多层介质膜脉宽压缩光栅的清洗及阈值研究
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摘要
CPA(Chirped Pulse Amplification)技术促进了高能激光器快速发展,多层介质膜脉宽压缩光栅(PCG)是CPA系统核心元件,PCG抗激光损伤能力是决定整个强激光系统能否持续稳定运行的关键。PCG在加工、制作工艺过程中会引入许多污染物质,其中包含光刻胶有机物、碳氟化合物沉积物、金属沉积物、颗粒等污染物,这些残留污染物对激光具有相当大的吸收系数,很容易形成吸热中心,进而导致PCG表面的损伤,通过选择恰当有效的清洗工艺去除PCG表面残留污染物是提高其抗激光损伤阈值的一种理想方法。
本论文紧紧围绕高性能高功率激光实验装置中一类关键的衍射光学元件—多层介质膜脉宽压缩光栅(PCG),研究PCG制作工艺过程中光栅表面引入非金属或者金属污染物这一突出问题,以扫描电镜显微镜和X射线光电子能谱为主要分析手段,定性和定量的判断PCG表面的污染物残留状态。为去除光栅表面污染物,系统开展PCG清洗研究,包括湿法清洗、干法清洗、超声辅助等。利用中国工程物理研究院八所的阈值测试平台和中科院上海光机所的阈值测试装置,进行了PCG的皮秒阂值状态确认,得到了优化的PCG清洗工艺,元件达到工程指标要求并成功应用于激光装置。在PCG清洗方面取得如下一系列重要成果。
1.对PCG湿法清洗和清洗安全进行研究。系统研究了SPM(浓硫酸和双氧水混合液)的清洗温度、组成成份、清洗时间、清洗遍数等主要参数,得到优化的SPM清洗方案；研究了不同浓度的DHF(稀释氢氟酸)对二氧化铪和二氧化硅的腐蚀特性,得到去除现行工艺PCG表面二氧化铪薄层的有效方法；研究了洗铬液对PCG顶层铬掩模去除特性,解决了洗铬液残留的铈二次污染问题,得到了理想的去除铬掩模工艺方案；研究了PCG湿法清洗安全问题,综合分析PCG湿法清洗损伤原因,发现多层膜表面节瘤是导致含双氧水清洗液清洗损伤的直接原因,并对多层膜节瘤缺陷的控制提出更高的要求；系统研究了不同频率的超声辅助清洗,得到超声辅助的有效性及不同频率下对PCG的清洗安全性,提出了兆赫兹超声辅助湿法清洗PCG的需求。
2.研究了各种气体等离子体干法清洗、相关真空设备的污染情况及干湿法结合清洗。研究了氧气、氢气和四氟化碳气体等离子体对PCG的表面干法清洗,发现氧等离子体和氢等离子体能有效的去除碳氟化合物,且前者能快速去除刻蚀残留光刻胶,尤其是利用四氟化碳等离子体剥离PCG表面材料去除其上污染物的研究,实验显示这种方法可以有效去除嵌入表层的污染物和氧等离子体难于去除的污染物；研究了PCG制作工艺相关的真空设备污染情况,光栅制作工艺中的离子束刻蚀过程存在铁等元素的污染,等离子体清洗去除光刻胶过程存在铝和铜元素污染,分析其来源,引出干法清洗之后加入一步湿法清洗的必要性,并为后续真空设备设计提出改进意见；研究HPM(盐酸、双氧水和去离子水)清洗去除金属元素污染物,并结合氧等离子体清洗,发展了一种新的干湿法结合清洗PCG方案。
3.使用10ps脉宽、1053nm波长皮秒激光对不同清洗工艺下PCG的阈值进行状态确认,在优化的SPM基础上定型了PCG清洗工艺Ⅰ,在结合氧等离子体和HPM清洗基础上定型了PCG清洗工艺Ⅱ；皮秒阂值结果显示清洗工艺Ⅱ优于清洗工艺Ⅰ,在氧等离子体处理的基础上,HPM可以在更低温度更短时间内取得与传统SPM相当甚至更好的清洗效果,能显著提升脉宽压缩光栅表面抗皮秒损伤阈值至1.6J/cm2(光栅面),通量阈值为3.4J/cm2。
4.对常见材料构成的容器进行光栅保存实验。发现PP塑料暴露空气中受湿度和光照影响会发生老化现象,有可能污染PCG表面,所以对于塑料密封容器需要避光、避氧、干燥环境下保存样品。对于受塑料老化污染的样品,在使用之前需要做进一步清洗。
Rapid development of ultra-high power laser device is attributable to the chirped pulse amplification (CPA) technology, and the induced laser damage of multilayer dielectric film gratings (PCG) wich are core components in CPA system is key factor influence on the operation of high power laser systen stable and sustainable. A wide variety of PCG surface contaminants, such as organic photoresist, fluoro-hydrocarbon deposits, metals deposits, airborne organic, and particulate contamination and so on, are introduced during the process of manufacturing gratings. These residual contaminants which have great absorption coefficient from incidencing laser pulses can easily form heat-absorbing centers and further lead to physics damage to the PCG. Therefore, selection of appropriate and effective cleaning method process to remove the surface contaminants is an ideal way to improve the laser induced damage threshold of PCG.
