CN106903424B - A kind of post-processing approach that optical element mechanical property is improved based on laser blast wave - Google Patents
A kind of post-processing approach that optical element mechanical property is improved based on laser blast wave Download PDFInfo
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Abstract
本发明提供了一种基于激光冲击波提高光学元件力学性能的后处理方法,以未进行激光冲击波后处理时薄膜元件的力学特性R0、A0、B0、H0和抗激光损伤能力F0、G0为基准,分别获得E0、Em和ΔE对S次激光冲击波处理后样品力学性能RS、AS、BS、HS和抗激光损伤能力FS、GS的影响规律;根据力学性能和抗激光损伤能力的提升情况,对初始激光能量E0、能量递增梯度ΔE和最大激光能量Em进行优化,当薄膜元件力学性能和抗激光损伤能力不再提升,且满足实验样品的要求时,停止循环,完成薄膜元件力学性能后处理。本发明实现了对高功率光学薄膜元件力学性能的改善,解决了光学薄膜元件附着力、膜层结合力、残余应力等力学性能目前缺乏有效手段控制的难题。The present invention provides a post-processing method for improving the mechanical properties of optical elements based on laser shock waves. The mechanical properties R 0 , A 0 , B 0 , H 0 and the ability to resist laser damage F0, G0 as the benchmark, the effects of E 0 , E m and ΔE on the mechanical properties R S , A S , B S , HS and laser damage resistance F S , G S of samples after S laser shock wave treatment were respectively obtained; The improvement of performance and laser damage resistance, optimize the initial laser energy E 0 , energy incremental gradient ΔE and maximum laser energy E m , when the mechanical properties and laser damage resistance of the thin film element are no longer improved, and meet the requirements of the experimental sample When , the cycle is stopped, and the post-processing of the mechanical properties of the thin film element is completed. The invention realizes the improvement of the mechanical properties of the high-power optical thin-film element, and solves the problem that the mechanical properties of the optical thin-film element, such as adhesive force, film layer bonding force, and residual stress, currently lack effective means to control.
Description
技术领域technical field
本发明属于光学薄膜元件后处理技术领域,具体涉及一种利用激光冲击波技术提高光学薄膜元件力学性能的后处理方法。The invention belongs to the technical field of post-processing of optical thin-film elements, and in particular relates to a post-processing method for improving the mechanical properties of optical thin-film elements by using laser shock wave technology.
背景技术Background technique
现代高功率激光技术的发展,特别是大口径系统的发展,对光学薄膜元件性能提出了越来越苛刻的要求,要求其具有高光性精度、高力学性能、高损伤阈值和高精度面形控制,将直接影响到大口径精密光学系统的功能实现和系统长时间运行的稳定性。影响光学薄膜各方面性能的因素有很多,包括薄膜自身特性、薄膜制备工艺以及激光参数等。The development of modern high-power laser technology, especially the development of large-aperture systems, puts forward more and more stringent requirements on the performance of optical thin-film components, requiring them to have high optical precision, high mechanical properties, high damage threshold and high-precision surface shape control , will directly affect the function realization of the large-aperture precision optical system and the stability of the long-term operation of the system. There are many factors that affect the performance of optical thin films, including the characteristics of the thin film itself, the preparation process of the thin film, and the laser parameters.
