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。     

光学亚表面损伤的探测和后处理技术

光学元件被污染和亚表面存在的缺陷将使它的性质受损。即使是微小尺寸的缺陷（小于φ1μm）也会引起激光损伤。国外研究表明，光学元件在其制造过程中形成的亚表面缺陷是导致紫外损伤的主要根源之一。光学元件的损伤问题已成为高功率固体激光装置研制的核心问题，而紫外的损伤尤为严重。     

磷酸盐钕玻璃表面/亚表面损伤特性实验研究

系统地研究了光学研磨过程中,磨料粒径、载荷大小以及机床转速对钕玻璃表面及亚表面损伤的影响。结果表明,机床转速和载荷基本不改变材料表面粗糙度,而较大载荷或较低机床转速产生较大的亚表面缺陷,表面粗糙度和亚表面缺陷缺陷深度基本与最大磨料粒径呈正比,载荷增倍使亚表面缺陷与表面粗糙度的常数比值增加0.05。研究结果为钕玻璃加工工艺改进提供了参考依据。     

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。     

熔石英亚表面划痕激光诱导损伤阈值实验研究

用原子力显微镜和光学显微镜观测酸蚀后熔石英亚表面划痕,并根据形貌特征将其分为Boussinesq-point-force crack(BPFC)、Hertzian-conical scratch(HCS)和Plastic indent(PI)三类,测试了各类划痕的损伤阈值,讨论了激光损伤机制。结果表明锐度较大的BPFC损伤阈值不超过2.0 J/cm<>2;深度小于1 μm的 HCS阈值可达2.6 J/cm2;形变较大的PI阈值至2.8 J/cm2,形变较小的PI的激光损伤阈值与无缺陷材料相当。BPFC 和深度超过1 μm的HCS是导致熔石英损伤阈值低的主要因素。     

熔石英亚表面划痕激光诱导损伤阈值实验研究

 用原子力显微镜和光学显微镜观测酸蚀后熔石英亚表面划痕,并根据形貌特征将其分为Boussinesq-point-force crack(BPFC)、Hertzian-conical scratch(HCS)和Plastic indent(PI)三类,测试了各类划痕的损伤阈值,讨论了激光损伤机制。结果表明锐度较大的BPFC损伤阈值不超过2.0 J/cm<>2;深度小于1 μm的 HCS阈值可达2.6 J/cm²;形变较大的PI阈值至2.8 J/cm2,形变较小的PI的激光损伤阈值与无缺陷材料相当。BPFC 和深度超过1 μm的HCS是导致熔石英损伤阈值低的主要因素。     

光学亚表面损伤的探测和后处理技术

光学元件的损伤问题已成为高功率固体激光装置研制的核心问题，而紫外的损伤尤为严重。光学元件的激光损伤与能吸收能量的多种缺陷有关，例如：表面污染、表面擦伤和材料本体的缺陷(气泡或所含杂质)等。研究工作拟从光学元件的亚表面损伤人手，探测不同的光学制造工艺造成的特征亚表面缺陷，研究这些缺陷对激光损伤研制的影响。建立亚表面缺陷化学后处理装置，减少或消除亚表面缺陷所引起激光损伤的程度，为光学元件制造工艺选型提供必要的依据。     

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。     

基于WLI原理K9基片的亚表层损伤检测

在现代激光技术的应用发展中，光学元件在其制造过程中形成的亚表层损伤是导致激光损伤的主要根源之一。光学元件亚表层的检测方法已成为光学加工领域的一个新的热点问题。利用非接触式白光干涉原理对K9基片进行亚表层损伤检测，获得基片表面至亚表面200μm深的三维立体图和纵向截切图，并精确地确定其亚表层损伤深度，以及在不同深度范围内的损伤密度。该方法与现阶段国内常用的亚表层损伤检测方法相比，具有非破坏性、纵向检测结果精确、检测过程简单快捷等特点。     

HF酸腐蚀提高K9基板损伤阈值

针对K9玻璃基板的HF酸化学腐蚀工艺开展研究,标定了40%和2%高低两种体积分数的HF酸的腐蚀速率;分析了基板表面形貌随腐蚀深度的变化规律;研究了腐蚀时间、HF酸体积分数、超声波工艺对激光损伤阈值的影响,提出了能够有效减少损伤敏感的氟硅盐沉淀、提高损伤阈值的优化腐蚀清洗工艺流程。采用优化的腐蚀清洗工艺流程进行了实验验证,结果表明用体积分数为2%的HF酸在高温和超声波条件下腐蚀90s后,测得1064nm波长激光作用下K9基板抗激光损伤阈值提高了75%。     

Controlling subsurface damage in neodymium-doped phosphate glass

We investigate the removal mechanism of neodymium-doped phosphate glass dominated in loose abrasive grinding and bound abrasive grinding. Moreover, we investigate the surface roughness and subsurface damage change with optical fabrication parameters, such as different spindle speed, load and abrasive size under different grinding processes in details. For a range of experimental conditions, we find that fracture is the principal removal mechanism for loose abrasive grinding, while plastic scratching is the dominating mechanism for bound abrasive grinding. The load has more influence on subsurface damage for bound abrasive grinding than for loose abrasive grinding. However, the spindle speed has different effect on subsurface damage produced with loose abrasive grinding and bound abrasive grinding. Moderate spindle speed and low load is preferred to produce smaller subsurface damage for loose abrasive grinding. Moreover, higher spindle speed and lower load are preferred to plastic scratching for bound abrasive grinding. Bound abrasive grinding produces 4 times lower surface roughness and 3 times lower subsurface damage than loose abrasive grinding.     

