亚表面缺陷和杂质诱导光增强的模拟及其检测和控制研究
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摘要
作为高功率激光系统的透射和衍射元件的体材料，熔石英在惯性约束聚变领域获得了广泛应用，并因此获得了广泛的研究。由于玻璃态石英的体材料缺陷和杂质极少，激光诱导损伤（LID）不容易在体内发生。相反，大多数的损伤发生在表面。目前，熔石英的表面损伤仍然是一个正在被广泛研究的突出问题，因为损伤点一旦发生，便会很快扩展，不仅会产生光学散射，而且会对下游元件施加额外的调制，从而极大地限制了光学元件的使用寿命。另一方面，由于昂贵的材料价格，又催生了损伤斑的修复工作，以利于元件的循环使用。
本论文结合光学显微镜、原子力显微镜（AFM）、探针式轮廓仪等相关检测结果，利用时域有限差分（FDTD）方法系统模拟了亚表面划痕、损伤修复坑和杂质对入射激光的调制作用。在实验上，对溶胶-凝胶薄膜进行了激光预处理，同时，初步开展了膜面颗粒污染的激光清洗工作和有机污染膜厚的精确测定工作。主要结论如下：
(1)根据研磨、抛光过程中碎裂的几何形貌，建立了熔石英亚表面的连续横向划痕、坑点状断点划痕、赫兹-锥型划痕（HCC）、拖尾的锯齿状划痕（TIC）的三维模型。使用FDTD模拟发现，对光场调制作用最强的是HCC，当其内界面与垂直方向的夹角θ约π/6时，可获得最大调制；当π/8<θ<π/4时，光强增强因子（LIEF）很容易突破100，且随着化学刻蚀的进行，调制有减弱趋势。连续横向划痕调制其次，当其宽深比值R取1~3时，可获最大调制，LIEFmax为18.49。断点划痕与TIC最弱，且相互接近，其LIEFmax分别为12.9和11.2。
(2)当横向划痕表面镀上HfO_2/SiO_2多层高反膜，并用基频光在前表面辐照时，膜系的不平整处最容易形成光场增强区，且强区可延伸到基底内部。膜系的这类缺陷产生LIEF可超过30。当划痕宽度达5λ时，其调制与节瘤缺陷相当。
(3)对于亚表面的损伤修复坑，FDTD研究指出镶嵌在亚表面内部的未修复裂纹对场的调制最显著，LIEFmax可达24.3。随着气泡数目的增多，调制有增强趋势。对于含有裂纹或气泡的修复坑，当裂纹或气泡位于近表面层3λ以内且靠近修复面边缘时，对场的调制最明显。使用不同的激光参数，修复坑将会带有不同程度的凸环和凹环。FDTD研究指出，当凹环坑将向凸环坑缓慢转化时，场调制先逐渐减小然后递增，即调制强弱依次为：凸环坑>凹环坑>高斯坑。
(4)对于溶胶-凝胶减反射膜表面的石英颗粒污染，颗粒位于前表面比位于后表面可产生更大的光场增强，前表面颗粒的LIEFmax达77.5。元件内部的调制峰值呈衰减趋势，颗粒位于前、后表面的衰减长度分别约3λ和2λ。此外，球形颗粒可比椭球颗粒产生更大的调制。
(5)对含有杂质的溶胶-凝胶SiO_2薄膜采用小光斑激光扫描预处理。预处理后，洁净薄膜的R:1损伤阈值变化不大，含非吸收性杂质的薄膜阈值有所增强，含吸收性杂质的薄膜阈值无显著变化且不足洁净样品的一半。
(6)用激光冲击波清洗（LSC）来移除溶胶-凝胶薄膜表面的颗粒污染。相比于直接将激光辐照于样品表面的干式激光清洗，LSC具有更高的清洗效率，且清洗后被污染膜面的透射率能较好地恢复到污染前的水平。
(7)椭圆偏振光谱法测试具有较好的准确性，有机膜厚的不均匀性是椭偏精确测定的最大障碍。AFM测试膜厚的关键在于所制备台阶的质量，台阶尺寸应在AFM测试量程之内。在AFM分析中，某点膜厚可采用单线台阶高度差，区域平均膜厚可采用台阶两侧像素中值作差。
上述结果表明在常见亚表面缺陷和杂质中，HCC对光场的近场增强作用最为明显，其次是透明石英颗粒杂质。但是相关缺陷对远场的调制作用，以及对热致损伤的影响还有待考证。在实验上，LSC的参数变量（颗粒尺寸、激光能量、瞄准距离等）与清洗效率的关系需要具体量化，其理论研究和工艺研究也需要进一步开展和验证。在污染物的检测方面，亟需展开对污染物质的化学成分分析，然后利用椭偏仪动态监测污染物的沉积过程。
Being as bulk material in transmissive and diffractive optics for high-power lasersystems, research of vitreous silica has been motivated prominently by its ubiquity ininertial confinement fusion. Since the amorphous silica bulk material is manufacturedfree of impurities and defects, laser-induced damage (LID) events rarely occur insidethe bulk. Instead, most damage is found on the surfaces. Up to now, the surface damageof fused silica has been a predominate issue subjecting to extensive studies. Once adamage site initiates, it grows catastrophically under further irradiation. Moreover, itnot only generates the optical scattering, but also imposes added modulation on thedownstream optical devices. Thereby, it dramatically shorten the service lifetime ofoptics. On the other hand, produced from high-quality SiO_2, these components arerelatively expensive and it is of great interest in terms of damage repair and recycling.
