HfO_2单层膜的吸收和激光损伤阈值测试

薄膜吸收是降低膜层激光损伤阈值的重要原因,为了研究薄膜吸收对激光损伤阈值的影响,对HfO2单层膜在1 064 nm处的吸收及其在不同波长激光辐照下的损伤阈值进行了测试和分析。研究结果表明:薄膜的激光损伤阈值由薄膜吸收平均值(决定于薄膜中缺陷的种类和数量)和吸收均匀性(决定于薄膜中缺陷的分布)共同决定;根据HfO2单层膜在1064 nm波长处的吸收值,不但可以定性判断薄膜在1 064 nm波长,而且还可以判断在其它波长激光辐照下的抗激光损伤能力。     

HfO_2/SiO_2薄膜的激光预处理作用研究北大核心CSCD

激光预处理是提高激光薄膜抗激光损伤阈值的重要手段。对电子束蒸发方式镀制的HfO2/SiO2反射膜采用大口径激光进行了辐照,并采用激光量热计测量了激光辐射前后的弱吸收值。采用聚焦离子束(FIB)技术分析了激光辐照后薄膜的损伤形态并探究了损伤原因,首次采用扫描电镜拍摄到了节瘤部分喷发时的形貌图,并对其进行了FIB分析,为进一步了解节瘤的损伤过程提供了依据。实验发现,激光辐照过后的激光薄膜弱吸收明显降低,激光预处理有效减少了引起薄膜吸收的缺陷,存在明显的清洗效应;在本实验采用的HfO2/SiO2反射膜中,激光预处理技术对于祛除位于基底上种子形成的节瘤是有效的,原因是激光辐射过后该节瘤进行了预喷发并不会对后续激光产生影响;而激光预处理技术对位于膜层中间的可能是镀膜过程中材料飞溅引起的缺陷是无效的,需要通过其他手段对该类节瘤进行祛除。     

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)。     

HfO2/SiO2薄膜的激光预处理作用研究

对电子束蒸发方式镀制的HfO2/SiO2反射膜采用大口径激光进行辐照,采用激光量热计测量了激光辐射前后的弱吸收值。实验发现HfO2/SiO2反射膜在分别采用1 064 nm和532 nm的激光辐照前后薄膜吸收分别从5.4%和1.7%降低到1.4和1.2%。采用聚焦离子束技术分析了激光辐照后薄膜的损伤形态并探究了损伤原因,发现：薄膜在激光辐照下存在节瘤的地方容易出现薄膜损伤,具体表现为熔融、部分喷发、完全脱落3种形态,节瘤缺陷种子来源的差异是导致其损伤机理也存在着巨大差异的主要原因。同时这些节瘤缺陷种子来源也影响着激光预处理作用效果,激光预处理技术对于祛除位于基底上种子形成的节瘤是有效的,原因是激光辐射过后该节瘤进行了预喷发而不会对后续激光产生影响;而激光预处理技术对位于膜层中间的可能是镀膜过程中材料飞溅引起的缺陷是无效的,需要通过飞秒激光手段对该类节瘤进行祛除。     

HfO2／SiO2高反射膜的缺陷及其激光损伤

用原子力、Normaski和扫描电子显微镜等分析仪器,对高损伤阈值薄膜常采用HfO2/SiO2薄膜进行了表面显微图象研究,分析了薄膜常见的表面缺陷,如节瘤,孔洞和划痕等。薄膜表面缺陷的激光损伤实验表明,不同缺陷的抗激光损伤能力不大相同。节瘤缺陷最低,约为15J/cm^2,薄膜的损伤阈值主要由其决定,孔洞的激光损伤能力与节瘤相比较高,约为节瘤的2－3倍。节瘤缺陷在低能量密度的激光损伤所形成的孔洞,与镀制过程中形成的孔洞形貌相似,激光再损伤能力也相似。低能量密度的激光把瘤缺陷变为孔洞缺陷是激光预处理提高薄膜损伤阈值的原因之一。     

