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。     

双离子束溅射沉积HfO­­2光学薄膜的研究

 用双离子束溅射沉积氧化铪光学薄膜，并对此工艺下制备的氧化铪薄膜进行了光学性质、残余应力、结构特性以及激光损伤特性的研究。实验结果表明，用双离子束溅射沉积的氧化铪薄膜不仅结构均匀,膜层致密,无定形结构，而且具有极低的散射和吸收,均匀的非晶结构,杂质缺陷少,激光损伤阈值高。     

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。     

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.     

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)。     

离子束溅射氧化铪薄膜的能带特性

氧化铪是高激光损伤阈值薄膜领域内一种重要的高折射率材料,其禁带宽度和Urbach带尾宽度直接影响到薄膜的吸收和激光损伤阈值。针对离子束溅射沉积法制备的氧化铪薄膜,以基板温度、离子束电压、离子束电流和氧气流量为主要制备参数,提出了基于正交实验的光学带隙调整方法,并采用Cody-Lorentz介电常数模型表征了薄膜的禁带宽度和带尾宽度。研究结果表明,当置信概率为90%时,在影响氧化铪薄膜禁带宽度的制备因素中,影响权重从大到小依次为基板温度、离子束电流和氧气流量,采用低基板温度、中等离子束电流和低氧气流量制备参数组合,可以获得高禁带宽度的氧化铪薄膜;对带尾宽度影响最大的制备参数是基板温度,其他参数影响不显著,在高基板温度下可以获得较低的带尾宽度,这表明氧化铪薄膜的无序度较低。     

一种大入射角容差宽带薄膜偏振器

通过组合长波通和短波通膜堆的方法,设计并制备了一种大入射角容差宽带薄膜偏振器。该薄膜为HfO_2/SiO_2结构,采用无离子束辅助的电子束蒸发工艺,蒸发金属铪和SiO_2制得。对该膜的透射率光谱、激光损伤阈值和形貌进行了研究,结果显示其不仅在1044~1084 nm波段内都具有很高的对比度,而且在1064 nm波长、53°~60°的入射角范围内具有很大的消光比和激光损伤阈值,且损伤特性基本不随入射角变化。该偏振器的P光损伤阈值约为20 J/cm~2,损伤主要由基板与薄膜界面处的纳米级缺陷所引起;S光损伤阈值约为45 J/cm~2,损伤主要由激光辐照下薄膜表面的等离子烧蚀现象引起。     

钛酸镧薄膜的制备及工艺优化

为了获得制备钛酸镧（LaTiO3）薄膜的最优工艺条件,采用电子束热蒸发技术在K9基底上制备了单层LaTiO3激光薄膜。研究了不同工艺条件对LaTiO3薄膜激光损伤特性的影响。研究结果表明,对LaTiO3薄膜激光损伤阈值（laser-induced damage threshold, LIDT）影响最大的工艺条件是沉积温度,其次是工作真空度,最后是蒸发束流。获得了制备单层LaTiO3激光薄膜的最优工艺条件:沉积温度175 ℃、工作真空度2.010-2 Pa、蒸发束流120 mA（8 keV）;证明了最优工艺下制备的LaTiO3薄膜具有良好的激光损伤特性、稳定性以及重复性,所制备LaTiO3薄膜的激光损伤阈值为16.9 J/cm2（1 064 nm,10 ns）。     

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.     

不同工艺制备的高反射薄膜在真空与大气环境下的激光损伤特性

 建立了光学元件在真空环境下的激光损伤测量系统,采用电子束蒸发和离子辅助技术制备了Hf­₂/SiO₂高反射薄膜。对不同工艺制备的薄膜在真空与大气环境下的1 064 nm波长的激光损伤阈值进行了测量,对薄膜的损伤形貌进行了观测。对薄膜的损伤特性研究分析结果表明：薄膜在真空环境中的损伤阈值相对大气环境中有明显下降,其1∶1测试和R1测试损伤阈值下降约30%;两种环境中的薄膜损伤特性也不同,真空环境中损伤阈值的下降可能与热传导的不同有关。     

Study on absorbance and laser damage threshold of HfO2 films prepared by ion-assisted reaction deposition

Using a new kind of EH1000 ion source, hafnium dioxide (HfO2) films are deposited with different deposition techniques and different conditions. The absorbance and the laser damage threshold of these films have been measured and studied. By comparing these characteristics, one can conclude that under right conditions, such as high partial pressure of oxygen and right kind of ion source, the ion-assisted reaction deposition can prepare HfO2 films with higher laser induced damage threshold.     

