was studied by X-ray diffraction, and the morphology and the element distribution in the coating were examined through scanning electron microscopy and energy dispersive spectroscopy. The thickness of the coatings was measured by eddy current coating thickness gauge. The corrosion resistance of the coated samples was examined by linear sweep voltammetry technique in 3.5% NaCl solution. The changes of the duty ratio (D) of the anode process led to the changes of the mode of the spark discharge during the pulsed single-polar MPO process, which further influenced the structure and the morphology of the ceramic coatings. The coatings prepared at D = 10% were composed of a large amount of Al₂TiO₅ and a little γ-Al₂O₃ while the coatings prepared at D = 45% were mainly composed of α-Al₂O₃ and γ-Al₂O₃. The coating thickness and the roughness were both increased with the increasing D due to the formation of Al₂O₃. The formation of Al₂TiO₅ resulted from the spark discharge due to the breakdown of the oxide film, while the formation of Al₂O₃ resulted from the spark discharge due to the breakdown of the vapor envelope. The ceramic coatings improved the corrosion resistance of Ti-6Al-4V alloy. And the surface morphology and the coating thickness determined the corrosion resistance of the coated samples prepared at D = 45% was better than that of the coated samples prepared at D = 10%.     

F2-laser ablation patterning of dielectric layers

Spatially defined patterning of multi-layer dielectric optical systems by laser-induced ablation is demonstrated. A 49-layer high-reflectivity mirror for 193-nm light was irradiated with F₂-laser light through the CaF₂-substrate to cleanly remove the whole dielectric stack by rear-sided ablation. The 157-nm light is absorbed efficiently by dielectric layers such as SiO₂ and Al₂O₃ that are typically used for ultraviolet (UV) transmission at 193-nm and longer wavelengths. Thus it is possible to ablate highly reflective UV-laser mirrors (HR 193 nm) and to create dielectric masks that withstand high power levels at 193 nm. A single 157-nm pulse with a fluence of less than 500 mJ/cm² is sufficient to cleanly ablate the whole layer stack with sharp edges and without debris deposition. Received: 31 October 2000 / Accepted: 14 November 2000 / Published online: 10 January 2001     

Atmospheric reactive plasma sprayed Fe-Al2O3-FeAl2O4 composite coating and its property evaluation

In the present study, Fe-Al₂O₃-FeAl₂O₄ composite coatings were successfully deposited by reactive plasma sprayed Al/Fe₂O₃ agglomerated powder. Phase composition and microstructure of the coatings were determined by XRD and SEM. The results indicated that the composite coatings were principally composed of three different phases, i.e. FeAl₂O₄ phase as main framework, dispersed ball-like Fe-rich phase, and small splats of Al₂O₃ phase, and it was thought that the in situ synthesized metal phase was helpful to toughen the coating matrix. According to the results of the indentation and frictional wear tests, the composite coating exhibited excellent toughness and anti-friction properties in comparison with conventional Al₂O₃ monophase coating, though its microhardness value was a little lower than that of Al₂O₃ coating. The formation mechanism and the toughening mechanism of the composite coating were clarified in detail.     

Influence of Vacuum Organic Contaminations on Laser-Induced Damage of 1064 nm Anti-Reflective Coatings

We investigate the influence of vacuum organic contaminations on laser-induced damage threshold （LIDT） of optical coatings. Anti-reflective （AIR） coatings at 1064 nm made by Ta2 O5/SiO2 are deposited by the ion beam sputtering method. The LIDTs of AR coatings are measured in vacuum and in atmosphere, respectively. It is exhibited that contaminations in vacuum are easily to be absorbed onto optical surface because of lower pressure, and they become origins of damage, resulting in the decrease of LIDT from 24.5J/cm^2 in air to 15.TJ/cm^2 in vacuum. The LIDT of coatings in vacuum has is slightly changed compared with the value in atmosphere after the organic contaminations are wiped off. These results indicate that organic contaminations are the main reason of the LIDT decrease in vacuum. Additionally, damage morphologies have distinct changes from vacuum to atmosphere because of the differences between the residual stress and thermal decomposability of filmy materials.     

1 053，527，351 nm倍频分离膜的制备与性能研究

 用电子束蒸发及光电极值监控技术在石英基底上沉积了三倍频分离膜，将部分样品置空气中于250 ℃温度下进行3 h热退火处理。然后用Lambda900分光光度计测量了样品的光谱性能；用表面热透镜技术测量了样品的弱吸收值；用调Q脉冲激光装置测试了样品分别在355 nm和1 064 nm的抗激光损伤阈值。实验结果发现，样品的实验光谱性能良好，退火前后其光谱性能几乎没有发生温漂，说明薄膜的温度稳定性好；同时弱吸收平均值从退火前的1.07×10^-4下降到退火后的6.2×10^-5，从而使对基频的抗激光损伤阈值提高，从14.6 J/cm²上升到18.8 J/cm²，但是三倍频阈值在退火后有显著降低，从7.5 J/cm²下降到2.5 J/cm²。