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。     

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。     

Low cost fabrication of SiO2 optical waveguides by laser direct writing on Ti-doped Sol-Gel films

A commercial direct laser writing (DLW) system operating at 1070 nm was used to fabricate SiO₂ optical waveguides on silicon wafers. A Ti-doped SiO₂ Sol-Gel film was deposited on the SiO₂/Si substrate by the dip-coating technique, based on which SiO₂ optical waveguides were patterned by DLW using a Ytterbium fiber laser and followed by chemical etching. The effects of laser parameters and the preheated temperature of Sol-Gel films on the dimensions of optical waveguides were studied systematically. The differences of etching rate between laser irradiated and non-irradiated areas in Sol-Gel films preheated at various temperatures are characterized by measuring the thickness of the films. Results demonstrate that the available laser power density range for laser densification and the width of the patterned optical waveguides are influenced strongly by the preheated temperature of the Sol-Gel films. The width of the optimized optical waveguide in this work is 25 μm. The minimum propagation loss of the fabricated optical waveguides is 1.7 dB cm⁻¹ at the wavelength of 1550 nm.     

Laser assisted modification and chemical metallization of electron-beam deposited ceria thin films

Excimer laser processing is applied for tailoring the surface morphology and phase composition of CeO₂ ceramic thin films. E-beam evaporation technique is used to deposit samples on stainless steel and silicate glass substrates. The films are then irradiated with ArF* excimer laser pulses under different exposure conditions. Scanning electron microscopy, optical spectrophotometry, X-ray diffractometry and EDS microanalysis are used to characterize the non-irradiated and laser-processed films. Upon UV laser exposure there is large increase of the surface roughness that is accompanied by photo-darkening and ceria reduction. It is shown that the laser induced changes in the CeO₂ films facilitate the deposition of metal nano-aggregates in a commercial copper electroless plating bath. The significance of laser modification as a novel approach for the production of CeO₂ based thin film catalysts is discussed.     

溶胶-凝胶TiO2和SiO2光学膜的结构

本文研究了TiO₂和SiO₂溶胶-凝胶光学膜在低温热处理下的组分、形貌特征、光散射特性.AES分析结果表明,在TiO₂膜和SiO₂膜的交界面处,Ti和Si相互扩散,从而证实了在多层膜中,膜层之间、膜层和基底之间有Ti-O-Si(或Si-O-Ti,或Si-O-Si)化学键形成.AES和ESCA分析结果显示溶胶-凝胶膜经过低温处理后C的含量较高,这归结为溶胶—凝胶膜的工艺特点.AFM测试结果显示,溶胶—凝胶TiO₂光学膜的表面形貌具有显著的柱状结构,薄膜表面起伏大约是7.5nm.TiO₂,SiO₂单层膜的表面散射率随着热处理温度的提高而变大,对于不同陈化时间的溶液镀制的膜有不同的表面散率.     

二氧化硅增透膜微观结构与激光损伤阈值的调控

采用溶胶-凝胶技术制备了二氧化硅增透膜,通过向溶胶中添加高分子聚乙烯醇缩丁醛（PVB）,调控胶体的粒径,进而控制膜层微观结构,研究膜层微观结构与激光损伤阈值的关系。纳米粒度仪和扫描探针显微镜测试表明:PVB加入溶胶后,控制了二氧化硅胶粒的生长,使二氧化硅胶粒生长更均匀,因而膜层的微观结构更均匀。当PVB质量分数为1%时,胶体粒径为15 nm,分散系数小于0.1。用该胶体镀膜,膜层均匀,表面粗糙度小于3.25 nm。并且PVB加入后增加了膜层胶粒间的黏附性,使得膜层强度增大。PVB加入使膜层的激光损伤阈值有所增加。当PVB的添加量为1%时,膜层的激光损失阈值从30.0 J/cm2增加到40.1 J/cm2。膜层激光损伤阈值的增加与膜层微观均匀性和物理强度的增加有关。     

Microstructure and roughness improvement of polycrystalline Bi thin films upon pulsed-laser melting

Bismuth films with different thicknesses have been grown by do sputtering on substrates held at room temperature. The films are always formed by columnar crystals with a grain size comparable to the film thickness which lead to surface roughness. It increases with the thickness of the films and has a strong influence on the film optical properties. The films have been irradiated with nanosecond laser pulses, and real-time reflectivity measurements during the irradiation were used to follow the changes in the film optical properties. It will be shown that pulsed-laser irradiation of films thinner than 100 nm improves substantially their surface roughness and their crystalline quality by increasing the grain size at least one order of magnitude.     

