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%。     

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。     

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%。     

ZrO2/ SiO2多层膜的化学法制备研究

 分别以ZrOCl₂·8H₂O 和正硅酸乙酯为原料,采用溶胶-凝胶工艺制备了性能稳定的ZrO₂和SiO₂溶胶。用旋转镀膜法分别在K9玻璃和单晶硅片上制备了ZrO₂/ SiO₂多层膜。采用溶剂替换和紫外光处理等手段,有效地解决了ZrO₂/SiO₂多层膜中膜层开裂和膜间渗透等问题。应用扫描电子显微镜观测了薄膜的表面和剖面微观形貌,并用椭偏仪测得薄膜的厚度和折射率,研究了薄膜厚度、折射率与热处理温度、紫外光处理时间的关系,对所获得薄膜的紫外-可见、红外光谱进行了分析。用输出波长1064nm ,脉宽15ns 的电光调Q光系统产生的强激光进行了单层膜的辐照实验,结果发现溶剂替换后激光损伤阈值有所提高。     

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。     

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。     

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。     

用1064nm激光增强HfO2/SiO2薄膜的抗激光损伤能力的实验研究

 用1 064nm激光实验研究了HfO₂/SiO₂薄膜的激光损伤增强效应，实验以薄膜激光损伤阈值70%的激光能量开始，采用N-ON-1方式处理薄膜，激光脉冲的能量增量为5J/cm²。实验结果表明，激光处理薄膜表面能使激光损伤阈值平均提高到3倍左右，并且薄膜的损伤尺度也明显减小。对有缺陷的薄膜，其缺陷经低能量激光后熔和消除，其抗激光损伤能力得到增强，但增强得并不显著，而薄膜本身的激光预处理，可以使其激光损伤阈值大大提高。     

波长1064nm脉冲激光高阈值反射膜的研制

 研究HfO₂/SiO₂高反射膜的制备工艺及其激光诱导损伤阈值的比较测试,分别采用了反应蒸镀HfO₂、反应离子辅助蒸镀HfO₂、反应离子辅助蒸镀金属Hf的源材料形成HfO₂薄膜。采用这三种工艺制备了HfO₂/SiO₂高反射膜,在中心波长1064nm处,反射率 R≥99.5%,其中反应蒸镀HfO₂/SiO₂高反射膜损伤阈值最高,可达60J/cm²(1064nm,5ns)。     

飞秒激光烧蚀LiNbO3晶体的形貌特征与机理研究

采用了不同能量的单脉冲和多脉冲飞秒激光对LiNbO₃晶体进行烧蚀，并刻蚀了表面衍射型光栅.通过扫描电镜和原子力显微镜观察了烧蚀点的形貌特征，首次发现利用单束飞秒激光脉冲对LiNbO₃晶体烧蚀，可以得到超衍射极限的烧蚀点，当聚焦光斑直径约为2μm、能量为170nJ的单脉冲飞秒激光作用时，烧蚀点的直径约为400nm，100nJ，17个脉冲作用时烧蚀点的直径约为800nm.同时可以观察到在能量较低的多脉冲飞秒激光作用下， LiNbO₃晶体呈现出大约200nm周期性分布的波纹状结构.实验结果表明，选择合适参数的飞秒激光脉冲可以对LiNbO₃晶体进行超衍射极限加工，这对于利用飞秒激光制作LiNbO₃基质的微纳光电子器件有十分重要的意义.     

Laser-induced damage threshold in n-on-1 regime of Ta2O5 films at 532, 800, and 1064 nm

Ta2O5 films were prepared with conventional electron beam evaporation and annealed in O2 at 673 K for 12 h. Laser-induced damage thresholds (LIDTs) of the films were performed at 532 and 1064 nm in 1-on-1 regime firstly, and then were performed at 532, 800, and 1064 nm in n-on-1 regime, respectively.The results showed that the LIDTs in n-on-1 regime were higher than that in 1-on-1 regime at 532 and 1064 nm. In addition, in n-on-1 regime, the LIDT increased with the increase of wavelength. Furthermore, both the optical property and LIDT of Ta2O5 films were influenced by annealing in O2.     