In this thesis, we detailedly investigated the light intensification around defects byusing finite-difference time-domain (FDTD) algorithm, associating with relevantexperimental results of optical microscope, atomic force microscope (AFM), and stylusprofilometer. The aforementioned defects are cracks in subsurface, repaired damagesites, and contaminants on anti-reflective film optics. In experimental department, laserconditioning of sol-gel SiO_2films, laser shockwave cleaning (LSC), and measuration oforganic film thickness have been investigated. Main conclusions are made as follows:
(1) According to fracture geometry during grinding and polishing steps, subsurfacecracks can be divided into lateral crack, discontinuous crack, Hertzian-conical crack(HCC), trailing indent crack (TIC), et al. FDTD numerical studies show that lightintensity enhancement induced by HCC is the most remarkable of all. There will be ahighest modulation when inclination angle θ is around π/6. When θ ranges from π/8toπ/4, the light intensity enhancement factor (LIEF) can easily break through100, and themodulation follows a decreasing trend in further etching. The intensification induced bylateral crack is the second strong, and the LIEFmaxis18.49when the breadth depth ratioR belongs to the range of1~3. The modulations formed by discontinuous crack and TICare the weakest and close to each other, and the LIEFmaxare12.9and11.2, respectively.
(2) The modulation of HfO_2/SiO_2high reflector deposited on lateral cracks hasbeen discussed when1053nm laser irradiates on the input surface. Results show thatthe catface of the reflectance coatings generate much larger intensity enhancement thanother sites. Moreover, the intensification extends to the substrate inside. The defectmentioned above can cause LIEF greater than30. When the crack width is larger than5λ, the modulation is equal to nodular defects.
(3) As for repaired damage sites, it is shown that the unrepaired cracks cangenerate notable modulation, whose LIEFmaxreaches24.3. With increasing the numberof bubble in subsurface, a larger modulation acquired. When crack or bubble distributesin the near-surface area (<3λ) and close to the edge of crater ring, the field modulationis obvious. Damage sites irradiated by CO_2laser at different parameters give birth totwo nonideal craters, with raised rim as well as with concave rim. When the concaverim converts to the raised rim, the modulation undergoes decreasing firstly and thenincreasing. That is to say, the order of laser intensification power is: craters with a raisedrim> craters with a concave rim> ideal Gaussian craters.