溶胶-凝胶法制备SiO2-TiO2平板光波导工艺研究

采用溶胶-凝胶法制备了SiO₂-TiO₂平板光波导,计算了平板光波导通光条件,分析了硅/钛溶胶-凝胶材料的热性能,观测了平板光波导的结构形貌,并测试了其通光损耗。结果表明：经过200℃,30 min干燥处理的凝胶薄膜呈疏松多孔状态,对于非对称平板波导,存在芯层通光截止厚度,而且当SiO₂-TiO₂芯层厚度为0.5 μm时,SiO₂下包层厚度至少有6 μm才能防止1550 nm波长光泄露入单晶硅衬底中。制备的光波导对于1550 nm波长光传输损耗最小值为0.34 dB/cm。     

光斑尺寸对光学薄膜元件温升的影响

 实验测量了波长1 064 nm， 10 kHz高重复频率激光辐照下在白宝石、石英玻璃、K9基片上制备的Ta₂O₅/SiO₂高反膜的温度变化，有限元分析的结果与实验结果相一致。用ANSYS程序计算了不同光斑直径、相同功率激光和相同功率密度激光辐照下薄膜元件温升的变化。结果表明：相同功率激光辐照光学薄膜元件时，光斑大小只影响激光辐照点的温升，对基板温升没有影响。基板温升只与激光功率有关，激光功率越大，基板温升越大。相同功率密度激光辐照光学薄膜元件时，光斑越大，激光辐照点温度及基板温度均越高。从激光损伤的热效应考虑，小光斑激光辐照时，光学薄膜的激光损伤阈值较高。     

溶胶-凝胶法制备高折射率TiO2薄膜

 采用溶胶- 凝胶法制备了TiO₂纳米晶溶胶,并以旋涂法（spin-coating）镀制了高折射率光学薄膜。借助光散射技术和透射电镜研究了溶胶的微结构。采用原子力显微镜、场发射扫描电镜、紫外-可见-近红外光谱仪、椭偏仪、漫反射吸收光谱及强激光辐照实验,对膜层的结构、光学性能及抗激光损伤性能进行了系统的表征。结果显示:纳米晶薄膜的折射率达到了1.9,而传统的溶胶-凝胶薄膜折射率只有1.6;同时纳米晶薄膜的抗激光损伤阈值与传统的溶胶-凝胶薄膜相差不大,在1 064 nm处分别为16.3 J/cm²(3 ns脉冲) 和16.6 J/cm²(3 ns脉冲);纳米晶溶胶薄膜可以在保持较高抗激光损伤阈值情况下,大幅度提高薄膜折射率。     

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。     

Damage performance of TiO2/SiO2 thin film components induced by a long-pulsed laser

In order to study the long-pulsed laser induced damage performance of optical thin films, damage experiments of TiO₂/SiO₂ films irradiated by a laser with 1 ms pulse duration and 1064 nm wavelength are performed. In the experiments, the damage threshold of the thin films is measured. The damages are observed to occur in isolated spots, which enlighten the inducement of the defects and impurities originated in the films. The threshold goes down when the laser spot size decreases. But there exists a minimum threshold, which cannot be further reduced by decreasing the laser spot size. Optical microscopy reveals a cone-shaped cavity in the film substrate. Changes of the damaged sizes in film components with laser fluence are also investigated. The results show that the damage efficiency increases with the laser fluence before the shielding effects start to act.     

Effect of H2 and O2 plasma etching treatment on the surface of diamond-like carbon thin film

In this study, we investigated the surface properties of diamond-like carbon (DLC) films for biomedical applications through plasma etching treatment using oxygen (O₂) and hydrogen (H₂) gas. The synthesis and post-plasma etching treatment of DLC films were carried out by 13.56 MHz RF plasma enhanced chemical vapor deposition (PECVD) system. In order to characterize the surface of DLC films, they were etched to a thickness of approximately 100 nm and were compared with an as-deposited DLC film. We obtained the optimum condition through power variation, at which the etching rate by H₂ and O₂ was 30 and 80 nm/min, respectively. The structural and chemical properties of these thin films after the plasma etching treatment were evaluated by Raman and Fourier transform infrared (FT-IR) spectroscopy. In the case of as-deposited and H₂ plasma etching-treated DLC film, the contact angle was 86.4° and 83.7°, respectively, whereas it was reduced to 35.5° in the etching-treated DLC film in O₂ plasma. The surface roughness of plasma etching-treated DLC with H₂ or O₂ was maintained smooth at 0.1 nm. These results indicated that the surface of the etching-treated DLC film in O₂ plasma was hydrophilic as well as smooth.     

Antireflection microstructures fabricated upon fluorine-doped SiO(2) films

Two-dimensional periodic structures were fabricated upon a fluorine-doped SiO(2) film in which the fluorine content changed gradually in the direction of film thickness. The films were deposited by plasma-enhanced chemical-vapor deposition. The film was periodically patterned into a 1-mum period and an ~1-mum -groove depth by inductive coupled plasma reactive-ion etching followed by chemical etching in a diluted HF solution. A surface reflectance of 0.7% was attained at 1.85-mum wavelength, a value that is one fifth as large as the 3.5% Fresnel reflection of a SiO(2) substrate with a flat surface.     

