CN102980844A - Method for detecting washed surface of optical substrate used for laser thin film element - Google Patents
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- 230000003287 optical effect Effects 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title claims abstract description 11
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- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 6
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 6
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- 238000011158 quantitative evaluation Methods 0.000 abstract 1
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Abstract
本发明涉及一种激光薄膜用光学基板清洗后表面检测方法，属于光学技术领域。所述检测流程工艺包括以下步骤：运用5μm、10μm尺寸的人造氧化硅小球定标白光表面检测灯的可见度，对基板清洗后的残留颗粒运用5μm～50μm尺寸的氧化硅小球进行尺度对比，统计残留颗粒的尺度和数量，实现用肉眼对基板表面微米尺度颗粒的半定量化检测；使用弱吸收仪扫描基板表面，统计基板表面上吸收高于20ppm小于100ppm，以及吸收值大于100ppm的点数，依此实现对基板表面纳米尺度金属氧化物粉粒的清洗去除效率的精确评价；运用原子力显微镜测量基板表面划痕的深度、表面粗糙度，并测量记录直径超过20nm的麻点个数，实现对基板表面疵病的量化评测。本发明的优点在于所述检测方法实现对光学基板清洗后表面的定量化检测，为基板清洗工艺的改进提供数据支撑，保证基板镀膜后达到激光损伤方面的要求。
The invention relates to a method for detecting the surface of a laser thin film after cleaning an optical substrate, and belongs to the field of optical technology. The detection process includes the following steps: using 5 μm and 10 μm artificial silicon oxide balls to calibrate the visibility of the white light surface detection lamp, and using 5 μm to 50 μm silicon oxide balls for scale comparison on the residual particles after substrate cleaning, Count the size and quantity of residual particles to realize semi-quantitative detection of micron-scale particles on the substrate surface with the naked eye; use a weak absorption meter to scan the substrate surface, and count the number of points on the substrate surface whose absorption is higher than 20ppm but less than 100ppm, and the absorption value is greater than 100ppm. In this way, the precise evaluation of the cleaning and removal efficiency of nanoscale metal oxide particles on the substrate surface is realized; the atomic force microscope is used to measure the depth and surface roughness of the scratches on the substrate surface, and the number of pits with a diameter exceeding 20nm is measured and recorded, so as to realize the Quantitative evaluation of substrate surface defects. The advantage of the present invention is that the detection method realizes the quantitative detection of the surface of the optical substrate after cleaning, provides data support for the improvement of the substrate cleaning process, and ensures that the substrate meets the requirements of laser damage after coating.
Description
技术领域 technical field
本发明涉及一种光学基板清洗后的表面检测方法，特别涉及一种激光薄膜用光学基板清洗后表面检测方法。 The invention relates to a method for detecting the surface of an optical substrate after cleaning, in particular to a method for detecting the surface of a laser thin film after cleaning the optical substrate.
背景技术 Background technique
激光薄膜是高功率激光系统中的关键元件，是实现系统的光学性能的关键因素之一。薄膜又是激光系统中最易损伤的薄弱环节，薄膜损伤不仅降低激光的输出质量，而且容易导致系统中其它光学元件的损伤，从而给整个光学系统带来灾难性的破坏。影响薄膜损伤阈值的因素众多，从基板的加工和清洗，到膜系的设计和制备以及后续的激光预处理等。而基板清洗作为高功率激光薄膜制备的首要工序将直接决定元件的最终抗激光损伤能力。一般抛光后的基板表面污染物主要包括有机污染、固体颗粒污染、可溶性污染等。基片上的这些残留污染物将大幅度降低基底和薄膜界面对高功率激光的承受能力，并且在后续的薄膜镀制过程中残留物容易产生诸如节瘤这样的薄膜缺陷，在这些缺陷处激光与薄膜的相互作用会被放大，缺陷成为损伤的诱发源和短板。 Laser thin films are key components in high-power laser systems and one of the key factors to achieve the optical performance of the system. Thin film is the most vulnerable link in the laser system. Film damage not only reduces the output quality of the laser, but also easily causes damage to other optical components in the system, thus bringing catastrophic damage to the entire optical system. There are many factors that affect the damage threshold of the thin film, from the processing and cleaning of the substrate, to the design and preparation of the film system, and the subsequent laser pretreatment. As the first step in the preparation of high-power laser thin films, substrate cleaning will directly determine the ultimate resistance to laser damage of components. Generally, the surface pollutants of the polished substrate mainly include organic pollution, solid particle pollution, and soluble pollution. These residual pollutants on the substrate will greatly reduce the ability of the substrate and film interface to withstand high-power lasers, and the residues are prone to produce film defects such as nodules in the subsequent film plating process, where the laser and The interaction of the film will be amplified, and the defect will become the source of damage and the short board.
