HfO2中ZrO2含量对266nm HfO2/SiO2多层膜反射率的影响

用两种不同纯度的HfO2材料与同一纯度的SiO2材料组合,沉积Λ／4规整膜系(HL)^11H形成266nm的紫外反射镜,发现反射率相差0．7％左右。用X光电子能谱法分析了高反膜中表层HfO2中的成分,发现ZrO2的含量相差一个数量级左右。为确定形成这种差别的原因,用辉光放电质谱法测定了这两种HfO2材料中锆(Zr)及其钛(Ti)、铁(Fe)的含量,发现Zr是其中的最主要的杂质,两种HfO2材料中Zr含量有一个数量级的差别。说明在266nm波段,HfO2中ZrO2的含量会对HfO2／SiO2高反膜的反射率造成影响。根据HfO2单层膜的光谱曲线,推算出了这两种材料的消光系数的差别,并用Tfcalc膜系设计软件进行理论和镀制结果的模拟,得到与实验测试一致的结果。     

Study on Laser Conditioning of Optical Coatings

ＳｔｕｄｙｏｎＬａｓｅｒＣｏｎｄｉｔｉｏｎｉｎｇｏｆＯｐｔｉｃａｌＣｏａｔｉｎｇｓ￥ＺＨＡＯＱｉａｎｇ；ＦＡＮＺｈｅｎｇｘｉｕ；ＷＡＮＧＺｈｉｊｉａｎｇ（ＳｈａｎｇｈａｉＩｎｓｔｉｔｕｔｅｏｆＯｐｔｉｃｓａｎｄＦｉｎｅＭｅｃｈａｎｉｃｓ，Ｃｈｉｎｅｓ...     

层间热处理对SiO2/ZrO2双层膜的影响

 以正硅酸乙酯和丙醇锆为前驱体,用溶胶-凝胶法在K9基片上提拉镀制SiO₂/ZrO₂双层膜。采用不同实验步骤制备了2个样品,样品1镀完SiO₂后直接镀ZrO₂ ,样品2镀完SiO₂经热处理后再镀ZrO₂。采用原子力显微镜、椭偏仪、紫外-可见分光光度计对薄膜进行表征。针对SiO₂/ZrO₂双层膜,考虑到膜间渗透的影响,采用３层Cauchy模型进行椭偏模拟,椭偏参数的模拟值曲线与椭偏仪的测量值曲线十分吻合,进而发现热处理可以使SiO₂/ZrO₂双层膜之间的渗透减少近23 nm,从而提高其峰值透射率。利用输出波长1.064 mm,脉宽8.1 ns的激光束对样品进行了损伤阈值的测试,用光学显微镜观察损伤形貌,结果发现两者损伤阈值分别为13.6 J/c2和14.18 J/cm²,均为膜的本征损伤。     

Influence of ZrO2 in HfO2 on reflectance of HfO2/SiO2 multilayer at 248 nm prepared by electron-beam evaporation

Influence of ZrO₂ in HfO₂ on the reflectance of HfO₂/SiO₂ multilayer at 248 nm was investigated. Two kinds of HfO₂ with different ZrO₂ content were chosen as high refractive index material and the same kind of SiO₂ as low refractive index material to prepare the mirrors by electron-beam evaporation. The impurities in two kinds of HfO₂ starting coating materials and in their corresponding single layer thin films were determined through glow discharge mass spectrum (GDMS) technology and secondary ion mass spectrometry (SIMS) equipment, respectively. It showed that between the two kinds of HfO₂, either the bulk materials or their corresponding films, the difference of ZrO₂ was much larger than that of the other impurities such as Ti and Fe. It is the Zr element that affects the property of thin films. Both in theoretical and in experimental, the mirror prepared with the HfO₂ starting material containing more Zr content has a lower reflectance. Because the extinction coefficient of zirconia is relatively high in UV region, it can be treated as one kind of absorbing defects to influence the optical property of the mirrors.     