The cleaning of surface contaminants that impact on the laser damage threshold of PCG is studied systematically in this paper. Complete physical and chemical surface analysis techniques of USTC (University of Science and Technology of China) can be carried out to qualitatively and quantitatively evaluate the cleanliness of PCG. The laser facility for laser damage test with picosecond pulses which has been built by CAEP (China Academy of Engineering Physics) and a similar test device which has been setting up by SIOM (Shanghai Institute of Optics and Fine Mechanics) both can be employed to evaluate the laser damage threshold. And a series significant achievements of PCG cleaning have been obtained.
(1) The system research of wet cleaning with different solutions has been made. The optimization of cleaning by SPM solution has been got in the experiment. The diluted hydrofluoric acid to remove the thin hafnium oxide film which exist the top layer of PCG has been explored. The ideal process which solves the problem of secondary contaminante from chromium-etching solution used to remove chromium mask of PCG has been obtained. The reason which lead to cleaning-damage by wet cleaning has been comprehensively analysised, and new demands relating to the pre-process of PCG manufacturing have been put forward. Safety and efficiency of different frequency of ultrasonic-assisted cleaning have been explored, and the suitable type of ultrasound for PCG cleaning has been gained.
(2) The dry cleaning of various gas-plasma has been researched. The high effectiveness of removing photoresist, fluorocarbon, and some particular contaminants has been gained by using corresponding gas-plasma cleaning. The source of metal contaminants from ion beam machine and photoresist-stripping device is analysised to direct improvements of the vacuum equipment design in future. The ability of HPM solution to remove metal contaminants of PCG surface has been explored, and a new cleaning method based on the HPM solution combined with oxygen plasma for PCG has been developed.
(3) Basing on evaluation of picosecond-laser threshold of different cleaning methods, cleaning process Ⅰ and Ⅱ of PCG have been confirmed. HPM solution of cleaning process Ⅱ, combined oxygen plasma cleaning, is operated at lower temperature and shorter time than the SPM solution of cleaning process I, and the damage threshold of cleaning process Ⅱ is equate to (or even better) cleaning process I.
(4) Storage condition of PCG of the laboratory of different functional areals of humidity, temperature and other environmental paramters has been studied. It found that PP plastic may contaminate the PCG surface when it is degraded by the humity and sun in the air. Therefore, PCG should be stored in sealing-container of glass materials. The samples polluted with the degradation of PP plastic should be further cleaning before use.
本论文紧紧围绕高性能高功率激光实验装置中一类关键的衍射光学元件—多层介质膜脉宽压缩光栅(PCG),研究PCG制作工艺过程中光栅表面引入非金属或者金属污染物这一突出问题,以扫描电镜显微镜和X射线光电子能谱为主要分析手段,定性和定量的判断PCG表面的污染物残留状态。为去除光栅表面污染物,系统开展PCG清洗研究,包括湿法清洗、干法清洗、超声辅助等。利用中国工程物理研究院八所的阈值测试平台和中科院上海光机所的阈值测试装置,进行了PCG的皮秒阂值状态确认,得到了优化的PCG清洗工艺,元件达到工程指标要求并成功应用于激光装置。在PCG清洗方面取得如下一系列重要成果。
1.对PCG湿法清洗和清洗安全进行研究。系统研究了SPM(浓硫酸和双氧水混合液)的清洗温度、组成成份、清洗时间、清洗遍数等主要参数,得到优化的SPM清洗方案；研究了不同浓度的DHF(稀释氢氟酸)对二氧化铪和二氧化硅的腐蚀特性,得到去除现行工艺PCG表面二氧化铪薄层的有效方法；研究了洗铬液对PCG顶层铬掩模去除特性,解决了洗铬液残留的铈二次污染问题,得到了理想的去除铬掩模工艺方案；研究了PCG湿法清洗安全问题,综合分析PCG湿法清洗损伤原因,发现多层膜表面节瘤是导致含双氧水清洗液清洗损伤的直接原因,并对多层膜节瘤缺陷的控制提出更高的要求；系统研究了不同频率的超声辅助清洗,得到超声辅助的有效性及不同频率下对PCG的清洗安全性,提出了兆赫兹超声辅助湿法清洗PCG的需求。
2.研究了各种气体等离子体干法清洗、相关真空设备的污染情况及干湿法结合清洗。研究了氧气、氢气和四氟化碳气体等离子体对PCG的表面干法清洗,发现氧等离子体和氢等离子体能有效的去除碳氟化合物,且前者能快速去除刻蚀残留光刻胶,尤其是利用四氟化碳等离子体剥离PCG表面材料去除其上污染物的研究,实验显示这种方法可以有效去除嵌入表层的污染物和氧等离子体难于去除的污染物；研究了PCG制作工艺相关的真空设备污染情况,光栅制作工艺中的离子束刻蚀过程存在铁等元素的污染,等离子体清洗去除光刻胶过程存在铝和铜元素污染,分析其来源,引出干法清洗之后加入一步湿法清洗的必要性,并为后续真空设备设计提出改进意见；研究HPM(盐酸、双氧水和去离子水)清洗去除金属元素污染物,并结合氧等离子体清洗,发展了一种新的干湿法结合清洗PCG方案。
3.使用10ps脉宽、1053nm波长皮秒激光对不同清洗工艺下PCG的阈值进行状态确认,在优化的SPM基础上定型了PCG清洗工艺Ⅰ,在结合氧等离子体和HPM清洗基础上定型了PCG清洗工艺Ⅱ；皮秒阂值结果显示清洗工艺Ⅱ优于清洗工艺Ⅰ,在氧等离子体处理的基础上,HPM可以在更低温度更短时间内取得与传统SPM相当甚至更好的清洗效果,能显著提升脉宽压缩光栅表面抗皮秒损伤阈值至1.6J/cm2(光栅面),通量阈值为3.4J/cm2。