因此光学基板在镀膜前需要进行有效清洗，目前常用的清洗方法有擦拭法、RCA清洗法、超声波清洗法。这三种方法各有优劣，其中擦拭法对微米以上的大尺度颗粒比较有效，而难于去除纳米尺度的颗粒；RCA清洗属于化学清洗，能够降低颗粒与基板之间的吸附力，但是如果控制不当化学溶液的浓度则会引起基板的严重腐蚀，造成表面粗糙度的增加；超声波清洗通过频率的选择可以高效去除基板表面从微米到亚微米各种尺度的颗粒，然而当超声频率选择不当或者超声时间过长，则会产生划痕、麻点等，造成基板表面的物理损伤。 Therefore, the optical substrate needs to be effectively cleaned before coating. Currently, the commonly used cleaning methods include wiping method, RCA cleaning method, and ultrasonic cleaning method. These three methods have their own advantages and disadvantages. Among them, the wiping method is more effective for large-scale particles above microns, but it is difficult to remove nano-scale particles; RCA cleaning belongs to chemical cleaning, which can reduce the adsorption force between particles and substrates, but if controlled Improper concentration of chemical solution will cause severe corrosion of the substrate, resulting in an increase in surface roughness; ultrasonic cleaning can efficiently remove particles of various sizes from micron to submicron on the surface of the substrate through the selection of ultrasonic cleaning frequency. If the time is too long, scratches, pitting, etc. will occur, causing physical damage to the surface of the substrate.
那么如何获得能够将基板清洗干净而又对基板光滑表面损伤最小的清洗工艺，则需要对清洗后的基板表面情况有客观准确的检测判断方法。目前对于微米尺度颗粒，常用的检测方法是用100W的白光表面检测灯检验，然而这种方法无法定量颗粒度大小，并且检验的准确度取决于灯泡亮度，而在实际使用中灯泡的亮度又受很多外界因素影响，比如开机时间、灯泡总使用时间等，因此在使用中若要保证检验的准确性与一致性，就必须具备对表面检测灯校准的方法。此外基板表面还有尺寸诸如几十纳米尺度的金属氧化物颗粒，由于尺度很小，这些微粒虽然在表面检测灯下无法看到，但在激光辐照下极易造成基板的损伤，而对于基板表面这样的污染物目前还缺乏有效检测。除了上述基板污染物之外，清洗过程对基板会造成一定程度的损伤，产生表面划痕和麻点，这些表面疵病同样影响元件的损伤阈值，所以我们也需要对基板表面的疵病进行有效和准确的检测表征方法。 Then how to obtain a cleaning process that can clean the substrate and minimize damage to the smooth surface of the substrate requires an objective and accurate detection and judgment method for the surface condition of the substrate after cleaning. At present, for micron-scale particles, the commonly used detection method is to use a 100W white light surface detection lamp to inspect, but this method cannot quantify the particle size, and the accuracy of the inspection depends on the brightness of the bulb, and the brightness of the bulb is affected by the actual use. There are many external factors, such as the start-up time, the total use time of the bulb, etc. Therefore, in order to ensure the accuracy and consistency of the inspection during use, it is necessary to have a method for calibrating the surface inspection lamp. In addition, there are metal oxide particles with a size of tens of nanometers on the surface of the substrate. Although these particles cannot be seen under the surface inspection lamp due to their small size, they can easily cause damage to the substrate under laser irradiation. Such contaminants on surfaces currently lack effective detection. In addition to the above-mentioned substrate contamination, the cleaning process will cause a certain degree of damage to the substrate, resulting in surface scratches and pitting. These surface defects also affect the damage threshold of the component, so we also need to effectively detect the defects on the substrate surface. and accurate detection and characterization methods.