SiO2/HfO2高反射膜的研制

主要讨论了电子束蒸发SiO2/HfO2薄膜的面形控制和损伤性能。研究了电子束蒸发工艺参数对薄膜应力以及面形的影响;分析了制备工艺对薄膜吸收、节瘤缺陷密度的影响,测量了制备薄膜的损伤阈值。研究结果表明:调整SiO2蒸发时的氧分压可以有效地将薄膜的应力控制在-250~-50 MPa。同时采用金属Hf蒸发可以显著地将节瘤缺陷密度从12.6 mm-2降低至2.7 mm-2,同时将损伤阈值从30 J/cm2提高至55 J/cm2。     

HfO2/SiO2高反射膜的缺陷及其激光损伤

用原子力、Normaski和扫描电子显微镜等分析仪器,对高损伤阈值薄膜常采用的HfO2光损伤所形成的孔洞,与镀制过程中形成的孔洞形貌相似,激光再损伤能力也相似。低能量密度的激光把节瘤缺陷变为孔洞缺陷是激光预处理提高薄膜损伤阈值的原因之一。     

制备工艺对HfO2薄膜抗激光损伤能力的影响

采用反应蒸镀法镀制了单层HfO2薄膜,观察了薄膜表面主要的微结构缺陷,研究了基片清洗工艺对薄膜损伤阈值的影响。测量了薄膜沉积前后表面粗糙度变化。结果表明：沉积工艺可以改变粗糙度,并对薄膜抗激光损伤能力有较大的影响。     

532nm HfO_2/SiO_2高反膜的激光预处理效应

采用单台阶能量光栅扫描以及R-on-1测试两种不同预处理方式研究了激光预处理技术对532nm HfO2/SiO2高反膜的阈值提升效果。用Nd:YAG二倍频激光对电子束蒸发制备的532nm HfO2/SiO2高反膜进行1-on-1损伤阈值测试,然后分别进行单台阶能量光栅扫描以及R-on-1测试。通过对损伤概率以及损伤形貌的分析,发现激光预处理能够去除薄膜内低阈值缺陷,达到提高损伤阈值的目的,损伤阈值分别提高38%和30%。     

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。     

Comparison of laser-induced damage in Ta2O5 and Nb2O5 single-layer films and high reflectors

Ta2O5 and Nb2O5 films are deposited on BK7 glass substrates using an electron beam evaporation method and are annealed at 673 K in the air.In this letter,comparative studies of the optical transmittance,microstructure,chemical composition,optical absorption,and laser-induced damage threshold(LIDT) of the two films are conducted.Findings indicate that the substoichiometric defect is very harmful to the laser damage resistance of Ta2O5 and Nb2O5 films.The decrease of absorption improves the LIDT in films deposited by the same material.However,although the absorption of the Ta2O5 single layer is less than that of the Nb2O5 single layer,the LIDT of the former is lower than that of the latter.High-reflective(HR) coatings have a higher LIDT than single layers due to the thermal dissipation of the SiO2 layers and the decreased electric field intensity(EFI).In addition,the Nb2O5 HR coating achieves the highest LIDT at 25.6 J/cm 2 in both single layers and HR coatings.     

单脉冲和多脉冲飞秒激光对单层光学薄膜的损伤

 利用掺钛的蓝宝石飞秒激光系统输出的单脉冲和多脉冲飞秒激光(中心波长800 nm，脉宽50 fs，靶面聚焦直径Ф 40 μm)，分别对BK7玻璃基底上厚约500 nm的单层HfO₂和单层ZrO₂薄膜进行辐照，得到了这两种薄膜在1-on-1和1 000-on-1测试方法下的激光损伤阈值。实验发现，两种方法下HfO₂单层膜的阈值均比ZrO₂单层膜的阈值高。从简化的Keldysh多光子离化理论出发，认为HfO₂薄膜材料的带比ZrO₂的宽是导致上述结果的主要原因。同时，同一种薄膜的多脉冲下的阈值比单脉冲下的低，原因是多脉冲下，飞秒激光对光学薄膜的损伤存在累积效应。     

Influence of porosity on laser damage threshold of sol–gel ZrO2 and SiO2 monolayer films