光学薄膜元件由于其特殊的高、低折射率材料交替沉积在光学玻璃基底上的多层结构,特别是在高激光损伤阈值薄膜研究领域最常用的电子束蒸发镀制的光学薄膜元件,相比体材料,存在基底与膜层之间的附着力、膜层与膜层之间结合力较弱的问题。而如果薄膜元件由缺陷诱导产生的激光损伤伴随着膜层剥落,在后续激光脉冲辐照下,损伤会迅速生长,发生灾难性破坏,严重影响系统运行稳定性。同时,由于薄膜元件材料间的应变不匹配造成的残余应力和面形精度的影响,同样对元件的性能和系统稳定性有着巨大的影响,因此必须对薄膜残余应力进行严格的控制。现阶段纯粹依赖改进制备工艺、优化膜系设计、发展新型镀膜材料等手段改进薄膜上述力学性能的代价是高昂的,为了进一步提高薄膜元件的性能,国内外的研究人员提出了后处理技术。Due to its special multi-layer structure of high and low refractive index materials alternately deposited on the optical glass substrate, especially the most commonly used electron beam evaporation plating optical thin film components in the field of high laser damage threshold thin film research, compared with For bulk materials, there are problems of weak adhesion between the substrate and the film layer, and weak bonding between the film layer and the film layer. However, if the defect-induced laser damage of the thin-film component is accompanied by film peeling, the damage will grow rapidly under the subsequent laser pulse irradiation, resulting in catastrophic damage, which seriously affects the stability of the system operation. At the same time, due to the influence of residual stress and surface shape accuracy caused by the strain mismatch between the materials of the thin film element, it also has a huge impact on the performance of the element and the stability of the system, so the residual stress of the thin film must be strictly controlled. At this stage, the cost of improving the above-mentioned mechanical properties of the film purely by improving the preparation process, optimizing the design of the film system, and developing new coating materials is high. In order to further improve the performance of the film element, researchers at home and abroad have proposed post-processing technology.
各种后处理技术,采用不同的工艺参数、后处理方式,针对不同的膜系材料和结构,可以获得不同方面的薄膜性能改善。目前常用的后处理手段包括:离子后处理、热处理和激光预处理。离子后处理,是薄膜在制备完成后,采用低能离子对其进行轰击以清除薄膜表面原有或粘附的结合较弱的表面显微缺陷,提高薄膜损伤阈值。目前工艺最成熟,效果最佳的激光预处理是通过激光辐照去除多层介质膜中低阈值的节瘤缺陷来提高薄膜的抗激光损伤能力。热处理也就是退火,目前虽然主要应用在释放薄膜残余应力和改善面形等方面,但是可重复性差,对不同材料、不同镀膜参数、不同类型的薄膜元件需要的热处理工艺参数不同,改善程度同样不同,故实际应用中存在难以控制等问题。Various post-processing technologies, using different process parameters and post-processing methods, can obtain different aspects of film performance improvement for different film materials and structures. The commonly used post-treatment methods include: ion post-treatment, heat treatment and laser pre-treatment. Ion post-treatment is to bombard the film with low-energy ions after the film is prepared to remove the original or adhered weak surface microscopic defects on the film surface and improve the film damage threshold. At present, the most mature technology and the most effective laser pretreatment is to remove the low-threshold nodule defects in the multilayer dielectric film by laser irradiation to improve the laser damage resistance of the film. Heat treatment is also annealing. Although it is mainly used to release the residual stress of the film and improve the surface shape, the repeatability is poor. The heat treatment process parameters required for different materials, different coating parameters, and different types of thin film elements are different, and the degree of improvement is also different. , so there are problems such as difficulty in control in practical applications.
发明内容Contents of the invention
本发明针对上述现有技术的不足,提供了一种基于激光冲击波提高光学元件力学性能的后处理方法。The present invention aims at the deficiencies of the above-mentioned prior art, and provides a post-processing method for improving the mechanical properties of optical elements based on laser shock waves.
