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。     

高折射率光学薄膜的化学法制备研究

 报道了一种以ZrOC₁₂·8H₂O为源,溶胶-凝胶法制备高激光负载高折射率薄膜的新方法。薄膜采用旋转镀膜法制备,对薄膜的结构、光学特性及激光损伤阈值进行了测量,有机粘接剂对薄膜折射率及机械强度的影响也作了探讨。以该薄膜与SiO₂溶胶凝胶膜交替涂覆制成的多层高反膜,剩余透过率仅0.98%,激光损伤阈值达16J/cm²（3ns）。     

化学法制备的HfO2薄膜的激光损伤阈值研究

 采用化学法制备了HfO₂介质膜，研究了热处理、紫外辐照以及Al₂O₃复合对HfO₂介质膜激光损伤阈值的影响。采用红外光谱（FTIR）和X射线衍射仪对薄膜进行了表征，并用输出波长为1.064 μm、脉宽为10 ns的电光调Q激光系统测试薄膜的激光损伤阈值。实验结果表明：采用150 ℃左右的温度对薄膜进行热处理可以提高薄膜的激光损伤阈值，所获得的薄膜的激光损伤阈值高达42.32 J/cm²，比热处理前的激光损伤阈值提高了82%；无机材料Al₂O₃的适量添加能够提高薄膜的激光损伤阈值，其中HfO₂与Al₂O₃的最佳质量配比约为95∶5；另外，对薄膜进行适当的紫外辐照也可改善HfO₂ 薄膜以及HfO₂-Al₂O₃复合薄膜的抗激光损伤性能。紫外辐照对提高HfO₂-Al₂O₃复合薄膜的激光损伤阈值效果尤为显著，辐照40 min后的激光损伤阈值达到44.33 J/cm²，比紫外辐照前的激光损伤阈值提高了90%。     

氧分压对ZrO2薄膜激光损伤阈值的影响

 在不同的氧分压下用电子束热蒸发的方法制备了ZrO₂薄膜。分别通过X射线衍射、光学光谱、热透镜技术、抗激光辐照等测试，对所制备样品的微结构、折射率、吸收率及激光损伤阈值进行了测量。实验结果表明，薄膜中晶粒主要是四方相为主的多晶结构，并且随着氧分压的增加，结晶度、折射率以及弱吸收均逐渐降低。薄膜的激光损伤阈值开始随着氧分压增加从18.5J/cm²逐渐增加，氧分压为9×10^-3Pa时达到最大，值为26.7 J/cm²，氧分压再增加时则又降低到17.5 J/cm²。由此可见，氧分压引起的薄膜微结构变化是ZrO₂薄膜激光损伤阈值变化的主要原因。     

ZrO2薄膜的改性与抗激光损伤研究

 采用水热合成技术，制备了ZrO₂胶体，用旋涂法镀制了单层ZrO₂介质膜以及添加了有机粘合剂PVP的复合ZrO₂-PVP薄膜。采用X射线衍射(XRD)、椭偏仪、红外分光光度计（FTIR）、原子力显微镜（AFM）等仪器对干凝胶及薄膜进行了性能测试和表征，并用输出波长为1.064 μm、脉宽为10 ns的电光调Q激光系统产生的强激光测试其激光损伤阈值。测得ZrO₂和ZrO₂-PVP薄膜在300 ℃热处理60 min后的激光损伤阈值分别为24.5 J/cm²和37.8 J/cm²。研究表明：添加有机粘合剂后的复合薄膜具有平整的表面结构；有机粘合剂的添加有助于提高薄膜的折射率和激光损伤阈值，其中，ZrO₂-PVP 复合薄膜的折射率可高达1.75，激光损伤阈值达到37.8 J/cm²，比ZrO₂单层膜的激光损伤阈值提高50%。     

