光学元件亚表面缺陷的损伤性检测方法

在磨削、研磨和抛光加工过程中产生的微裂纹、划痕、残余应力等亚表面缺陷会导致熔石英元件抗激光损伤能力下降,如何快速、准确地检测亚表面损伤成为光学领域亟待解决的关键问题。采用HF酸蚀刻法、角度抛光法和磁流变斜面抛光法对熔石英元件在研磨加工中产生的亚表面缺陷形貌特征及损伤深度进行了检测和对比分析,结果表明,不同检测方法得到的亚表层损伤深度的检测结果存在一定差异,HF酸蚀刻法检测得到的亚表面损伤深度要比角度抛光法和磁流变斜面抛光法检测结果大一些。且采用的磨粒粒径越大,试件表面及亚表面的脆性断裂现象越严重,亚表面缺陷层深度越大。     

Effect of HF etching on the surface quality and laser-induced damage of fused silica

The surface hardness of polished and HF etched fused silica has been investigated by nanoindentation technique. The results of polished fused silica indicate that the hardness of surface layer is greater than that of the bulk material. The difference should be attributed to the polishing induced deformation of the thin surface layer. The various removal depths of surface layer by HF etching has been confirmed by the surface hardness results. The initial laser damage threshold and damage possibility of unetched and etched samples were also measured. The results show a great improvement of damage resistance by slight etching and a reduction by excess etching. The correlation between surface hardness and damage threshold indicates that the mechanical strength plays an important role in the initiation of laser-induced damage.     

熔石英表面杂质元素在酸蚀过程中的变化

为了探寻熔石英表面痕量杂质元素种类以及随HF酸蚀刻过程中的变化情况,用质量分数为1%HF酸溶液对熔石英进行长达24,48,72,96 h的静态蚀刻实验。结合飞行时间二次离子质谱（TOF-SIMS）和X射线光电子能谱（XPS）测试分析结果发现,熔石英试片表面的痕量杂质元素主要含有B,F,K,Ca,Na,Al,Zn和Cr元素,其中绝大部分都存在于贝氏层中,在亚表面缺陷层检测到有K,Ca元素。所含有的K,Na杂质元素会与氟硅酸反应生成氟硅酸盐化合物。分析表明,在HF酸蚀刻的过程中一部分杂质元素将被消除,一部分杂质元素和生成氟硅酸盐化合物会随着蚀刻液逐渐从熔石英表面向表面纵深方向扩散并被试片吸附沉积,且随着深度的加深各元素的相对含量逐渐减少。     

Subsurface defect characterization and laser-induced damage performance of fused silica optics polished with colloidal silica and ceria

This paper mainly focuses on the influence of colloidal silica polishing on the damage performance of fused silica optics. In this paper, nanometer sized colloidal silica and micron sized ceria are used to polish fused silica optics. The colloidal silica polished samples and ceria polished samples exhibit that the root-mean-squared(RMS) average surface roughness values are 0.7 nm and 1.0 nm, respectively. The subsurface defects and damage performance of the polished optics are analyzed and discussed. It is revealed that colloidal silica polishing will introduce much fewer absorptive contaminant elements and subsurface damages especially no trailing indentation fracture. The 355-nm laser damage test reveals that each of the fused silica samples polished with colloidal silica has a much higher damage threshold and lower damage density than ceria polished samples. Colloidal silica polishing is potential in manufacturing high power laser optics.     

酸蚀与紫外激光预处理结合提高熔石英损伤阈值

采用HF酸刻蚀和紫外激光预处理相结合的方式提升熔石英元件的负载能力,用质量分数为1%的HF缓冲溶液对熔石英刻蚀1~100 min,综合透过率、粗糙度和损伤阈值测试结果,发现刻蚀时间为10min的熔石英抗损伤能力最佳。采用355 nm紫外激光对HF酸刻蚀10 min的熔石英进行预处理,结果表明:紫外预处理能量密度在熔石英零损伤阈值的60%以下时,激光损伤阈值单调递增;能量到达80%时,阈值反而低于原始样片的损伤阈值。适当地控制酸蚀时间和紫外激光预处理参数能有效提高熔石英的抗损伤能力。     