(4) The light intensity enhancement induced by particulate silica contaminants onanti-reflective film has been studied by utilizing the FDTD method. Result showsparticles on the input surface generate much larger intensity enhancement than on theoutput surface. Peak field modulation inside the component manifests an attenuationtrend, and the attenuation length are3λ and2λ for the input-and output-surface particlesrespectively. Comparing with the ellipsoidal structure, the spherical particles cangenerate larger ehancement. For irradiation under3ω laser, silica particles can causeLIEF as high as77.5.
(5) The influence of sol-gel SiO_2films after raster scanning laser conditioning witha1064nm Nd:YAG pulsed laser has been investigated. The results show no obviouschange of the laser-induced damage threshold (LIDT,“R-on-1” regime) of clean films.Damage characteristics of transparent impurities films have been improved. The LIDTsof the samples contained absorbing impurities are less than half of the clean ones.
(6) LSC has been used to remove the particulate contamination from SiO_2sol-geloptical film. Compared with dry laser cleaning (DLC), LSC with shockwave initiatedby plasma formation under a focused laser beam pulse has much better efficiency.Furthermore, it has been demonstrated that the transmittance of contaminated SiO_2film can restores to the non-contaminated after LSC.
(7) The spectroscopic ellipsometry is a precision instrument in measuring filmthickness. The inhomogeneity of the film is the most notable obstacle for precisemeasurement. Thickness measured by AFM is mostly determined by the prepared steps.The step size should be within the range of the AFM. In AFM analysis, the thickness ofa point is corresponding to one-line step height difference. And the average thickness ofan area is corresponding to the median pixel value difference on both step sides.
Above results indicate that the HCC can generate the most obvious lightintensification of all, followed by silica particles impurities. The theoretical simulationsand experimental investigations progress greatly and achieve the anticipative objectives.However, related defects in the far-field modulation, and thermal induced damage is yetto be verified. In the LSC experiments, dependences of the parameter variables (particlesize, laser energy, gap distance) and cleaning efficiency need to be quantified, andtheoretical research and technology research also need further development andvalidation. In addition, it is necessary to carry out the analysis of the chemicalcomposition in pollutants detection, and then take advantage of the ellipsometerdynamic monitoring the pollutant deposition process.
本论文结合光学显微镜、原子力显微镜（AFM）、探针式轮廓仪等相关检测结果，利用时域有限差分（FDTD）方法系统模拟了亚表面划痕、损伤修复坑和杂质对入射激光的调制作用。在实验上，对溶胶-凝胶薄膜进行了激光预处理，同时，初步开展了膜面颗粒污染的激光清洗工作和有机污染膜厚的精确测定工作。主要结论如下：
(1)根据研磨、抛光过程中碎裂的几何形貌，建立了熔石英亚表面的连续横向划痕、坑点状断点划痕、赫兹-锥型划痕（HCC）、拖尾的锯齿状划痕（TIC）的三维模型。使用FDTD模拟发现，对光场调制作用最强的是HCC，当其内界面与垂直方向的夹角θ约π/6时，可获得最大调制；当π/8<θ<π/4时，光强增强因子（LIEF）很容易突破100，且随着化学刻蚀的进行，调制有减弱趋势。连续横向划痕调制其次，当其宽深比值R取1~3时，可获最大调制，LIEFmax为18.49。断点划痕与TIC最弱，且相互接近，其LIEFmax分别为12.9和11.2。
(2)当横向划痕表面镀上HfO_2/SiO_2多层高反膜，并用基频光在前表面辐照时，膜系的不平整处最容易形成光场增强区，且强区可延伸到基底内部。膜系的这类缺陷产生LIEF可超过30。当划痕宽度达5λ时，其调制与节瘤缺陷相当。