SiO2和HfO2薄膜光学性能的椭偏光谱测量

结合XRD和原子力显微镜等方法,利用椭圆偏振光谱仪测试了单层SiO2薄膜（K9基片）和单层HfO2薄膜（K9基片）的椭偏参数,并用Sellmeier模型和Cauchy模型对两种薄膜进行拟合,获得了SiO2薄膜和HfO2薄膜在300-800nm波段内的色散关系。用X射线衍射仪确定薄膜结构,并用原子力显微镜观察薄膜的微观形貌,分析表明：SiO2薄膜晶相结构呈现无定型结构,HfO2薄膜的晶相结构呈现单斜相结构;薄膜光学常数的大小和薄膜的表面形貌有关;Sellmeier和Cauchy模型较好地描述了该波段内薄膜的光学性能,并得到薄膜的折射率和消光系数等光学常数随波长的变化规律。     

ZrO2/SiO2溶胶-凝胶薄膜膜层间的渗透行为

 分别以丙醇锆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。用旋转镀膜法在K9玻璃上分别制备了单层SiO₂薄膜、单层ZrO₂薄膜、ZrO₂/ SiO₂双层膜和SiO₂/ZrO₂双层膜。采用原子力显微镜观察了薄膜的表面形貌，用椭偏仪测量薄膜的厚度与折射率，用紫外-可见光分光光度计测量了薄膜的透射率。对薄膜的透射光谱和椭偏仪模拟的数据进行分析，发现SiO₂/ZrO₂双层膜之间的渗透十分明显，而ZrO₂/SiO₂双层膜之间几乎不发生渗透。利用TFCalc模系设计软件,采用三层膜模型对薄膜的透射率进行模拟，得出的透射曲线与用紫外-可见光分光光度计测量的透射曲线十分符合。     

多层膜界面结构探测技术

分别以丙醇锆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Si O2溶胶。用旋转镀膜法在K9玻璃上分别制备了Si O2单层膜、ZrO2单层膜和ZrO2/Si O2/ZrO2三层膜。采用椭偏仪测量薄膜的厚度与折射率,用紫外-可见分光光度计测量了薄膜的透过率,利用TFCalc_Demo模系设计软件,采用三层理论模型对薄膜的透过率进行模拟,用扫描电镜(SEM)观察了三层膜的断面结构,用X射线光电子能谱仪(XPS)测量了薄膜的成分随深度方向的变化,进一步验证了ZrO2/Si O2/ZrO2三层膜之间的渗透关系,同时对多层膜的界面结构探测方法起到了借鉴作用。     

ZrO_2/SiO_2溶胶-凝胶薄膜膜层间的渗透行为

分别以丙醇锆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。用旋转镀膜法在K9玻璃上分别制备了单层SiO2薄膜、单层ZrO2薄膜、ZrO2/SiO2双层膜和SiO2/ZrO2双层膜。采用原子力显微镜观察了薄膜的表面形貌,用椭偏仪测量薄膜的厚度与折射率,用紫外-可见光分光光度计测量了薄膜的透射率。对薄膜的透射光谱和椭偏仪模拟的数据进行分析,发现SiO2/ZrO2双层膜之间的渗透十分明显,而ZrO2/SiO2双层膜之间几乎不发生渗透。利用TFCalc模系设计软件,采用三层膜模型对薄膜的透射率进行模拟,得出的透射曲线与用紫外-可见光分光光度计测量的透射曲线十分符合。     

溶胶-凝胶光学薄膜的激光损伤研究

 采用溶胶-凝胶工艺制备了SiO₂与ZrO₂单层介质膜，用输出波长1.06μm，脉宽15ns的电光调Q激光系统产生的强激光进行辐照实验。观察了光学薄膜经强激光辐照后的损伤情况，讨论了溶胶 凝胶光学薄膜在强激光照射下的损伤机理，提出了溶剂替换、紫外光处理、添加有机粘接剂等提高溶胶 凝胶光学薄膜激光损伤阈值的方法。     

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。     

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.     

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)。     

电子束蒸发和离子束溅射HfO_2紫外光学薄膜

HfO2薄膜在紫外光学中具有十分重要的地位,不同方法制备的HfO2薄膜特性不同,可以满足不同的实际应用需求。本文分别利用电子束蒸发和离子束溅射方法制备了用于紫外光区域的HfO2薄膜,并对薄膜的材料和光学特性进行了表征与比较。通过对单层HfO2薄膜的实测透射和反射光谱进行数值反演,得到了HfO2薄膜在230～800 nm波段的折射率和消光系数色散曲线,结果表明两种方法制备的HfO2薄膜在250nm的消光系数均小于2×10-3。在此基础上,制备了两种典型的紫外光学薄膜元件(紫外低通滤波器和240nm高反射镜),其光谱性能测试结果表明,两种不同方法制备的器件均具有较好的光学特性。     