本发明是通过如下技术方案实现的:The present invention is achieved through the following technical solutions:
一种基于激光冲击波提高光学元件力学性能的后处理方法,包括如下步骤:A post-processing method for improving the mechanical properties of optical elements based on laser shock waves, comprising the following steps:
(1)采用电子束蒸发镀制一批光学薄膜元件;任意选取一个光学薄膜元件作为被测样品,测量被测样品的残余应力R0、膜层与基底的临界附着力A0、膜层临界界面结合力B0和硬度H0;(1) A batch of optical thin-film elements are prepared by electron beam evaporation; randomly select an optical thin-film element as the sample to be tested, and measure the residual stress R 0 of the tested sample, the critical adhesion A 0 of the film layer and the substrate, and the critical adhesion force of the film layer. Interface bonding force B 0 and hardness H 0 ;
(2)在被测样品上选择200个测试点,每20个测试点作为一个测试组;并选取10个不同的激光能量,作为10个测试组分别对应的激光能量,每个测试组内的所有测试点对应的激光能量相同;设定每个测试点的辐照脉冲数目均为N1,采用泵浦激光以选定的激光能量依次辐照被测样品上的测试点,并通过在线监控系统对准泵浦激光辐照被测样品的位置来检测损伤的发生和生长,获得被测样品在不同能量下的初始损伤几率和该脉冲数目下的损伤生长几率;并通过线性拟合的方式获得被测样品在辐照脉冲数目N1下的初始损伤阈值F01以及损伤生长阈值G01;(2) Select 200 test points on the sample to be tested, and every 20 test points are used as a test group; and 10 different laser energies are selected as the laser energies corresponding to the 10 test groups respectively. The laser energy corresponding to all test points is the same; the number of irradiation pulses for each test point is set to be N 1 , and the pump laser is used to irradiate the test points on the sample under test with the selected laser energy in sequence, and through online monitoring The system aligns the position where the pump laser irradiates the test sample to detect the occurrence and growth of damage, and obtains the initial damage probability of the test sample under different energies and the damage growth probability under the number of pulses; and through linear fitting Obtain the initial damage threshold F 01 and the damage growth threshold G 01 of the tested sample under the irradiation pulse number N 1 ;
(3)重新选取一个被测样品,将测试点的辐照脉冲数目改为Nk,Nk≠N1,按照步骤(2)的方法,获得被测样品在辐照脉冲数目Nk下的初始损伤阈值F0k和损伤生长阈值G0k;(3) Reselect a sample to be tested, change the number of irradiation pulses at the test point to N k , N k ≠ N 1 , and follow the method in step (2) to obtain the Initial lesion threshold F 0k and lesion growth threshold G 0k ;
(4)重复执行步骤(3),获得m个不同脉冲辐照数目下的初始损伤阈值F0和损伤生长阈值G0;其中,F0={F01,F02,F03……F0m},G0={G01,G02,G03……G0m},要求脉冲辐照数目m不小于激光重复频率的200倍;(4) Repeat step (3) to obtain the initial damage threshold F0 and damage growth threshold G0 under m different pulse irradiation numbers; where, F0={F 01 , F 02 , F 03 ... F 0m }, G0 ={G 01 , G 02 , G 03 ...G 0m }, the number m of pulse irradiation is required to be not less than 200 times of the laser repetition frequency;
⑸在步骤(1)中制作的一批光学薄膜元件中重新选取一组薄膜元件,在该组薄膜元件膜面粘贴吸收层;在吸收层的表面放置约束层,形成用于激光冲击波后处理的实验样品;(5) Reselect a group of thin film elements from a batch of optical thin film elements produced in step (1), and paste an absorbing layer on the film surface of the group of thin film elements; place a constrained layer on the surface of the absorbing layer to form a laser shock wave post-treatment experimental samples;
⑹将实验样品放置在电动平移台上,同时保证同一样品每次放置的位置都相同;使在线显微镜始终对准泵浦激光辐照实验样品的位置,用以实时检测后处理过程中实验样品、吸收层和约束层的状态;⑹ Place the experimental sample on the electric translation stage, and at the same time ensure that the position of the same sample is the same every time; make the online microscope always align with the position of the experimental sample irradiated by the pump laser for real-time detection of the experimental sample, The state of the absorbing and constraining layers;