物理法和化学法制备的单层ZrO2膜的激光损伤行为差异

 分别采用电子束热蒸发技术和溶胶-凝胶技术在K9基片上镀制了光学厚度相近的ZrO₂单层薄膜,测试了两类薄膜的激光损伤阈值。分别采用透射式光热透镜技术、椭偏仪、原子力显微镜和光学显微镜研究了两类薄膜的热吸收、孔隙率、微观表面形貌、激光辐照前薄膜的杂质和缺陷状况以及激光辐照后薄膜的损伤形貌。实验结果表明：两类薄膜的不同损伤形貌与薄膜的热吸收与微观结构有关， 物理法制备的ZrO₂膜结构致密紧凑，膜层的杂质和缺陷多；化学法制备的ZrO₂膜结构疏松多孔，膜层纯净杂质少，激光损伤阈值达26.9 J/cm²；因物理法制备的ZrO₂膜拥有更大的热吸收(115.10×10^-6)和更小的孔隙率(0.20)，其激光损伤阈值较小(18.8 J/cm²)，损伤主要为溅射和应力破坏，而化学法制备的ZrO₂膜的损伤主要为剥层。理论上对实验结果进行了解释。     

真空环境下光学薄膜的激光损伤

利用1-on-1损伤测试方法,比较研究了电子束沉积制备的几种薄膜在真空、大气环境下的损伤特性,并对真空环境与大气环境损伤的差异进行了分析。研究结果显示:真空环境下的损伤阈值明显低于大气环境下的损伤阈值,真空环境下的破斑形貌也与大气环境下的破斑形貌有显著差异。气体热传导差异不是真空环境与空气环境下损伤差异的原因。由水的解吸而引起膜层在真空环境中张应力的增大及真空环境中激光辐照过程中产生的非化学计量比缺陷是导致电子束沉积的薄膜真空与大气环境中损伤差异的原因。     

1 064 nm高反射薄膜激光损伤阈值测量方法

 参照国际上对激光损伤阈值不同测量技术建立起来的相应检测规范和标准,分别采用1-on-1,S-on-1,R-on-1和光栅扫描共4种测量方式,在1 064 nm波长下对HfO₂/SiO₂周期性高反射薄膜进行了激光损伤阈值的测量研究。根据测量结果,比较并分析了这4种测量方式之间的差异,重点研究了R-on-1和光栅扫描测量方式中存在的激光预处理效应对薄膜损伤阈值的影响,以及辐照激光光斑尺寸与损伤阈值之间的联系,并讨论了光栅扫描方式中预处理效应与扫描间距和扫描能量密度梯度的关系。研究表明：R-on-1方式下测得的损伤阈值最高,光栅扫描和1-on-1次之,S-on-1最小;1 000个脉冲激光辐照下的累积效应不显著,并且在激光光斑尺寸的差异较小时,阈值与光斑尺寸的对应关系并不明显;光斑尺寸相同时,扫描光斑的间距越小,激光预处理效果越好。     

SiO2内保护层对LiB3O5晶体倍频增透膜损伤阈值的影响

 利用离子辅助电子束沉积方法在LiB₃O₅基底上镀制了不加SiO₂内保护层和加SiO₂内保护层的倍频增透膜，测量了两类薄膜在波长1 064 nm多脉冲辐照下的激光损伤阈值，获得了两种不同的损伤形貌，并对损伤原因作了初步探讨。实验结果表明：保护层的加入把由基底膜层界面缺陷吸收所决定的阈值改变到由HfO₂膜层内缺陷吸收所决定的阈值，显著提高了倍频增透膜的抗激光损伤能力。     

SiO2半波覆盖层对HfO2/SiO2高反膜激光损伤的影响

 研究了SiO₂半波覆盖层对HfO₂/SiO₂高反射膜1064nm激光损伤的影响,分析薄膜的激光损伤特性及图貌得出, 对于单脉冲（1-ON-1）激光损伤,SiO₂半波覆盖层能提高HfO₂/SiO₂高反膜的激光损伤阈值;可显著降低激光损伤程度,减小灾难性损伤发生的概率;可大幅度提高HfO₂/SiO₂高反膜膜的抗激光损伤能力。     

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 CO₂ 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.     

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.     

