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.     

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。     

Improvement of laser damage thresholds of fused silica by ultrasonic-assisted hydrofluoric acid etching

Polished fused silica samples were etched for different durations by using hydrofluoric(HF) acid solution with HF concentrations in an ultrasonic field. Surface and subsurface polishing residues and molecular structure parameters before and after the etching process were characterized by using a fluorescence microscope and infrared(IR) spectrometer, respectively. The laser induced damage thresholds(LIDTs) of the samples were measured by using pulsed nanosecond laser with wavelength of 355 nm. The results showed that surface and subsurface polishing residues can be effectively reduced by the acid etching process, and the LIDTs of fused silica are significantly improved. The etching effects increased with the increase of the HF concentration from 5 wt.% to 40 wt.%. The amount of polishing residues decreased with the increase of the etching duration and then kept stable. Simultaneously, with the increase of the etching time, the mechanical strength and molecular structure were improved.     

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。     

激光诱导熔石英表面损伤修复中的气泡形成和控制研究

基于熔石英材料在CO_2激光作用下的温度分布和结构参数变化的计算结果,对熔石英损伤修复中的气泡形成和控制进行了研究.针对损伤尺寸介于150—250μm之间的损伤点,提出了一种能够有效控制气泡形成的长时间低温预热修复方法.基于低温下熔石英材料结构弛豫时间常数较长的特点,该方法在不引起熔石英材料结构发生显著变化的同时,能够解吸附表面和裂纹处所附着的气体和杂质,可有效降低裂纹闭合过程中气泡形成的概率.实验结果表明,长时间低温预热修复方法的成功修复概率可达到98%.     

熔石英紫外激光初始损伤形态分析

 采取355 nm激光脉冲辐照熔石英样品,利用Nomarski微分干涉差显微镜、原子力显微镜和扫描电子显微镜观测手段对前后表面产生的损伤点进行了观察分析。对前后表面损伤形态做出详细的描述和分类,从理论上对每种损伤类型产生的条件与机理做出推测。实验结果表明：熔石英前表面存在小麻点群损伤和星状裂纹损伤两种损伤形态,横向尺寸分别为0.8～2.5和1.0～5.5 μm;后表面存在小麻点群损伤、壳状剥离损伤和火山口3种损伤形态,损伤横向尺寸分别为0.48～1.33,4～20和12～30 μm。实验证明了1 μm尺度损伤点的产生与再沉积层密切相关。     

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.     

Incident laser modulation of a repaired damage site with a rim in fused silica rear subsurface

Local CO2 laser treatment has proved to be an effective method to prevent the 351-nm laser-induced damage sites in a fused silica surface from exponentially growing, which is responsible for limiting the lifetime of optics in high fluence laser systems. However, the CO2 laser induced ablation crater is often surrounded by a raised rim at the edge, which can also result in the intensification of transmitted ultraviolet light that may damage the downstream optics. In this work, the three-dimensional finite-difference time-domain method is developed to simulate the distribution of electrical field intensity in the vicinity of the CO2 laser mitigated damage site located in the exit subsurface of fused silica. The simulated results show that the repaired damage sites with raised rims cause more notable modulation to the incident laser than those without rims. Specifically, we present a theoretical model of using dimpled patterning to control the rim structure around the edge of repaired damage sites to avoid damage to downstream optics. The calculated results accord well with previous experimental results and the underlying physical mechanism is analysed in detail.     

CO_2激光光栅式扫描修复熔石英表面缺陷的实验研究与数值模拟

基于熔石英材料对波长为10.6μm的CO2激光具有强吸收作用这一特点,提出采用CO2激光光栅式多次扫描修复熔石英光学元件表面密集分布的划痕和抛光点等缺陷的方法.实验结果表明,在合理的扫描参数下,元件表面的划痕和抛光点等缺陷可被充分地消除.损伤阈值测试结果表明,表面划痕和抛光点等缺陷被完全消除的元件的损伤阈值可回复到或超过基底的损伤阈值.同时结合有限元软件Ansys的模拟结果分析了CO2激光扫描修复及消除元件表面划痕和抛光点等缺陷的过程.本文为消除元件表面划痕和抛光点等缺陷提供了非常有意义的参考.     