熔石英元件抛光表面的亚表面损伤研究

通过结合HF酸洗和微分干涉差显微成像对两组抛光元件的亚表面损伤进行直接观测和分析。结果显示微分干涉差显微成像相比于传统的明场成像具有更好的分辨率,可以更有效检测HF酸洗后暴露的各种浅塑性亚表面损伤。对两组抛光元件的亚表面损伤的对比分析发现熔石英元件在抛光中会产生大量的亚表面损伤,这些亚表面损伤绝大多数是浅塑性的划痕和坑,仅有少量的脆性断裂损伤,较大的抛光颗粒会产生更多更严重的亚表面损伤,并且这些亚表面损伤被表面沉积层所掩盖,表面粗糙度不能反映亚表面损伤的严重程度。     

静/动态刻蚀对熔石英表面质量和激光损伤的影响

为了研究静/动态刻蚀过程中熔石英表面质量和抗激光损伤性能的演变规律,优化化学刻蚀工艺,使用HF酸缓冲液对熔石英分别进行了不同时间的静/动态刻蚀处理。实验表明,由于兆声场辅助搅拌作用,熔石英动态刻蚀的刻蚀速率快于静态刻蚀。动态刻蚀后熔石英表面均方根(RMS)粗糙度和反射面形分别为 < 1 nm和0.46λ,其3倍频透射率先小幅增加后保持稳定,相比初始表面增加约0.1%。而静态刻蚀使得表面RMS粗糙度和反射面形分别增加至~5 nm和0.82λ,其3倍频透射率先基本不变后下降,相比初始表面下降约0.4%。二者损伤阈值呈现明显不同变化规律:静态刻蚀使熔石英损伤阈值先小幅增加约30%后逐渐降低,动态刻蚀使熔石英损伤阈值增加近一倍后保持相对稳定。结果表明,动态刻蚀后熔石英光学元件性能明显优于静态刻蚀。     

熔石英再沉积层结构的纳米级表征和杂质分析

利用原子力显微镜观察熔石英不同蚀刻时间的表面形貌,结合二次离子质谱分析,研究了熔石英的再沉积层结构和杂质分布。结果表明,熔石英表面深度10nm的再沉积层内存在大量微裂纹和杂质,经蚀刻展开形成nm级划痕和坑点,其分布随着深度增加呈指数衰减。根据nm级划痕密度、宽深比随蚀刻深度变化的规律,估算出再沉积层厚度,估算结果与二次离子质谱测得的杂质嵌入深度基本一致。杂质元素嵌入深度与抛光微裂纹分布特征的关联性表明,杂质很有可能藏匿在抛光微裂纹中。     

熔石英元件HF刻蚀的实验研究

为深入了解熔石英元件化学刻蚀过程,研究了HF刻蚀反应机理、HF刻蚀工艺参数以及刻蚀对表面质量的影响规律。通过控制变量法,获得刻蚀速率随HF浓度、刻蚀温度以及NH4F浓度的变化规律。对刻蚀不同深度后的元件表面粗糙度、形貌、杂质含量以及激光损伤阈值进行了检测,实验结果表明:刻蚀速率受多种因素共同影响,其中HF浓度的促进作用最为显著;刻蚀后的熔石英表面形貌复杂,有横向、纵向、拖尾等形式的划痕,以及坑点、杂质等缺陷,其中横向划痕和纵向划痕占据了缺陷部分的主体,主要杂质铈元素随刻蚀时间的增长不断减少;激光损伤阈值测量实验表明,通过HF刻蚀将元件损伤阈值提高了59.6%。     

酸蚀深度对熔石英三倍频激光损伤阈值的影响

 采用干涉仪和台阶仪测试蚀刻深度随时间的变化,结合材料去除速率测量,研究了HF酸蚀液对熔石英表面蚀刻的影响。测试了蚀刻后损伤阈值和表面粗糙度的变化。研究表明,熔石英表面重沉积层厚度约16 nm,亚表面缺陷层大于106 nm;重沉积层去除后损伤阈值增大,随亚表面缺陷层暴露其阈值先降低后又增加,最后趋于稳定;然而,随蚀刻时间的增加,其表面粗糙度增大。分析表明,蚀刻到200 nm能有效地提高熔石英的低损伤阈值,有利于降低初始损伤点数量和提高熔石英表面的机械强度。     

