光学玻璃基底原子层同质材料沉积薄膜光谱及激光诱导损伤特性研究

通过原子层沉积技术在熔石英玻璃表面制备了同质材料的单层SiO₂薄膜,对光学薄膜的物理化学性质和强激光辐照下的激光诱导损伤性能进行了深入研究。实验中采用双叔丁基氨基硅烷（BTBAS）和臭氧（O₃）作为反应前驱体,在熔石英光学元件表面进行了SiO₂薄膜的原子层沉积工艺研究,以不同沉积温度条件制备了一系列膜样品。首先对原子层沉积特性和薄膜均匀性展开了研究,发现薄膜生长厚度与沉积循环次数之间符合线性生长规律,验证了制备薄膜的原子级逐层生长特性,并且表面沉积膜层的均匀性很好,其测得膜厚波动不超过2%。然后针对不同温度条件下沉积的SiO₂薄膜,对其粗糙度及各类光谱特性展开了研究,对比结果表明：样品的表面粗糙度在镀膜后有轻微的降低;薄膜样品在200～1 000 nm范围内具有出色的透过率,均超过90%并逐渐趋近于93.3%,且其透射光谱与在裸露熔石英衬底上测得的光谱没有明显差异;镀膜前后荧光光谱和傅里叶变换红外光谱的差异证实了原子层沉积SiO₂膜中点缺陷（非桥键氧、氧空位、羟基等）的存在,这将会影响薄膜耐损伤性能。最后对衬底和膜样品进行了紫外激光诱导损伤测试,损伤阈值的变化表明熔石英元件表面沉积薄膜后的激光损伤性能有所降低,其零概率损伤阈值从31.8 J·cm-2减小到20 J·cm-2左右,与光谱缺陷情况表征相符合。薄膜中点缺陷部位会吸收紫外激光能量,导致局域温度升高,进而出现激光诱导损伤现象并降低抗激光损伤阈值。在选定的沉积温度范围内,较高温度条件下沉积的SiO₂薄膜其激光诱导损伤性能更好,可以控制沉积温度条件使得元件的抗损伤性能更为接近衬底本身,后续有望通过其他反应参数的优化来获得薄膜抗损伤性能的进一步提升。     

退火对EBE,IBS和ALD沉积HfO2薄膜的抗激光损伤性能影响

结合自身实验条件采用电子束蒸发(EBE)、离子束溅射(IBS)和原子层沉积(ALD)三种工艺制备了HfO2薄膜,对其进行退火实验,采用1064 nm Nd:YAG激光测定了即时沉积和退火后各HfO2薄膜的抗激光损伤能力。研究发现,ALD HfO2薄膜的激光损伤阈值最高,EBE HfO2薄膜次之,IBS HfO2薄膜的损伤阈值最低;300℃退火对各工艺薄膜抗激光损伤能力的影响均为负面,500℃退火则会显著降低ALD HfO2薄膜的抗激光损伤能力。     

HfO2薄膜的结构对抗激光损伤阈值的影响

利用蒸发氧化铪和离子辅助蒸发金属铪反应沉积氧化铪薄膜，对两种工艺下制备的氧化铪薄膜进行光学和结构以及激光损伤特性的研究. 实验结果表明，用金属铪反应沉积的氧化铪薄膜不仅结构均匀，并且具有较高的激光损伤阈值. 文章对损伤阈值和薄膜的结构及光学特性之间的关系进行了讨论.     

退火对ZrO2薄膜微结构及激光损伤阈值的影响

利用电子束蒸发方法在Yb∶YAG晶体和熔融石英衬底上沉积单层ZrO2薄膜,分别在673 K和1 073 K的温度下经过12 h退火以后,通过X射线衍射（XRD）分析了薄膜晶相,计算了薄膜的晶粒尺寸;利用表面热透镜技术获得了薄膜的吸收;测量了退火后薄膜的激光损伤阈值。实验结果表明:两种衬底上的薄膜结构受到退火温度和衬底表面结构的影响,高温退火有利于单斜相的形成,含单斜相的ZrO2薄膜具有较高的激光损伤阈值,而由于衬底的吸收,Yb∶YAG晶体上薄膜的损伤阈值远小于石英衬底上薄膜的损伤阈值。     