(3)对于亚表面的损伤修复坑，FDTD研究指出镶嵌在亚表面内部的未修复裂纹对场的调制最显著，LIEFmax可达24.3。随着气泡数目的增多，调制有增强趋势。对于含有裂纹或气泡的修复坑，当裂纹或气泡位于近表面层3λ以内且靠近修复面边缘时，对场的调制最明显。使用不同的激光参数，修复坑将会带有不同程度的凸环和凹环。FDTD研究指出，当凹环坑将向凸环坑缓慢转化时，场调制先逐渐减小然后递增，即调制强弱依次为：凸环坑>凹环坑>高斯坑。
(4)对于溶胶-凝胶减反射膜表面的石英颗粒污染，颗粒位于前表面比位于后表面可产生更大的光场增强，前表面颗粒的LIEFmax达77.5。元件内部的调制峰值呈衰减趋势，颗粒位于前、后表面的衰减长度分别约3λ和2λ。此外，球形颗粒可比椭球颗粒产生更大的调制。
(5)对含有杂质的溶胶-凝胶SiO_2薄膜采用小光斑激光扫描预处理。预处理后，洁净薄膜的R:1损伤阈值变化不大，含非吸收性杂质的薄膜阈值有所增强，含吸收性杂质的薄膜阈值无显著变化且不足洁净样品的一半。
(6)用激光冲击波清洗（LSC）来移除溶胶-凝胶薄膜表面的颗粒污染。相比于直接将激光辐照于样品表面的干式激光清洗，LSC具有更高的清洗效率，且清洗后被污染膜面的透射率能较好地恢复到污染前的水平。
(7)椭圆偏振光谱法测试具有较好的准确性，有机膜厚的不均匀性是椭偏精确测定的最大障碍。AFM测试膜厚的关键在于所制备台阶的质量，台阶尺寸应在AFM测试量程之内。在AFM分析中，某点膜厚可采用单线台阶高度差，区域平均膜厚可采用台阶两侧像素中值作差。
上述结果表明在常见亚表面缺陷和杂质中，HCC对光场的近场增强作用最为明显，其次是透明石英颗粒杂质。但是相关缺陷对远场的调制作用，以及对热致损伤的影响还有待考证。在实验上，LSC的参数变量（颗粒尺寸、激光能量、瞄准距离等）与清洗效率的关系需要具体量化，其理论研究和工艺研究也需要进一步开展和验证。在污染物的检测方面，亟需展开对污染物质的化学成分分析，然后利用椭偏仪动态监测污染物的沉积过程。
Being as bulk material in transmissive and diffractive optics for high-power lasersystems, research of vitreous silica has been motivated prominently by its ubiquity ininertial confinement fusion. Since the amorphous silica bulk material is manufacturedfree of impurities and defects, laser-induced damage (LID) events rarely occur insidethe bulk. Instead, most damage is found on the surfaces. Up to now, the surface damageof fused silica has been a predominate issue subjecting to extensive studies. Once adamage site initiates, it grows catastrophically under further irradiation. Moreover, itnot only generates the optical scattering, but also imposes added modulation on thedownstream optical devices. Thereby, it dramatically shorten the service lifetime ofoptics. On the other hand, produced from high-quality SiO_2, these components arerelatively expensive and it is of great interest in terms of damage repair and recycling.
In this thesis, we detailedly investigated the light intensification around defects byusing finite-difference time-domain (FDTD) algorithm, associating with relevantexperimental results of optical microscope, atomic force microscope (AFM), and stylusprofilometer. The aforementioned defects are cracks in subsurface, repaired damagesites, and contaminants on anti-reflective film optics. In experimental department, laserconditioning of sol-gel SiO_2films, laser shockwave cleaning (LSC), and measuration oforganic film thickness have been investigated. Main conclusions are made as follows:
(1) According to fracture geometry during grinding and polishing steps, subsurfacecracks can be divided into lateral crack, discontinuous crack, Hertzian-conical crack(HCC), trailing indent crack (TIC), et al. FDTD numerical studies show that lightintensity enhancement induced by HCC is the most remarkable of all. There will be ahighest modulation when inclination angle θ is around π/6. When θ ranges from π/8toπ/4, the light intensity enhancement factor (LIEF) can easily break through100, and themodulation follows a decreasing trend in further etching. The intensification induced bylateral crack is the second strong, and the LIEFmaxis18.49when the breadth depth ratioR belongs to the range of1~3. The modulations formed by discontinuous crack and TICare the weakest and close to each other, and the LIEFmaxare12.9and11.2, respectively.