因此，本发明针对上述问题，提出一种激光薄膜元件用光学基板清洗后表面质量的检测方法，为光学基板的清洗工艺研发提供技术支持。 Therefore, in view of the above problems, the present invention proposes a method for detecting the surface quality of the laser thin film element after cleaning the optical substrate, so as to provide technical support for the research and development of the cleaning process of the optical substrate.
发明内容 Contents of the invention
本发明的目的是提出一种激光薄膜元件用光学基板清洗后表面检测方法。 The object of the invention is to propose a method for detecting the surface of a laser thin film element after cleaning an optical substrate.
本发明提出的激光薄膜元件用光学基板清洗后表面检测方法，具体步骤如下： The surface detection method of the laser thin film element proposed by the present invention is cleaned with an optical substrate, and the specific steps are as follows:
(1) 在表面洁净的熔石英光学基板上分别旋涂尺寸均一的直径为5μm、10μm氧化硅小球，使用白光表面检测灯观测涂有氧化硅小球的熔石英光学基板，确认检测者肉眼能够看到熔石英光学基板表面吸附的氧化硅小球，并能分辨小球的尺度大小，确认白光表面检测灯的可见度达到对微米尺度颗粒检测的标准，开始对清洗后熔石英光学基板表面进行残留颗粒的检测； (1) Spin-coat silicon oxide pellets with uniform diameters of 5 μm and 10 μm on fused silica optical substrates with a clean surface, respectively, and observe the fused silica optical substrates coated with silicon oxide pellets with a white light surface inspection lamp to confirm that the tester’s naked eyes Can see the silica pellets adsorbed on the surface of the fused silica optical substrate, and can distinguish the size of the pellets, confirm that the visibility of the white light surface detection lamp meets the detection standard for micron-scale particles, and start to clean the surface of the fused silica optical substrate Detection of residual particles;
（2）在熔石英光学基板检测过程中，当检测者观测到残留颗粒后，分别将此颗粒与标准片上的5～50μm尺度的标准氧化硅小球对比，获得该残留颗粒的尺度范围，统计熔石英光学基板表面的残留颗粒的数目以及尺度信息； (2) During the detection process of fused silica optical substrates, when the inspector observes the residual particles, the particles are compared with the standard silicon oxide balls on the standard plate with a scale of 5-50 μm to obtain the scale range of the residual particles, and statistics The number and size information of residual particles on the surface of the fused silica optical substrate;
(3)将清洗之后在白光表面检测灯下确认无可见颗粒的熔石英光学基板，使用弱吸收仪扫描测量基板表面弱吸收值，记录熔石英光学基板清洗后全表面的平均弱吸收值，统计整个熔石英光学基板表面上吸收高于20ppm小于100ppm的吸收点，以及大于100ppm的吸收点的个数，确认纳米尺度金属氧化物粉粒污染的清洗去除程度； (3) Confirm the fused silica optical substrate without visible particles under the white light surface detection lamp after cleaning, use a weak absorption meter to scan and measure the weak absorption value of the substrate surface, record the average weak absorption value of the entire surface of the fused silica optical substrate after cleaning, and make statistics The number of absorption points with absorption higher than 20ppm and less than 100ppm on the surface of the entire fused silica optical substrate, and the number of absorption points greater than 100ppm, confirms the degree of cleaning and removal of nanoscale metal oxide particle pollution;
(4) 对通过上述检测的清洗后熔石英光学基板作原子力显微镜检测,扫描尺寸为10μm，每个熔石英光学基板表面随机选择3～6个测试点，探测区域内划痕的深度，测量区域内熔石英光学基板表面的粗糙度，并测量记录直径超过20nm的凹坑个数。 (4) Perform atomic force microscope inspection on the cleaned fused silica optical substrate that has passed the above inspection, with a scanning size of 10 μm, randomly select 3 to 6 test points on the surface of each fused silica optical substrate, detect the depth of scratches in the area, and measure the area The surface roughness of the inner fused silica optical substrate is measured and the number of pits with a diameter exceeding 20nm is recorded.