PVP掺杂-ZrO2溶胶-凝胶工艺制备多层激光高反射膜的研究

以丙醇锆(ZrPr)为锆源，二乙醇胺(DEA)为络合剂，原位引入聚乙烯吡咯烷酮(PVP)，在乙醇体系中成功地合成了PVP掺杂-ZrO₂溶胶.采用旋涂法在K9玻璃基片上制备了PVP-ZrO₂单层杂化薄膜.用不同掺杂量的PVP-ZrO₂高折射率膜层与相同的SiO₂低折射率膜层交替沉积四分之一波堆高反射膜.借助小角X射线散射研究胶体微结构，用红外光谱、原子力显微镜、紫外/可见/近红外透射光谱、椭圆偏振仪以及1064nm的强激光辐照实验对薄膜的结构、光学和抗激光损伤性能进行表征.研究发现，体系组成的适当配置可以在溶胶稳定的前提下实现ZrPr的充分水解，赋予薄膜良好的结构、光学和抗激光损伤性能.杂化体系中，DEA与ZPr之间强的配合作用大大降低了ZrO₂颗粒表面羟基的活性，使得PVP大分子只是以微弱的氢键与颗粒的表面羟基作用而均匀分散于ZrO₂颗粒的周围，对颗粒的形成和生长无显著影响.因而在实验研究范围内，随PVP含量的增大，PVP-ZrO₂杂化膜层的折射率和激光损伤阈值均无显著变化.但是，薄膜中均匀分布的PVP柔性链可以有效促进膜层应力松弛，显著削弱不同膜层之间的应力不匹配程度、大大方便多层光学薄膜的制备.当高折射率膜层中PVP的质量分数达到15%—20%时，膜层之间良好的应力匹配使得多层高反射膜的沉积周期数可达到10以上.沉积10个周期的多层反射膜，在中心波长1064nm处透射率约为1.6%—2.1%，接近全反射特征，其激光损伤阈值为16.4—18.2J/cm²(脉冲宽度为1ns). 关键词： 溶胶-凝胶 2')" href="#">PVP-ZrO₂ 高反射膜 激光损伤     

Stress, absorptance and laser-induced damage threshold properties of 355-nm HR coatings

A number of 355-nm Al₂O₃/MgF₂ high-reflectance (HR) coatings were prepared by electron-beam evaporation. The influences of the number of coating layers and deposition temperature on the 355-nm Al₂O₃/MgF₂ HR coatings were investigated. The stress was measured by viewing the substrate deformation before and after coating deposition using an optical interferometer. The laser-induced damage threshold (LIDT) of the samples was measured by a 355-nm Nd:YAG laser with a pulse width of 8 ns. Transmittance and reflectance of the samples were measured by a Lambda 900 spectrometer. It was found that absorptance was the main reason to result in a low LIDT of 355-nm Al₂O₃/MgF₂ HR coatings. The stress in Al₂O₃/MgF₂ HR coatings played an unimportant role in the LIDT, although MgF₂ is known to have high tensile stress.     

Impact of organic contamination on laser-induced damage threshold of high reflectance coatings in vacuum

The influence of organic contamination in vacuum on the laser-induced damage threshold (LIDT) of coatings is studied. TiO₂/SiO₂ dielectric mirrors with high reflection at 1064 nm are deposited by the electron beam evaporation method. The LIDTs of mirrors are measured in vacuum and atmosphere, respectively. It is found that the contamination in vacuum is easily attracted to optical surfaces because of the low pressure and becomes the source of damage. LIDTs of mirrors have a little change in vacuum compared with in atmosphere when the organic contamination is wiped off. The results indicate that organic contamination is a significant reason to decrease the LIDT. N₂ molecules in vacuum can reduce the influence of the organic contaminations and prtectect high reflectance coatings.     

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.     

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.     

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.     

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.     

Non-destructive reading of laser-induced single-shot incubation in dielectric coatings

Two-dimensional photothermal displacement measurements were carried out on TiO₂, ZrO₂, and HfO₂ coatings to uncover single shot incubation produced by 248 nm laser light at fluences below the damage threshold. The incubation behavior of the three coatings differs and correlates with the ratio of band gap to photon energy. The non-destructive nature of the photothermal displacement technique, its high lateral resolution, and its sensitivity for reading single shot imprints by an excimer laser lends this scheme a capacity for use in optical storage.Alexander von Humboldt fellow 1991/92