4.对常见材料构成的容器进行光栅保存实验。发现PP塑料暴露空气中受湿度和光照影响会发生老化现象,有可能污染PCG表面,所以对于塑料密封容器需要避光、避氧、干燥环境下保存样品。对于受塑料老化污染的样品,在使用之前需要做进一步清洗。
Rapid development of ultra-high power laser device is attributable to the chirped pulse amplification (CPA) technology, and the induced laser damage of multilayer dielectric film gratings (PCG) wich are core components in CPA system is key factor influence on the operation of high power laser systen stable and sustainable. A wide variety of PCG surface contaminants, such as organic photoresist, fluoro-hydrocarbon deposits, metals deposits, airborne organic, and particulate contamination and so on, are introduced during the process of manufacturing gratings. These residual contaminants which have great absorption coefficient from incidencing laser pulses can easily form heat-absorbing centers and further lead to physics damage to the PCG. Therefore, selection of appropriate and effective cleaning method process to remove the surface contaminants is an ideal way to improve the laser induced damage threshold of PCG.
The cleaning of surface contaminants that impact on the laser damage threshold of PCG is studied systematically in this paper. Complete physical and chemical surface analysis techniques of USTC (University of Science and Technology of China) can be carried out to qualitatively and quantitatively evaluate the cleanliness of PCG. The laser facility for laser damage test with picosecond pulses which has been built by CAEP (China Academy of Engineering Physics) and a similar test device which has been setting up by SIOM (Shanghai Institute of Optics and Fine Mechanics) both can be employed to evaluate the laser damage threshold. And a series significant achievements of PCG cleaning have been obtained.
(1) The system research of wet cleaning with different solutions has been made. The optimization of cleaning by SPM solution has been got in the experiment. The diluted hydrofluoric acid to remove the thin hafnium oxide film which exist the top layer of PCG has been explored. The ideal process which solves the problem of secondary contaminante from chromium-etching solution used to remove chromium mask of PCG has been obtained. The reason which lead to cleaning-damage by wet cleaning has been comprehensively analysised, and new demands relating to the pre-process of PCG manufacturing have been put forward. Safety and efficiency of different frequency of ultrasonic-assisted cleaning have been explored, and the suitable type of ultrasound for PCG cleaning has been gained.
(2) The dry cleaning of various gas-plasma has been researched. The high effectiveness of removing photoresist, fluorocarbon, and some particular contaminants has been gained by using corresponding gas-plasma cleaning. The source of metal contaminants from ion beam machine and photoresist-stripping device is analysised to direct improvements of the vacuum equipment design in future. The ability of HPM solution to remove metal contaminants of PCG surface has been explored, and a new cleaning method based on the HPM solution combined with oxygen plasma for PCG has been developed.
(3) Basing on evaluation of picosecond-laser threshold of different cleaning methods, cleaning process Ⅰ and Ⅱ of PCG have been confirmed. HPM solution of cleaning process Ⅱ, combined oxygen plasma cleaning, is operated at lower temperature and shorter time than the SPM solution of cleaning process I, and the damage threshold of cleaning process Ⅱ is equate to (or even better) cleaning process I.
(4) Storage condition of PCG of the laboratory of different functional areals of humidity, temperature and other environmental paramters has been studied. It found that PP plastic may contaminate the PCG surface when it is degraded by the humity and sun in the air. Therefore, PCG should be stored in sealing-container of glass materials. The samples polluted with the degradation of PP plastic should be further cleaning before use.
引文
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