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。     

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。     

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。     

熔石英损伤修复坑下游光场调制的数值模拟与实验研究

系统研究了熔石英激光损伤修复后的形貌特征,根据测量数据建立了典型的损伤修复坑三维模型,利用标量衍射理论并结合快速傅里叶变换算法研究了修复坑在351 nm激光辐照下游光场调制的分布规律.研究表明,修复坑引起的光场调制会使得下游不同距离位置处出现环形光场增强区和轴上位置光场增强点;环形光场增强区位置距离修复元件较近,其环形调制极大值主要受修复坑深度的影响,且随修复坑深度的增大而逐渐增加;轴上位置光场增强点位置距离修复元件较远,其轴上调制极大值主要受修复坑边缘凸起高度的影响,且随凸起高度的增大而快速增加;环形调制极大值或轴上调制极大值增大的同时,其分布位置与修复元件之间的距离均会逐渐减小.实验验证表明,利用三维修复坑模型得到的下游光场调制数值模拟结果与实验测量结果具有较好的一致性.本研究结果对控制熔石英元件损伤修复形貌特征以抑制调制增强效应给出了具体的控制方向,对修复工艺的改进与完善提供了非常有意义的参考.     

Numerical simulation of the modulation to incident laser by the repaired damage site in a fused silica subsurface

One of the main factors of laser induced damage is the modulation to incident laser which is caused by the defect in the subsurface of the fused silica.In this work,the repaired damage site irradiated by CO 2 laser is simplified to a Gaussian rotation according to the corresponding experimental results.Then,the three-dimensional finite-difference time-domain method is employed to simulate the electric field intensity distribution in the vicinity of this kind of defect in fused silica front subsurface.The simulated results show that the modulation is notable,the E max is about 2.6 times the irradiated electric field intensity in the fused silica with the damage site (the width is 1.5 μm and depth is 2.3 μm) though the damage site is repaired by CO 2 laser.The phenomenon and the theoretical result of the annular laser enhancement existed on the rear surface are first verified effectively,which agrees well with the corresponding experimental results.The relations between the maximal electric field intensity in fused silica with defect depth and width are given respectively.Meanwhile,the corresponding physical mechanism is analysed theoretically in detail.     

化学刻蚀过程中熔石英表面沉积物的形成及其对激光损伤的影响

化学刻蚀是提升熔石英光学元件抗激光损伤性能的重要后处理技术之一,但刻蚀后熔石英表面附着的沉积物对其表面质量、透射性能和抗激光损伤性能有很大影响。使用光学显微镜和原子力显微镜表征了化学刻蚀后附着于熔石英表面的沉积物的微观形貌,并分析了其形成机理;X射线能谱分析表明化学刻蚀后熔石英表面沉积物主要由Fe,Ni,Al等元素的金属盐组成。损伤阈值测试结果表明熔石英表面高密度沉积物区域的损伤阈值明显低于非沉积物区域,沉积物对熔石英光学元件的抗激光损伤性能产生严重影响,它们是诱导熔石英激光损伤的前驱体。     

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。     

熔石英光学元件的损伤前驱及其抑制技术北大核心CSCD

基于抛光所引起的熔石英元件表面、亚表面所存在的损伤前驱体分布,研究了不同种类的损伤前驱体所引起的损伤形貌。然后根据不同种类的损伤前驱体分别采用表面活性剂、强氧化性酸、氢氟酸的水溶液对不同的损伤前驱体进行处理。研究结果显示:经过前期预先清洗以后,吸收性杂质所导致的雾状损伤得以消除,亚表面分布的裂纹得以很好地平滑钝化,极大地提升了熔石英光学元件的抗损伤性能,损伤阈值从4.8J/cm2提高到11.0J/cm2,最大提升幅度达到原来的2.3倍。     

Optical characterization and laser damage of fused silica optics after ion beam sputtering

The sputtering process of fused silica bombarded by Ar ion beam is simulated with the SRIM software. The effects of ion beam energy and incident angle on sputtering yield and surface damage are computed. Since ion beam sputtering will result in defects in fused silica, such as E′ color centers and other lattice defects and probably Argon bubbles, the optimized sputtering energy is selected below 1 keV so that the projected range of Ar ions is less than 10 Å. The experimental results show that the scratches in subsurface of fused silica can be smoothed obviously and better surface can be obtained as the optimized parameters are used for ion beam sputtering. The laser induced damage threshold of fused silica increases by about 18% after ion beam sputtering.     

退火参数对熔石英透射波前和损伤阈值的影响

 采用高温退火技术去除熔石英元件表面由于CO2激光修复带来的残余应力,研究了退火环境对元件的表面污染,分析了不同退火温度（600～900 ℃）和保温时间（3～10 h）对于元件残余应力、透射波前、表面粗糙度和激光损伤阈值的影响。结果表明:在800 ℃以下,高温退火10 h可有效去除CO₂激光修复带来的残余应力,对元件的透射波前和表面粗糙度无明显影响;石英保护盒能有效减少退火环境对元件表面产生的污染,但仍有X射线光电子能谱检测不到的表面污染物存在;在退火后采用质量分数为1%的HF刻蚀15 min,激光损伤阈值可恢复,同时元件透射波前和表面粗糙度并无明显的增加。