本发明中，所述步骤（1）中白光表面检测灯的灯泡功率为80～150W。 In the present invention, the bulb power of the white light surface detection lamp in the step (1) is 80-150W. the
本发明中，所述步骤（2）中标准氧化硅小球尺寸为50μm，30μm，10μm或5μm中任一种；标准氧化硅小球的分布密度控制在10～20个/mm2。 In the present invention, the size of the standard silica spheres in the step (2) is any one of 50 μm, 30 μm, 10 μm or 5 μm; the distribution density of the standard silica spheres is controlled at 10-20 pieces/mm 2 .
本发明中，所述步骤（3）中弱吸收的分辨率为10-6 .。 In the present invention, the resolution of the weak absorption in the step (3) is 10 -6 .
本发明中，所述步骤（4）中原子力显微镜的纵向分辨率为0.1nm。 In the present invention, the longitudinal resolution of the atomic force microscope in the step (4) is 0.1 nm.
本发明的核心是运用尺寸均一的人造氧化硅微米小球实现了对白光表面检测灯的定标，达到用肉眼对表面微米尺度残留颗粒的半定量化检验，使用弱吸收测试仪检测纳米尺度的金属氧化物颗粒的去除效果，运用原子力显微镜检测基板清洗后表面划痕、粗糙度、麻点的变化，从而实现对光学基板的清洗效果的准确检测。 The core of the present invention is to use artificial silicon oxide micron balls with uniform size to realize the calibration of the white light surface detection lamp, to achieve the semi-quantitative inspection of the micron-scale residual particles on the surface with the naked eye, and to use the weak absorption tester to detect the nano-scale particles. For the removal effect of metal oxide particles, the atomic force microscope is used to detect the changes of scratches, roughness and pitting on the surface of the substrate after cleaning, so as to realize the accurate detection of the cleaning effect of the optical substrate.
本发明尤其实现光学基板表面检测的定量化，为基板清洗工艺的改进提供数据支撑，避免了基板内部和表面由于清洗过度而产生缺陷，保证基板具有高的损伤阈值，同时具有检测速度快、检测结果直观、检测精度高等优点。 In particular, the present invention realizes the quantitative detection of the surface of the optical substrate, provides data support for the improvement of the substrate cleaning process, avoids defects inside and on the surface of the substrate due to excessive cleaning, ensures that the substrate has a high damage threshold, and has fast detection speed, detection The results are intuitive and the detection accuracy is high.
附图说明 Description of drawings
图1：光学显微镜下10μm小球图像。 Figure 1: Image of a 10 μm sphere under an optical microscope.
图2：光学基板表面弱吸收图像。 Figure 2: Image of weak absorption on the surface of an optical substrate.
图3：光学基板表面划痕、麻点原子力显微镜图像。 Figure 3: AFM images of scratches and pits on the surface of optical substrates.
具体实施方式 Detailed ways
下面结合附图和实例对本发明作详细说明。 The present invention will be described in detail below in conjunction with the accompanying drawings and examples.
实施例1： Example 1:
以BK7光学基板清洗后的检测： Detection after cleaning with BK7 optical substrate:
在干净的φ30mm熔石英光学基板上分别旋涂尺寸均一10μm、5μm小球，小球的分布密度控制在10～20个/mm2，甩干后作为标准片。利用放大倍数为50倍的明场显微镜标定小球的尺寸与分布密度，如附图一所示。在开始对基板检测前，打开白光表面检测灯，5分钟预热后，使用10μm、5μm小球在检测灯下观测，确认能够看到基板表面吸附的小球，并能分辨二者的尺度大小，从而确认检测灯的可见度状态为正常，即可开始对清洗后光学基板的颗粒检测。 Spin-coat small balls with uniform size of 10 μm and 5 μm on a clean φ30 mm fused silica optical substrate, control the distribution density of the small balls at 10-20 pieces/mm 2 , and use it as a standard piece after drying. Use a bright-field microscope with a magnification of 50 times to calibrate the size and distribution density of the beads, as shown in Figure 1. Before starting to inspect the substrate, turn on the white light surface detection lamp, and after 5 minutes of warm-up, use 10 μm, 5 μm balls to observe under the detection lamp to confirm that the beads adsorbed on the substrate surface can be seen, and the scales of the two can be distinguished , so as to confirm that the visibility state of the detection lamp is normal, and the particle detection of the cleaned optical substrate can be started.