等离子体辅助沉积HfO_2/SiO_2减反、高反光学薄膜

本文报导了用等离子体辅助（Ｐｌａｓｍａ－ＩＡＤ）沉积技术沉积ＨｆＯ２／ＳｉＯ２减反及高反光学薄膜。在波长１０６４ｎｍ处，ＨｆＯ２／ＳｉＯ２减反膜透过率大于９９．５％，ＨｆＯ２／ＳｉＯ２高反膜反射率大于９９．５％。     

反应离子镀光学薄膜的微观结构分析

用反应离子镀方法制备了ＴｉＯ２单层膜及ＴｉＯ２／ＳｉＯ２多层膜，用透射电子显微镜分别观察了由反应离子镀方法及传统蒸镀法二种不同工艺制得的ＴｉＯ２单层膜及ＴｉＯ２／ＳｉＯ２多层膜的断面结构，并对ＴｉＯ２单层膜进行了喇曼分析和卢瑟福背散射分析。     

Influence of different oxidants on the band alignment of HfO₂ films deposited by atomic layer deposition

Based on X-ray photoelectron spectroscopy(XPS),influences of different oxidants on band alignment of HfO2 films deposited by atomic layer deposition(ALD) are investigated in this paper.The measured valence band offset(VBO) value for H2 O-based HfO2 increases from 3.17 eV to 3.32 eV after annealing,whereas the VBO value for O 3-based HfO2 decreases from 3.57 eV to 3.46 eV.The research results indicate that the silicate layer changes in different ways for H2 O-based and O3-based HfO2 films after the annealing process,which plays a key role in generating the internal electric field formed by the dipoles.The variations of the dipoles at the interface between the HfO2 and SiO2 after annealing may lead the VBO values of H2 O-based and O 3-based HfO2 to vary in different ways,which fits with the variation of flat band(VFB) voltage.     

溶胶-凝胶ZrO_2/SiO_2薄膜的激光损伤研究

采用溶胶-凝胶工艺分别制备了SiO2和ZrO2单层薄膜、ZrO2/SiO2双层膜以及ZrO2/SiO2多层高反膜。用输出波长为1064nm、脉宽为6.3ns的YAG激光器对薄膜进行了激光损伤实验。观察了薄膜经强激光辐照后的损伤情况,讨论了薄膜的激光损伤行为,并从理论上分析了产生这些损伤的原因,为进一步镀制高质量的ZrO2/SiO2多层高反膜提供了依据。     

硅基光波导芯层材料及波导分束器的制备

本文采用溶胶－凝胶法制备了具有紫外感光性的SiO2/ZrO2/H有机无机复合薄膜,利用分光式椭偏仪测得该薄膜在光纤的常用通信窗口0.85 μm、1.31 μm和1.55 μm波长附近折射率分别为1.556 9、1.548 9和1.547 2,与下包层SiO2的折射率（1.46）相比,其折射率差比δ分别为6.64％,6.09％和5.97％,可作为芯层材料用于光波导的制备.通过控制提拉速率可以制作出厚度分别为1.29,2.20,4.00,5.44和6.82 μm的SiO2/ZrO2/H芯层薄膜,以满足0,1,2,3和4阶导模的传输要求.进而利用该薄膜自身的感光特性结合紫外掩模法,制备出相应厚度的1×8Y分支光功率分配器.通光实验表明,该光功分器能够将1.53～1.56 μm波长的光限制在波导内,实现光的传输和分束功能.     

基片温度对磁控溅射HfO2薄膜结构和性能影响分析

在纯氧条件下,采用直流磁控溅射技术在单晶硅基片上沉积氧化铪（HfO2）薄膜,并研究了沉积过程中基片温度对薄膜结构和性能的影响规律。利用X射线衍射仪（XRD）和X射线能谱（XPS）表征了薄膜的晶体结构和组分,利用原子力显微镜（AFM）观察薄膜表面形貌,利用纳米力学测试系统表征了薄膜的纳米硬度和弹性模量。结果表明:磁控溅射制备的HfO2薄膜样品呈(111)择优生长,其晶粒尺寸随着基片温度的升高而增大,但其晶型并不发生转变。随着基片温度的增加,基片中的硅元素向薄膜内扩散,影响了薄膜的化学计量比。沉积薄膜的表面形貌和力学性能亦受到其结构和组分变化的影响。在200 ℃条件下制备的HfO2薄膜纯度高,O、Hf元素化学计量达到了1.99,其表面质量和力学性能均达到了最佳值,随着基片温度升高至300 ℃以上,薄膜纯度下降,表面质量和力学性能均产生劣化。     

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.