Ultraviolet laser-induced damage on fused silica substrate and its sol-gel coating

A comparative study of the laser-induced damage thresholds (LIDTs) of fused silica substrates and their sol-gel silica coatings was carried out with 355 nm laser irradiation. Chemical etching and superpolishing were employed in different ways to improve the substrate. The laser damage tests showed that the coated substrate was no more susceptible to laser damage than the bare substrate, showing that the substrate quality was the dominant factor limiting the LIDT for UV irradiation. In addition, it was found that high value of substrate microroughness was more harmful to the LIDT of the coated than the bare substrate, and that a proper combination of etching and superpolishing can optimize the LIDT.     

激光诱导HF酸刻蚀后熔石英后表面划痕的损伤行为研究

用光学显微镜和原子力显微镜记录HF酸刻蚀后熔石英元件后表面划痕的形貌结构,并利用单脉冲激光对其进行辐照测试,以研究不同结构参数划痕的激光损伤特性.实验结果表明,由于HF酸的腐蚀钝化作用,划痕结构横向截面呈余弦形分布;其初始损伤阈值并非由单一的划痕宽度或深度参数决定,而是与其横向剖面结构的宽深比值密切相关;通过实验得到了二者之间的关系曲线,并采用时域有限差分算法对不同结构参数划痕附近光场分布进行理论模拟,理论场计算得到的增强结果与实验值符合得很好.     

低亚表面损伤石英光学基底的加工和检测技术

制备低亚表面损伤的超光滑光学基底,是获得高损伤阈值薄膜的前提条件。针对石英材料在不同加工工序中引入亚表面损伤层的差异,首先利用共焦显微成像结合光散射的层析扫描技术,对W10和W5牌号SiC磨料研磨后的亚表面缺陷进行了检测,讨论了缺陷尺寸与散射信号强度、磨料粒径与损伤层深度间的对应关系;同时,采用化学腐蚀处理技术对抛光后样品的亚表面形貌进行了刻蚀研究,分析了化学反应生成物和亚表面缺陷对刻蚀速率的影响、不同深度下亚表面缺陷的分布特征,以及均方根粗糙度与刻蚀深度间的联系。根据各道加工工艺的不同采用了相应的亚表面检测技术,由此来确定下一道加工工序,合理的去除深度,最终获得了极低亚表面损伤的超光滑光学基底。     

K9基片的亚表面损伤探测及化学腐蚀处理技术研究

 研究了几种类型的腐蚀液对K9基片化学腐蚀的影响。通过腐蚀液对基片纵向腐蚀速度的变化初步判断了K9基片重沉积层的深度。考察了腐蚀前后基片表面参数的变化以及腐蚀对激光损伤阈值的影响。研究表明,特定的腐蚀液能够对K9基片进行平稳可控的腐蚀,并且腐蚀能提高其激光损伤阈值,其主要原因是去除了重沉积层及表面、亚表面缺陷中的污染物,但过多的腐蚀会暴露本来为重沉积层所掩盖的划痕等亚表面缺陷,所以腐蚀并非越深越好。同时,表面各种杂质与缺陷的去除能够提高材料的机械强度,从而也有利于提高材料的激光损伤阈值。     

预处理对355nm激光作用下熔石英损伤增长的影响

测试了经化学蚀刻、紫外激光预处理及其共同处理后的熔石英355 nm激光损伤阈值;研究了处理前后其损伤斑面积随激光辐照脉冲数的增长情况。结果表明,处理后熔石英355 nm激光损伤阈值得到了提高,且损伤斑面积增长变慢。利用CO2激光对熔石英表面损伤点进行了修复处理,修复后的损伤点R-on-1抗损伤阈值和基底阈值相当,损伤增长得到有效抑制。     

Femtosecond laser-assisted etching of three-dimensional inverted-woodpile structures in fused silica