原子层沉积HfO_2薄膜的激光损伤特性分析

以目前激光惯性约束聚变中应用最广泛的高折射率材料二氧化铪(HfO2)为研究对象,在熔石英基底上分别采用TEMAH和HfCl4前驱体制备了HfO2薄膜,沉积温度分别为100,200和300℃。采用椭偏仪和激光量热计对薄膜的光学性能进行了测量分析,采用X射线衍射仪(XRD)对薄膜的微结构进行了测量。最后在小口径激光阈值测量平台上按照1-on-1测量模式对薄膜的损伤阈值进行了测试,并采用扫描电子显微镜(SEM)对损伤形貌进行了分析。研究表明,用同一种前驱体源时,随着沉积温度升高,薄膜折射率增加,吸收增多,损伤阈值降低。在相同温度下,采用有机源制备的薄膜更容易在薄膜内部形成有机残留,导致薄膜吸收增加,损伤阈值降低。采用HfCl4作为前驱体源在100℃制备氧化铪薄膜时,损伤阈值能够达到31.8J/cm2(1064nm,3ns)。     

Accumulation effect of SiO_2 protective layer on multi-shot laser-induced damage in high-reflectivity HfO_2/SiO_2 coatings

The accumulation effects in high-reflectivity(HR) HfO2/SiO2 coatings under laser irradiation are investigated.The HR HfO2/SiO2 coatings are prepared by electron beam evaporation at 1 064 nm.The laser-induced damage threshold(LIDT) are measured at 1 064 nm and at a pulse duration of 12 ns,in 1-on-1 and S-on-1 modes.Multi-shot LIDT is lower than single-shot LIDT.The laser-induced and native defects play an important role in the multi-shot mode.A correlative theory model based on critical conduction band electron density is constructed to elucidate the experimental phenomena.     

Study on the laser-induced damage threshold of sol-gel ZO_2-PVP coatings

<正>In order to improve the laser-induced damage threshold(LIDT) of the ZrO_2 film,the effect of polyvinyl pyrrolidone(PVP) with different average molecular weight on coatings is studied.The ZrO_2 sol is prepared by the hydrolysis of zirconium n-propoxide with acetylacetone as the chelating agent.The PVP(K16-18) is more suitable to obtain high LIDT coatings than other PVPs.The LIDT of the ZrO_2-PVP coatings is improved with the increase of the PVP(K16-18) content.When the PVP(K16-18) content is 2.4 wt.-%, the LIDT of the ZrO_2-PVP coatings is 43.5 J/cm~2(1064 nm,12 ns).The ZrO_2 sol and ZrO_2-PVP(K16- 18) sol have the good stability in 3 months.The refractive indices of the ZrO_2-PVP coatings decrease with the increase of the PVP(K16-18) content.     

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34.8 ppm和9.0 ppm,而基频(1 064 nm)激光损伤阈值分别为10.0 J/cm2和21.4 J/cm2.     

Effect of native defects and laser-induced defects on multi-shot laser-induced damage in multilayer mirrors

The roles of laser-induced defects and native defects in multilayer mirrors under multi-shot irradiation condition are investigated. The HfO 2 /SiO 2 dielectric mirrors are deposited by electron beam evaporation(EBE) . Laser damage testing is carried out on both the 1-on-1 and S-on-1 regimes using 355-nm pulsed laser at a duration of 8 ns. It is found that the single-shot laser-induced damage threshold(LIDT) is much higher than the multi-shot LIDT. In the multi-shot mode,the main factor influencing LIDT is the accumulation of irreversible laser-induced defects and native defects. The surface morphologies of the samples are observed by optical microscopy. Moreover,the number of laser-induced defects affects the damage probability of the samples. A correlative model based on critical conduction band(CB) electron density(ED) is presented to simulate the multi-shot damage behavior.     

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/cm², but it is increased to 8.98 J/cm² after annealing under temperature of 200 °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.     

The effect of porosity on the laser induced damage threshold of TiO2 and ZrO2 single layer films

Monolayer ZrO₂ and TiO₂ films were prepared on BK7 glass by physical vapor deposition (PVD) and were subsequently annealed for 1 h at 300 °C. By using the transmission spectra of two samples and the envelope method, the refractive index dispersion and extinction coefficients have been calculated. Laser induced damage threshold (LIDT) measurement shows that despite slight differences between the extinction coefficients of the two samples, the LIDT parameter of the ZrO₂ film is greater than that of the TiO₂ film. This fact leads us to consider thermal conductivity as an important parameter for interpreting the LIDT difference. According to our theoretical analysis, as a consequence of increase in the number of thermal barriers along poorer film, its thermal conductivity, and hence LIDT, decreased, which is in agreement with our experimental results. The measured porosity of the two samples shows higher porosity for TiO₂ single layer, which is in agreement with atomic force (AFM) images. The gradual and smooth damage morphology of ZrO₂ observed in optical images implies higher thermal conductivity than TiO₂.