⑺设定用于激光冲击波处理的泵浦激光器的初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,并固定光斑尺寸、搭接率及扫描区域;要求E0和Em小于激光冲击波作用时使薄膜元件不发生破坏的最大激光能量;并标记S为小于等于(Em-E0)/ΔE的最大整数;令i=1;(7) Set the initial incident laser energy E 0 , maximum incident laser energy E m and laser energy incremental gradient ΔE of the pump laser used for laser shock wave processing, and fix the spot size, overlapping ratio and scanning area; require E 0 and E m is less than the maximum laser energy that prevents damage to the thin film element when the laser shock wave acts; and mark S as the largest integer less than or equal to (E m -E 0 )/ΔE; let i=1;
⑻令实际入射激光能量E=E0+ΔE*i;(8) Let the actual incident laser energy E=E 0 +ΔE*i;
⑼采用光栅扫描方式对样品进行一次激光冲击波扫描处理,使得薄膜元件表面微结构发生变化;⑼Using the raster scanning method to scan the sample with a laser shock wave, the microstructure of the surface of the thin film element changes;
⑽去除薄膜样品表面残留的吸收层和约束层,并对薄膜样品进行喷淋和超声清洗,获得经过激光冲击波后处理的一组实验样品;⑽ Remove the residual absorbing layer and constrained layer on the surface of the film sample, and spray and ultrasonically clean the film sample to obtain a set of experimental samples after laser shock wave post-treatment;
⑾利用该组实验样品分别测量经冲击波后处理后的残余应力Ri、膜层与基底的临界附着力Ai、膜层临界界面结合力Bi和硬度Hi,并重复执行步骤⑵~⑷,获得激光冲击波后处理后m个不同脉冲辐照数目下的初始损伤阈值F0i和损伤生长阈值G0i;⑾ Use this group of experimental samples to measure the residual stress R i after the shock wave post-treatment, the critical adhesion force A i between the film layer and the substrate, the critical interface bonding force B i of the film layer, and the hardness H i , and repeat steps (2) to (4) , to obtain the initial damage threshold F0 i and damage growth threshold G0 i under m different pulse irradiation numbers after laser shock wave post-processing;
⑿令i=i+1;判断i是否小于等于S,若是,转入步骤(5),若否,进入步骤(13);⑿ Make i=i+1; judge whether i is less than or equal to S, if so, go to step (5), if not, go to step (13);
⒀通过被测样品相同区域在泵浦激光器不同能量下的辐照,完成了对该实验样品多个能量梯度的激光冲击波后处理,并获得了S次激光冲击波后处理后薄膜元件力学性能变化特性,包括残余应力R1~RS、临界附着力A1~AS、临界界面结合力B1~BS、硬度H1~HS和m个不同脉冲辐照数目下的初始损伤阈值F01~F0S和损伤生长阈值G01~G0S;⒀By irradiating the same area of the tested sample under different energies of the pump laser, the laser shock wave post-processing of the experimental sample with multiple energy gradients was completed, and the mechanical properties of the film element after S laser shock wave post-processing were obtained. , including residual stress R 1 ~ RS , critical adhesion force A 1 ~ AS , critical interfacial bonding force B 1 ~B S , hardness H 1 ~ HS and initial damage threshold F0 1 under m different pulse irradiation numbers ~F0 S and damage growth threshold G0 1 ~G0 S ;
⒁改变初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,重复步骤⑸~⒀;以未进行激光冲击波后处理时薄膜元件的力学特性R0、A0、B0、H0和抗激光损伤能力F0、G0为基准,分别获得E0、Em和ΔE对S次激光冲击波处理后样品力学性能RS、AS、BS、HS和抗激光损伤能力FS、GS的影响规律;根据力学性能和抗激光损伤能力的提升情况,对初始激光能量E0、能量递增梯度ΔE和最大激光能量Em进行优化,当薄膜元件力学性能和抗激光损伤能力不再提升,且满足实验样品的要求时,停止循环,完成薄膜元件力学性能后处理。⒁Change the initial incident laser energy E 0 , the maximum incident laser energy E m and the laser energy incremental gradient ΔE, and repeat steps ⑸ to ⒀; the mechanical properties of the film element R 0 , A 0 , B 0 , Based on H 0 and laser damage resistance F0 and G0, the mechanical properties R S , A S , B S , H S and laser damage resistance F S of samples after S laser shock wave treatment were obtained by E 0 , E m and ΔE, respectively. , G S ; according to the improvement of mechanical properties and laser damage resistance, the initial laser energy E 0 , energy incremental gradient ΔE and maximum laser energy E m are optimized. When the mechanical properties and laser damage resistance of thin film elements are not When it is raised again and meets the requirements of the experimental sample, the cycle is stopped to complete the post-processing of the mechanical properties of the thin film element.