光学元件亚表面缺陷结构的蚀刻消除

 针对强激光光学元件的应用要求,对光学材料在研磨和抛光过程中形成的亚表面缺陷进行了分析,并借鉴小工具数控抛光和Marangoni界面效应,提出采用数控化学刻蚀技术来实现光学表面面形和微结构形貌的高精度加工,对亚表面缺陷具有很好的克服和消除作用。通过实验对亚表面缺陷的分布位置和特性进行了分析,同时实验验证了在静止和移动条件下Marangoni界面效应的存在,对材料的定量去除进行了实验,提出了亚表面缺陷的去除方法。     

Subsurface damage in optical substrates

The origin, character, analysis and treatment of subsurface damage (SSD) were summarized in this paper. SSD, which was introduced to substrates by manufacture processes, may bring about the decrease of laser-induced damage threshold (LIDT) of substrates and thin films. Nondestructive evaluation (NDE) methods for the measurement of SSD were used extensively because of their conveniences and reliabilities. The principle, experimental setup and some other technological details were given for total internal reflection microscopy (TIRM), high-frequency scanning acoustic microscopy (HFSAM) and laser-modulated scattering (LMS). However, the spatial resolution, probing depth and theoretic models of these NDE methods demanded further studies. Furthermore, effective surface treatments for minimizing or eliminating SSD were also presented in this paper. Both advantages and disadvantages of ion beam etching (IBE) and magnetorheological finishing (MRF) were discussed. Finally, the key problems and research directions of SSD were summarized.     

Subsurface damage of Nd-doped phosphate glasses in optical fabrication

We present a destructive method for detecting and measuring subsurface damage of Nd-doped phosphate glasses. An instrument based on the dimple method - a destructive method - was developed. Subsurface damage depth produced in each fabrication procedure was obtained. We extend the surface roughness-subsurface damage relation to Nd-doped phosphate glasses. The constant ratio of subsurface damage and surface roughness was obtained as well. We also analyse the relation of abrasive size and subsurface damage experimentally. From a measurement of the surface roughness or abrasive size, one can obtain an accurate estimate of the damage layer thickness that must be eliminated by polishing or subsequent grinding operations.     

光学元件的表面划痕及其对入射激光的调制作用

 对光学元件表面划痕进行了细致的观察,并将它们分为单划痕、双划痕和多划痕三类,采用时域有限差分方法,以加工过程中常见的直径为二分之一波长的半圆形划痕为基本研究对象,数值模拟了位于光学元件前后表面的多条划痕附近的空间光强分布,总结了在不同划痕条数下光强最大值随着划痕间距变化的曲线图。结果表明：位于光学元件后表面的划痕比位于前表面时更加容易引起光学损伤;在多条划痕情况下,空间光强最大值随着划痕间距的增大呈周期性变化,并随着划痕间距的不断增大而趋于一稳定数值。     

Analytical prediction for depth of subsurface damage in silicon wafer due to self-rotating grinding process

Subsurface damage (SSD) induced by silicon wafer grinding process is an unavoidable problem in semiconductor manufacturing. Although experimental attempts have been made on investigation of the influential factors on the SSD depth, however, few theoretical studies have been conducted to obtain SSD depth through grinding parameters. To fill the gap, an analytical model is developed to predict the SSD depth in silicon wafer due to self-rotating grinding process, which can reveal the relationship among SSD depth and the grinding parameters, the size of the abrasive grains and the radial distance from the wafer center. The establishment of the proposed model is based on scratch theory and fracture mechanics of isotropic brittle materials, and we further consider the effects of elastic recovery, cleavage plane and crystalline orientation on SSD formation. To validate the applicability of the proposed predictive model, grinding experiments with varied grinding parameters are performed and the depths of SSD along the <110> and <100> crystal directions are also measured and analyzed. The results given by the proposed model present reasonable accuracy of less than 20% deviation with experimental results. Effects of grinding parameters, wafer radial distance, crystalline orientation, and abrasive grain size on SSD depth are discussed in detail.     

Effect of polyvinylpyrrolidone on the structure and laser damage resistance of sol–gel silica anti-reflective films

The effect of polyvinylpyrrolidone (PVP) on the structure and laser-induced damage threshold (LIDT) of sol–gel silica anti-reflective films is investigated. The results of dynamic light scattering, transmission electron microscopy, and small angle X-ray scattering, show that the PVP molecules surrounded the silica sol particles through the strong hydrogen bonds between Si-OH groups and the PVP. As a result, the growth of silica particles was restricted and thus the interface layer between the silica particles and the solvent become thickened with PVP content. Furthermore, the PVP reduced the porosity of the film, so the anti-reflection properties of the film were weakened. A multi-fractal analysis showed that the appropriate addition of PVP, 1 weight percent (wt%), could improve the surface fractal structure of the film, but that higher PVP content resulted in reduced surface uniformity. The addition of PVP lead to improved LIDT.