离子束辅助反应制备的氧化铪薄膜特性

 采用电子束直接蒸发氧化铪、无辅助电子束反应蒸发和离子束辅助反应蒸发金属铪3种沉积方式制备了单层HfO₂薄膜，对样品的光学性能、结构特性以及激光损伤特性进行了研究。实验结果表明：通过反应沉积的方法可以有效减少缺陷产生并改善均匀性，施加离子辅助可以提高薄膜的折射率，在一定条件下还可以有效地降低吸收，但激光损伤阈值仍未达到直接采用氧化铪制备的水平；晶体结构方面，离子辅助条件下可以获得单斜相氧化铪薄膜，并且随着轰击能量的提高由(002)面的择优取向向(-111)面转变。     

LBO晶体上1064 nm,532 nm二倍频增透膜的制备和性能

采用电子束蒸发方法在三硼酸锂(LBO)晶体上制备了1064 nm,532 nm二倍频增透膜.利用Lambda900分光光度计、MTSNanoIndenter纳米力学综合测试系统以及调Q脉冲激光装置对样品的光学性能、附着力和激光损伤阈值进行了分析测试.结果表明,通过多次实验,不断改进薄膜沉积工艺条件,在LBO晶体上获得了综合性能优异的二倍频增透膜.样品在1064 nm,532 nm波长的剩余反射率分别为0.07%和0.16%,薄膜粘附失效的临界附着力和激光损伤阈值分别为137.4 mN和15.14 J/cm2,薄膜激光损伤发生在Al2O3膜层.     

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。     

类金刚石薄膜及其进展

为了使研究者能更详细地了解类金刚石（DLC）薄膜的研究现状,综述了类金刚石薄膜的特性及应用,分析对比了目前常用的一些类金刚石薄膜的制备方法,包括物理气相沉积法（PVD）和化学气相沉积法（CVD）,并对类金刚石薄膜的抗强激光损伤特性以及提高其激光损伤阈值的方法进行了论述。结果发现,利用PVD法制备的DLC膜的硬度可以达到40 GPa~80 GPa,且薄膜的残余应力可以达到0.9 GPa~2.2 GPa之间,而CVD法则由于反应气体的充入导致类DLC薄膜的沉积速率大大降低,故使用率不高。同时,优化膜系的电场强度设计,采用合理的制备工艺,进行激光辐照后处理,施加外界电场干预均可有效地提高DLC薄膜的抗激光损伤能力, 且目前的DLC薄膜的激光损伤阈值可达到2.4 J/cm2。     

高反射光学薄膜激光损伤研究进展

激光诱导损伤阈值是大功率光学系统中重要参数,其数值大小对激光系统的输出功率与稳定性具有重要影响。为了突破损伤阈值对激光光学系统输出功率的限制,科研人员主要从制备薄膜工艺、激光特性、薄膜特性以及薄膜后工艺等方面开展研究。本文介绍了高反膜理论、制备工艺;综述了近十年来国内外对高反膜损伤研究的成果;阐述了激光特性、薄膜特性以及薄膜后工艺对薄膜损伤阈值的影响。在此基础上,对提高高反膜损伤阈值的研究和发展趋势进行了分析与展望。     

紫外Sc_2O_3薄膜的光学和结构性能表征及其激光作用下的损伤机理

利用电子束蒸发方法,在不同沉积温度(50~350℃)下制备了Sc2O3薄膜。分别用分光光度计,小角掠入射X射线衍射仪和轮廓仪测试了薄膜样品的光谱、微结构和表面粗糙度信息,并用薄膜分析软件Essential Macleod计算了Sc2O3薄膜的折射率和消光系数。结果表明:随着沉积温度升高,Sc2O3薄膜结晶程度增强,晶粒尺寸增大,且较高的沉积温度有利于获得较高的折射率。最后用355 nm,8 ns的三倍频Nd:YAG激光器测试了其激光损伤阈值(LIDT),最大值为2.6 J/cm2,且阈值与薄膜的消光系数、表面粗糙度、光学损耗均呈现相反的变化趋势。用光学显微镜和扫描电子显微镜表征了该薄膜的破坏形貌,详细分析了薄膜在不同激光能量作用下破坏的发展过程,以及Sc2O3薄膜在355 nm紫外激光作用下LIDT与制备工艺的关系,重点分析了355 nm激光作用下薄膜的破坏机理。     

Experimental research of laser-induced damage of the monolayer ZrO2 PVD and sol–gel films

Monolayer zirconia physical vapor deposition (PVD) and sol–gel films on K9 glass substrates were prepared by electron beam evaporation and spin coating methods, respectively. The laser-induced damage threshold (LIDT) of each film was measured. Properties of the films were analyzed using Stanford photo-thermal solutions (SPTS), ellipsometry, atomic force microscopy (AFM) and optical microscopy to study the damage mechanism of films under laser irradiation. The experimental results showed that, compared with the monolayer zirconia sol–gel film, the monolayer zirconia PVD film had larger absorption and smaller porous ratio, and that it had smaller LIDT. The different damage morphologies of films were influenced by their different absorption and microstructure characteristics. The zirconia sol–gel film is more suitable for applications involving high-power lasers.     