在基板检测过程中，当检测者观测到残留颗粒后，分别将此颗粒与标准片上的5至50μm尺度的标准氧化硅小球对比，从而获得该残留颗粒的尺度范围，并以此方法统计出基板表面的残留颗粒的数目以及尺度信息，若大于10μm的残留颗粒的数目超过10个，则需要提高清洗的力度。 During the substrate detection process, when the inspector observes the residual particles, they compare the particles with the standard silicon oxide balls on the standard sheet with a scale of 5 to 50 μm, so as to obtain the scale range of the residual particles, and use this method to calculate The number of residual particles on the surface of the substrate and the size information, if the number of residual particles larger than 10 μm exceeds 10, it is necessary to increase the cleaning intensity.
将清洗后在表面检测灯下观测确认无可见颗粒的光学基板，使用弱吸收仪测量基板表面弱吸收值，如附图二所示，确认基板清洗后平均弱吸收值低于20ppm，并且整个基板上高于20ppm小于100ppm的吸收点数小于5个，整个基板上不能有大于100ppm的点子，若不符合上述各吸收值则说明目前清洗方式对纳米尺度金属氧化物颗粒的去处力度还不够，需要增加清洗溶剂的浓度。 After cleaning, observe the optical substrate under the surface detection lamp to confirm that there are no visible particles, and use a weak absorption meter to measure the weak absorption value of the substrate surface, as shown in Figure 2, confirm that the average weak absorption value of the substrate after cleaning is lower than 20ppm, and the entire substrate The number of absorption points higher than 20ppm but less than 100ppm is less than 5, and there should be no more than 100ppm on the entire substrate. If the above absorption values do not meet the above-mentioned absorption values, it means that the current cleaning method is not strong enough to remove nanoscale metal oxide particles, and needs to be increased. The concentration of the cleaning solvent.
对清洗后基板作原子力显微镜检测，如附图三所示。扫描尺寸为10μm，每个样品表面随机选择3至6个以上点进行测试，若检测后测量区域内划痕的最大深度超过2nm，基板粗糙度为清洗前的两倍，直径超过20nm的麻点个数大于20个，则说明清洗力度过大，需要降低溶液酸碱度或者超声波超声时间。 An atomic force microscope inspection is performed on the cleaned substrate, as shown in Figure 3. The scanning size is 10 μm, and more than 3 to 6 points are randomly selected on the surface of each sample for testing. If the maximum depth of scratches in the measurement area exceeds 2 nm after detection, the roughness of the substrate is twice that of before cleaning, and pits with a diameter of more than 20 nm If the number is greater than 20, it means that the cleaning force is too high, and it is necessary to reduce the pH of the solution or the ultrasonic time.
用通过上述检测方法确认的清洗后基板制备1064nm高反射膜，并进行1064nm波长的激光损伤阈值测试，测试方式为1-on-1，测试结果表明元件的损伤阈值均高于30J/cm2。 A 1064nm high-reflection film was prepared with the cleaned substrate confirmed by the above detection method, and a laser damage threshold test with a wavelength of 1064nm was performed. The test method was 1-on-1. The test results showed that the damage threshold of the components was higher than 30J/cm 2 .
上述的对实施例的描述是为说明本发明的技术思想和特点，目的在于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施例，本领域技术人员根据本发明的揭示，对于本发明做出的改进和修改都涵盖在本发明的保护范围之内。 The above description of the embodiments is to illustrate the technical ideas and features of the present invention, and aims to enable those of ordinary skill in the technical field to understand and apply the present invention. It is obvious that those skilled in the art can easily make various modifications to these embodiments, and apply the general principles described here to other embodiments without creative efforts. Therefore, the present invention is not limited to the embodiments herein, and improvements and modifications made by those skilled in the art according to the disclosure of the present invention are covered within the protection scope of the present invention.
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