248 nm高反膜抗激光损伤性能

用电子束蒸发法在熔融石英基底上沉积了适用于248nm的HfO2/SiO2高反膜,为提高其抗激光损伤能力,设计并制备了两种保护层,一种是在常规高反膜系的基础上镀制二分之一波长厚度的SiO2保护层,另一种是用Al2O3/MgF2做保护层。测试了3种高反膜样品的激光损伤情况,通过损伤形貌的变化分析了两种保护层使抗激光损伤能力提高的原因以及存在的问题。     

电子束蒸发TiO2薄膜的光学特性

研究了不同工艺参数条件下，电子束蒸发TiO2薄膜的光学特性。在正交实验的基础上，利用离子束辅助沉积技术，获得了影响TiO2薄膜折射率的主要因素．得到了TiO2薄膜的折射率随氧气分压的关系。对离子氧和分子氧两种情况下TiO2薄膜的折射率进行了比较．得到了TiO2薄膜的折射率与沉积速度的关系，并给出了TiO2薄膜的红外吸收光谱。     

A comparative study of the influence of different post-treatment methods on the properties of HfO2 single layers

Heat treatment, laser conditioning and ion post-treatment were used, respectively, on HfO₂ single layers deposited by electron beam evaporation (EBE). Optical, structural and laser-induced damage threshold (LIDT) properties of the films had been studied. It was found that all of the post-treatment methods are effective for improving the LIDT, but the mechanism for the improvement differs. Heat treatment in atmosphere was found to be effective for improving film stoichiometry. Laser conditioning was useful to decrease the defects by stress release. While in the ion post-treatment, the defects were removed by ion sputtering and the absorption was reduced at the effect of compression induced by ion bombardment. The most suitable method should be chosen for the required characteristics of the coatings.     

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.     

Influence of APS bias voltage on properties of HfO_2 and SiO_2 single layer deposited by plasma ion-assisted deposition

HfO2 and SiO2 single layer is deposited on glass substrate with plasma ion assistance provided by Leybold advanced plasma source (APS). The deposition is performed with a bias voltage in the range of 70-130 V for HfO2, and 70-170 V for SiO2. Optical, structural, mechanical properties, as well as absorption and laser induced damage threshold at 1064 nm of HfO2 and SiO2 single layer deposited with the plasma ion assistance are systematically investigated. With the increase of APS bias voltage, coatings with higher refractive index, reduced surface roughness, and higher laser-induced damage threshold (LIDT) are obtained, and no significant change of the absorption at 1064 nm is observed. For HfO2, a bias voltage can be identified to achieve coatings without any stress. However, too-high bias voltage can cause the increase of surface roughness and stress, and decrease the LIDT. The bias voltage can be properly identified to achieve coatings with desired properties.     

Laser-induced damage of high reflectors for Ti:sapphire laser system

A broadband (～ 176 nm, R ＞ 98%, λ0 = 800 nm) and high laser-induced damage threshold (LIDT =2.4 J/cm2) TiO2/HfO2/SiO2 high reflector (HR) for Ti:sapphire chirped-pulse amplification (CPA) laser system is fabricated by the electron beam evaporation. The refractive index and extinction coefficient of TiO2 and HfO2 films are calculated from single-layer films' transmittance spectra. The properties of HR are mainly determined by the high refractive index material. The high refractive index leads to wide bandwidth. A low extinction coefficient indicates low absorption and high LIDT. The possible damage mechanism of HR is discussed.