Monolayer ZrO₂ sol–gel and physical vapor deposition (PVD) films were prepared by spin method and electron beam evaporation method, respectively. Monolayer sol–gel SiO₂ films were prepared with the dip-coating method from acid and base catalyzed SiO₂ sols, respectively. Some of the SiO₂ base films were subsequently treated in saturated ammonia gas for 20 h. The laser induced damage threshold (LIDT) of each film was measured. Properties of the films were analyzed by using Stanford photo-thermal solutions (SPTSs), ellipsometer, atomic force microscopy (AFM) and optical microscopy. The experimental results showed that porous ratio is an essential factor to decide the LIDT for sol–gel films, which benefits the pressure exerted on the film or substrate by the moving particle to dissipate. The films with lower thermal absorption and higher porous ratio have higher LIDT.     

电子束蒸发法制备ZrO2薄膜的相变模型分析

 用电子束蒸发方法制备了纯的ZrO₂薄膜和含Y₂O₃摩尔分数为7%和13%的ZrO₂薄膜,即YSZ薄膜,通过测定薄膜的损伤阈值来验证温度诱导相变模型;并用X射线衍射（XRD）来测定ZrO₂和YSZ镀膜材料和薄膜的结构特征。结果表明：ZrO₂镀膜材料和薄膜室温下都表现为单斜相,YSZ镀膜材料和薄膜室温下都以立方相存在;YSZ薄膜的损伤阈值远高于ZrO₂薄膜的损伤阈值,这是因为添加Y₂O₃后的YSZ材料的相比较稳定,在蒸发过程中不会发生相变,而ZrO₂材料则发生相变,产生缺陷,缺陷在激光作用下成为吸收中心和初始破坏点,导致ZrO₂薄膜的损伤阈值降低。     

窄带干涉滤光片抗击不同输出方式激光的损伤特性研究

利用Nd∶YAG调Q单脉冲激光和自由脉冲激光对硬膜窄带干涉滤光片进行激光损伤阈值的测试,并且采用表面热透镜技术测量了滤光片的吸收率。实验发现:窄带干涉滤光片的吸收率和激光损伤阈值强烈依赖于辐照激光波长与窄带干涉滤光片通带的相对位置;在调Q单脉冲激光作用下,不同中心波长的滤光片损伤形貌存在明显的差别,而在自由脉冲激光作用下,各滤光片的损伤形貌则趋于相同,均表现为典型的热熔烧蚀破坏。根据实验结果,结合损伤形貌,通过驻波场理论对激光作用下滤光片内电场分布的分析与模拟,探讨了两种激光模式作用下滤光片的损伤特征和损伤机理的不同特点。     

Study on high-reflective coatings of different designs at 532 nm

Conventional HfO2/SiO2 and Al2O3/HfO2/SiO2 double stack high reflective （HR） coatings at 532 nm are deposited by electron beam evaporation onto BK7 substrates. The laser-induced damage threshold （LIDT） of two kinds of HR coatings is tested, showing that the laser damage resistance of the double stack HR coatings （16 J/cm2） is better than that of the conventional HR coatings （12.8 J/cm2）. Besides, the optical properties, surface conditions, and damage morphologies of each group samples are characterized. The results show that laser damage resistance of conventional HR coatings is determined by absorptive defect, while nodular defect is responsible for the LIDT of double stack HR coatings.     

Comparison of TiO2 and ZrO2 Films Deposited by Electron-Beam Evaporation and by Sol-Gel Process

TiO2 and ZrO2 films are deposited by electron-beam （EB） evaporation and by sol-gel process. The film properties are characterized by visible and Fourier-transform infrared spectrometry, x-ray diffraction analysis, surface roughness measure, absorption and laser-induced damage threshold （LIDT） test. It is found that the sol-gel films have lower refractive index, packing density and roughness than EB deposited films due to their amorphous structure and high OH group concentration in the film. The high LIDT of sol-gel films is mainly due to their amorphous and porous structure, and low absorption. LIDT of EB deposited film is considerably affected by defects in the film, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.     

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.