Three-dimensional inverted-woodpile (WP) structures were embedded in a microchannel by femtosecond laser direct-writing of fused silica followed by chemical etching with diluted hydrofluoric acid. We show the hole size is linearly dependent on laser-scanning depth for various pulse energies, permitting the control of laser exposures to facilitate close 5 μm periodic packing of uniform microcapillary arrays. Exposure compensation for depth-dependent etching rate and optical beam aberrations yielded stable and crack-free uniform inverted-WP structures. The direct formation of the inverted-WP structure together with microchannels in an all-fused silica substrate, offers chemical stability and inertness, and biocompatibility to be exploited as new microfluidic systems for chromatography and electro-osmotic pumps.     

HF酸刻蚀提升熔石英亚表面划痕抗损伤性能的机理

用HF酸刻蚀熔石英元件,研究刻蚀对元件后表面划痕的形貌结构及损伤性能的影响,探索损伤阈值提升的原因.时域有限差分算法理论计算结果表明:对于含有50nm直径氧化锆颗粒的划痕,对入射光调制引发场增强的最大值是入射光强的6.1倍,且最强点位于划痕内部氧化锆颗粒附近,而结构相同但不含杂质的划痕引发的最大场增强为入射光强的3.6倍,最强区位于划痕外围;HF酸刻蚀能够有效去除划痕中的杂质,改变划痕结构,增加其宽深比值,经刻蚀的划痕对入射光调制引发场增强降低到入射光强的2.2倍.实验结果表明,经过深度刻蚀的划痕初始损伤阈值较刻蚀之前提高一倍多;光热弱吸收测试仪测试刻蚀后划痕对1 064nm激光的吸收最大值仅为230ppm.HF酸刻蚀同时可以提升元件整体损伤阈值,由于元件上无缺陷区域损伤阈值随刻蚀的深入先增加后降低,因此HF酸刻蚀应进行到元件损伤阈值提升到最大值为止.     

Correlation of polishing-induced shallow subsurface damages with laser-induced gray haze damages in fused silica optics

Laser-induced damage in fused silica optics greatly restricts the performances of laser facilities. Gray haze damage,which is always initiated on ceria polished optics, is one of the most important damage morphologies in fused silica optics.In this paper, the laser-induced gray haze damages of four fused silica samples polished with CeO_2, Al_2O_3, ZrO_2, and colloidal silica slurries are investigated. Four samples all present gray haze damages with much different damage densities.Then, the polishing-induced contaminant and subsurface damages in four samples are analyzed. The results reveal that the gray haze damages could be initiated on the samples without Ce contaminant and are inclined to show a tight correlation with the shallow subsurface damages.     

超声波辅助酸蚀提高熔石英损伤阈值

为了提高熔石英元件表面抗激光损伤阈值,利用超声波辅助HF酸研究平滑光学元件表面缺陷形貌和去除刻蚀后残留物效果,通过扫描电子显微镜电镜和原子力显微镜记录表面形貌结构,以及单脉冲激光辐照测试抗损伤阈值确定实验参数。研究表明,超声波场的引入能催化HF酸的刻蚀速率、提高钝化效果并且更易剥离嵌入的亚μm级杂质粒子。经过实验测试,获得了熔石英类元件相匹配的超声辅助HF酸刻蚀实验参数,研究结果对应用超声波辅助HF酸研究熔石英表面抗激光损伤有重要意义。     

Subwavelength structures for high power laser antireflection application on fused silica by one-step reactive ion etching

In this paper we report a simple method to fabricate a novel subwavelength structure surface on fused silica substrate using one-step reactive ion etching with two-dimensional polystyrene colloidal crystals as masks. The etching process and the morphologies of the obtained structure are controlled. We show that the period of the obtained fused silica pillar-like arrays were determined by the initial polystyrene nanoparticle size. The height of pillar arrays can be adjusted by controlling the etching duration, which is proved to be of importance in tailoring the antireflection properties of subwavelength structures surface. The novel subwavelength structures surface exhibit excellent broadband antireflection properties, but the size of the pillar affects the antireflective properties in short wavelength region. We anticipate this method would offer a convenient and scalable way for inexpensive and high-efficiency high power laser field designs.