Influence on the laser induced backside dry etching of thickness and material of the absorber, laser spot size and multipulse irradiation

Laser induced backside dry etching method (LIBDE) was developed - analogously to the well-known laser induced backside wet etching (LIBWE) technique - for the micromachining of transparent materials. In this procedure, the absorbing liquid applied during LIBWE was replaced with solid metal layers. Fused silica plates were used as transparent targets. These were coated with 15-120 nm thick layers of different metals (silver, aluminium and copper). The absorbing films were irradiated by a nanosecond KrF excimer laser beam through the quartz plate. The applied fluence was varied in the 150-2000 mJ/cm² range, while the irradiated area was between 0.35 and 3.6 mm². At fluences above the threshold values, it was found that the metal layers were removed from the irradiated spots and the fused silica was etched at the same time. In our experiments, we investigated the dependence of the main parameters (etch rate and threshold) of LIBDE on the absorption of the different metal layers (silver, copper, aluminium), on the size of the irradiated area, on the film thickness and on the number of processing laser pulses.     

脉冲紫外激光刻蚀聚合物薄膜的发射光谱和形貌学研究

用聚焦的紫外XeCl准分子激光器轰击高分子聚合物薄膜(涤纶薄膜),由OMA系统接收其发射光谱.发现谱线主要为C2的Swan带和CN的红带,并与高压汞灯照射后的聚合物薄膜的发射谱进行了比较,在我们的实验精度内,没有发现区别.实验显示,每个光脉冲能刻蚀掉几分之一到几个微米的薄膜.激光的刻蚀效应存在波长和能量密度两个阈值.对于涤纶薄膜,能量密度的阈值约为40mJ/cm2.同时还作了紫外吸收光谱和SEM照片的分析.     

采用泵浦探测技术研究VO2薄膜相变特性

为研究纳秒激光作用下的VO₂薄膜的相变特性,采用泵浦-探测技术进行实验。首先,利用直流磁控溅射法制备VO₂薄膜,经X射线衍射（XRD）和原子力显微镜（AFM）分析表明样品质量较高。然后,测量VO₂薄膜在波长532 nm处的透过率随温度的变化情况,发现透过率随温度升高由32%上升到37%,与红外波段完全相反。在此基础上,选择1 064 nm泵浦光和532 nm探测光研究激光参数中能量密度和重频对VO₂薄膜相变特性的影响,同时结合ANSYS有限元软件对纳秒激光作用下VO₂薄膜的单脉冲温升情况进行分析。结果表明：VO₂薄膜在大于30 mJ/cm²的纳秒激光能量密度作用下,单脉冲温升可达相变温度,最小相变响应时间在14 ns左右。进一步提高纳秒激光能量密度,其相变响应时间略有增加但变化不大。在100 Hz以内改变纳秒激光重频对VO₂薄膜的相变响应基本无影响。VO₂薄膜的相变恢复时间随着纳秒激光能量密度的增大而呈自然指数增加,其变化过程与基底材料和纳秒激光参数密切相关。因此,可以通过优化VO₂薄膜基底材料参数提高其激光防护效果。     

Ultraviolet irradiation induced changes in the surface of phenolphthalein poly(ether sulfone) film

Changes in surface characteristics of phenolphthalein poly(ether sulfone) (PES-C) film induced by ultraviolet (UV) irradiation were investigated. The surface properties of the pristine and irradiated films were studied by attenuated total-reflection FTIR (FTIR-ATR), X-ray photoelectron spectroscopy (XPS), contact angle measurements and atomic force microscopy (AFM). It was found that photooxidation degradation took place on the sample surface after irradiation and the oxygen content in the surface increased as evidenced by FTIR-ATR and XPS results. The water contact angle of the irradiated films decreased with increasing irradiation time, which was ascribed to the increased polarity of the surface induced by photooxidation. The etching of ultraviolet irradiation induced the roughening of PES-C surface after irradiation with its root-mean-square roughness (RMS) determined by AFM increased from 2.097 nm before irradiation to 7.403 nm in the area of 25 μm × 25 μm.     

CVD金刚石中的氮对等离子体刻蚀的影响

采用非对称磁镜场电子回旋共振等离子体分别对沉积过程中掺氮和未掺氮的化学气相沉积金刚石膜进行了刻蚀研究, 结果表明: 掺氮制备的金刚石膜的刻蚀主要集中在晶棱处, 经过4h刻蚀后其表面粗糙度由刻蚀前的4.761 μm下降至3.701 μm, 刻蚀对金刚石膜的表面粗糙度的影响较小; 而未掺氮制备的金刚石膜的刻蚀表现为晶面的均匀刻蚀, 晶粒坍塌,刻蚀4h后其表面粗糙度由刻蚀前的3.061 μm下降至1.083 μm. 刻蚀导致表面粗糙度显著降低. 上述差别的主要原因在于金刚石膜沉积过程中掺氮导致氮缺陷在金刚石晶棱处富集, 晶棱处电子发射加强, 引导离子向晶棱运动并产生刻蚀, 从而加剧晶棱的刻蚀. 而未掺氮金刚石膜,其缺陷相对较少且分布较均匀 ,刻蚀时整体呈现为 (111) 晶面被均匀刻蚀继而晶粒坍塌的现象. 关键词： 掺氮 金刚石膜 刻蚀 非对称磁镜场     

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。