本发明具有如下有益效果:The present invention has following beneficial effects:
1、本发明所述的后处理方法实现了对高功率光学薄膜元件力学性能的改善,结合实时在线调整后处理工艺参数,解决了光学薄膜元件附着力、膜层结合力、残余应力等力学性能目前缺乏有效手段控制的难题。本发明可以根据薄膜元件力学性能需求和评判标准,判断扫描次数和激光能量台阶等工艺参数,直至满足系统要求为止。1. The post-processing method of the present invention realizes the improvement of the mechanical properties of high-power optical thin-film elements, and combines the real-time online adjustment of post-processing process parameters to solve the mechanical properties of optical thin-film elements such as adhesion, film layer bonding force, and residual stress. At present, there is a lack of effective means to control the problem. The present invention can judge technological parameters such as scanning times and laser energy steps according to the mechanical performance requirements and evaluation criteria of the thin film element until the system requirements are met.
2、本发明所述的后处理方法对光学薄膜元件类型、材料、薄膜沉积参数没有限制,如减反膜、高反膜和偏振膜等均可兼容。2. The post-processing method described in the present invention has no limitation on the type, material, and film deposition parameters of the optical thin film element, such as anti-reflection film, high-reflection film and polarizing film, etc. are all compatible.
3、本发明所述的后处理方法不受光学元件尺寸限制,对大口径光学薄膜元件同样适用,这对大口径精密光学系统的功能实现和系统长时间运行的稳定性提供了保证,解决了光学系统向高能量、高精度方向发展的“瓶颈”之一。3. The post-processing method described in the present invention is not limited by the size of optical elements, and is also applicable to large-diameter optical film elements, which provides a guarantee for the function realization of large-diameter precision optical systems and the stability of the system for a long time, and solves the problem of One of the "bottlenecks" in the development of optical systems in the direction of high energy and high precision.
4、相比于传统的热处理方法存在只能改善光学薄膜元件力学性能中的残余应力问题,且存在可控性差、重复性低、不适用于大口径光学元件等问题,本发明所述的后处理方法精度大大提高,可控性和适用范围大大提升。4. Compared with the traditional heat treatment method, it can only improve the residual stress in the mechanical properties of optical thin film elements, and there are problems such as poor controllability, low repeatability, and unsuitability for large-diameter optical elements. The latter described in the present invention The precision of the processing method is greatly improved, and the controllability and scope of application are greatly improved.
5、本发明所述的后处理方法完成后,可以立刻在线检测,实时获得薄膜元件附着力、界面结合力、硬度、残余应力等力学信息,用于检测评估薄膜元件的力学性能是否达标。5. After the post-processing method of the present invention is completed, it can be detected online immediately, and the mechanical information such as adhesion force, interface bonding force, hardness, residual stress and the like of the thin film element can be obtained in real time, which is used to detect and evaluate whether the mechanical properties of the thin film element are up to standard.
6、本发明所述的后处理方法实现简单、可靠,适用性广泛。6. The post-processing method described in the present invention is simple, reliable and widely applicable.
具体实施方式Detailed ways
下面结合具体实施方式对本发明做进一步详细的说明。The present invention will be described in further detail below in combination with specific embodiments.