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。     

Effect of ammonia treatment on laser-induced damage of nano-porous silica film

The sol-gel monolayer silica films on K9 glass substrates were prepared with the dip method, and then treated in saturated ammonia gas. The laser-induced damage threshold (LIDT) of silica films with and without ammonia treatment was measured. Properties of the films were analyzed by using Stanford photo-thermal solutions (SPTS), ellipsometry, atomic force microscopy (AFM), and optical microscopy to study the effect of ammonia treatment on laser-induced damage of sol-gel monolayer silica film under laser irradiation. The experimental results showed that compared with the as-grown silica film, the silica film with ammonia treatment had larger absorption and smaller porous ratio, and it had smaller LIDT. Considering the improved abrasion resistance of films with ammonia treatment, a trade-off is always needed between abrasion resistance and LIDT in practice.     

辐照激光能量对SiO2薄膜特性及结构的影响

 为了认识SiO2薄膜在激光辐照下的变化,本文以K9玻璃为基底,采用电子束热蒸发方法制备了SiO2薄膜,并将此组在相同实验条件下制备的薄膜加以不同能量的激光辐照,研究在激光辐照前后样片的透射率、折射率、消光系数、膜厚、表面形貌及激光损伤阈值（LIDT）的变化。结果表明,样片膜厚随激光能量的增加而减小,辐照激光能改善薄膜表面形貌,并使样片LIDT值提高,最终能使样片的LIDT值从16.96 J/cm2提高至18.8 J/cm2。     

Influences of SiO2 protective layers and annealing on the laser-induced damage threshold of Ta2O5 films

Ta2O5 films are prepared on BK7 substrates with conventional electron beam evaporation deposition.The effects of SiO2 protective layers and annealing on the laser-induced damage threshold (LIDT) of the films are investigated.The results show that SiO2 protective layers exert little influence on the electric field intensity(EFI)distribution,microstructure and microdefect density but increase the absorption slightly.Annealing iS effective on decreasing the microdefect density and the absorption of the films.Both SiO2 protective layers and annealing are beneficial to the damage resistance of the films and the latter is more effective to improve the LIDT.Moreover,the maximal LIDT of Ta2O5 films is achieved by the combination of SiO2 protective layers and annealing.     

Electron beam evaporated LaF3 thin films prepared by different temperatures and deposition rates

LaF₃ thin films were prepared by electron beam evaporation with different temperatures and deposition rates. Microstructure properties including crystalline structure and surface roughness were investigated by X-ray diffraction (XRD) and optical profilograph. X-ray photoelectron spectroscopy (XPS) was employed to study the chemical composition of the films. Optical properties (transmittance and refractive index) and laser induce damage threshold (LIDT) at 355 nm of the films were also characterized. The effects of deposition rate and substrate temperature on microstructure, optical properties and LIDT of LaF₃ thin films were discussed, respectively.     

离子束技术对氧化铪薄膜性能的影响

 在基底清洗、薄膜沉积和薄膜后处理三个阶段均采用离子束技术,制备了氧化铪薄膜,并对薄膜的光学性能、表面特性和激光损伤阈值特性进行测试和研究。结果表明,利用离子束技术清洗基底可以增强表面吸附;离子束辅助沉积在合适离子束能量下可以得到高堆积密度、高损伤阈值的薄膜;离子束后处理氧化铪薄膜可以降低表面粗糙度,改善抗激光损伤阈值。说明在三个薄膜制备阶段同时采用合适的离子束参数可以制备出结构致密、阈值高、表面粗糙度好的氧化铪薄膜。     

Influence of Annealing Temperature on Structure, Optical Loss and Laser-Induced Damage Threshold of TiO2 Thin Films

TiO2 thin films are prepared on fused silica with conventional electron beam evaporation deposition. After annealed at different temperatures for 4h, the spectra and XRD patterns of the TiO2 thin film are obtained. Weak absorption of coatings is measured by the surface thermal lensing technique, and laser-induced damage threshold （LIDT） is determined. It is found that with the increasing annealing temperature, the transmittance of TiO2 films decreases. Especially when coatings are annealed at high temperature over 1173K, the optical loss is very serious. Weak absorption detection indicates that the absorption of coatings decreases firstly and then increases, and the absorption and defects play major roles in the LIDT of TiO2 thin films.