(2) The modulation of HfO_2/SiO_2high reflector deposited on lateral cracks hasbeen discussed when1053nm laser irradiates on the input surface. Results show thatthe catface of the reflectance coatings generate much larger intensity enhancement thanother sites. Moreover, the intensification extends to the substrate inside. The defectmentioned above can cause LIEF greater than30. When the crack width is larger than5λ, the modulation is equal to nodular defects.
(3) As for repaired damage sites, it is shown that the unrepaired cracks cangenerate notable modulation, whose LIEFmaxreaches24.3. With increasing the numberof bubble in subsurface, a larger modulation acquired. When crack or bubble distributesin the near-surface area (<3λ) and close to the edge of crater ring, the field modulationis obvious. Damage sites irradiated by CO_2laser at different parameters give birth totwo nonideal craters, with raised rim as well as with concave rim. When the concaverim converts to the raised rim, the modulation undergoes decreasing firstly and thenincreasing. That is to say, the order of laser intensification power is: craters with a raisedrim> craters with a concave rim> ideal Gaussian craters.
(4) The light intensity enhancement induced by particulate silica contaminants onanti-reflective film has been studied by utilizing the FDTD method. Result showsparticles on the input surface generate much larger intensity enhancement than on theoutput surface. Peak field modulation inside the component manifests an attenuationtrend, and the attenuation length are3λ and2λ for the input-and output-surface particlesrespectively. Comparing with the ellipsoidal structure, the spherical particles cangenerate larger ehancement. For irradiation under3ω laser, silica particles can causeLIEF as high as77.5.
(5) The influence of sol-gel SiO_2films after raster scanning laser conditioning witha1064nm Nd:YAG pulsed laser has been investigated. The results show no obviouschange of the laser-induced damage threshold (LIDT,“R-on-1” regime) of clean films.Damage characteristics of transparent impurities films have been improved. The LIDTsof the samples contained absorbing impurities are less than half of the clean ones.
(6) LSC has been used to remove the particulate contamination from SiO_2sol-geloptical film. Compared with dry laser cleaning (DLC), LSC with shockwave initiatedby plasma formation under a focused laser beam pulse has much better efficiency.Furthermore, it has been demonstrated that the transmittance of contaminated SiO_2film can restores to the non-contaminated after LSC.
(7) The spectroscopic ellipsometry is a precision instrument in measuring filmthickness. The inhomogeneity of the film is the most notable obstacle for precisemeasurement. Thickness measured by AFM is mostly determined by the prepared steps.The step size should be within the range of the AFM. In AFM analysis, the thickness ofa point is corresponding to one-line step height difference. And the average thickness ofan area is corresponding to the median pixel value difference on both step sides.
Above results indicate that the HCC can generate the most obvious lightintensification of all, followed by silica particles impurities. The theoretical simulationsand experimental investigations progress greatly and achieve the anticipative objectives.However, related defects in the far-field modulation, and thermal induced damage is yetto be verified. In the LSC experiments, dependences of the parameter variables (particlesize, laser energy, gap distance) and cleaning efficiency need to be quantified, andtheoretical research and technology research also need further development andvalidation. In addition, it is necessary to carry out the analysis of the chemicalcomposition in pollutants detection, and then take advantage of the ellipsometerdynamic monitoring the pollutant deposition process.
引文
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