实施例1:Example 1:
一种基于激光冲击波提高光学元件力学性能的后处理方法,包括如下步骤:A post-processing method for improving the mechanical properties of optical elements based on laser shock waves, comprising the following steps:
⑴采用电子束蒸发镀制大小为φ50×5mm的1064nm高反膜,利用波面干涉仪获得样品残余应力R0,并利用纳米划痕仪测量样品膜层与基底的临界附着力A0,膜层临界界面结合力B0和硬度H0;(1) A 1064nm high-reflection film with a size of φ50×5mm is produced by electron beam evaporation, the residual stress R 0 of the sample is obtained by a wave surface interferometer, and the critical adhesion A 0 between the sample film and the substrate is measured by a nano-scratch instrument. Critical interfacial bonding force B 0 and hardness H 0 ;
(2)任意选取10个激光能量台阶Fj(j=1,2,…,10),每个激光能量台阶对应20个测试点,设定每个测试点的辐照脉冲数目N1,通过在线监控系统对准泵浦激光辐照被测样品的位置来检测损伤的发生和生长,从而获得损伤点数目与所有测试点数目的百分比,以及获得损伤生长点数目与所有测试点数目的百分比,即获得被测样品在不同能量下的初始损伤几率和该脉冲数目下的损伤生长几率;并通过线性拟合的方式获得被测样品在辐照脉冲数目N1下的初始损伤阈值F01以及损伤生长阈值G01;(2) Randomly select 10 laser energy steps F j (j=1, 2, ..., 10), each laser energy step corresponds to 20 test points, set the number of irradiation pulses N 1 for each test point, and pass The on-line monitoring system aims at the position where the pump laser irradiates the sample to detect the occurrence and growth of damage, so as to obtain the percentage of the number of damage points to the number of all test points, and the percentage of the number of damage growth points to the number of all test points, that is, to obtain The initial damage probability of the tested sample under different energies and the damage growth probability under the number of pulses; and the initial damage threshold F 01 and the damage growth threshold of the tested sample under the irradiation pulse number N 1 are obtained by linear fitting G 01 ;
(3)在步骤(1)中制作的一批光学薄膜元件中重新选取一个被测样品,将测试点的辐照脉冲数目改为Nk(Nk≠N1),按照步骤(2)的方法,获得被测样品在辐照脉冲数目Nk下的初始损伤阈值F0k和损伤生长阈值G0k;(3) Re-select a sample to be tested from a batch of optical thin film elements made in step (1), change the number of irradiation pulses at the test point to N k (N k ≠ N 1 ), follow the steps in (2) method, obtaining the initial damage threshold F 0k and the damage growth threshold G 0k of the tested sample under the irradiation pulse number N k ;
(4)重复执行步骤(3),获得m个不同脉冲辐照数目下的初始损伤阈值F0(F0={F01,F02,F03……F0m}和损伤生长阈值G0(G0={G01,G02,G03……G0m};要求脉冲辐照数目m不小于激光重复频率的200倍,例如重复频率为5Hz的话,测试的最大脉冲数目要不小于1000;(4) Repeat step (3) to obtain the initial damage threshold F0 (F0={F 01 , F 02 , F 03 ... F 0m } and damage growth threshold G0 (G0={ G 01 , G 02 , G 03 ... G 0m }; the number m of pulse irradiation is required to be not less than 200 times the laser repetition frequency, for example, if the repetition frequency is 5Hz, the maximum number of pulses to be tested should be not less than 1000;
⑸在步骤(1)中制作的一批光学薄膜元件中重新选取一组薄膜元件,在薄膜元件膜面粘贴吸收层,吸收层选用市场购买的以黑漆为材料的柔性贴膜,吸收层的厚度为120μm,吸收层厚度波动为8nm,面积覆盖整个样品表面;之后在吸收层的表面放置约束层,本实施例中选用去离子水为约束层,去离子水在吸收层表面上形成稳定的厚度为2.5mm的均匀水膜,形成激光冲击波后处理的实验样品;(5) Reselect a group of thin film elements from a batch of optical thin film elements produced in step (1), and paste an absorbing layer on the film surface of the thin film element. The absorbing layer is a flexible film made of black paint purchased in the market. The thickness of the absorbing layer is 120 μm, and the thickness fluctuation of the absorbing layer is 8nm, covering the entire sample surface; then a constraining layer is placed on the surface of the absorbing layer. In this embodiment, deionized water is selected as the constraining layer, and deionized water forms a stable thickness on the surface of the absorbing layer A uniform water film of 2.5 mm is used to form an experimental sample after laser shock wave treatment;
⑹将被测样品放置在电动平移台上,同时要保证同一样品每次放置的位置都相同,从而使得每次后处理的区域均相同,在线显微镜始终对准泵浦激光辐照被测样品的位置,用以实时检测后处理过程中被测样品、吸收层和约束层的状态;⑹ Place the sample to be tested on the electric translation stage, and at the same time, ensure that the position of the same sample is the same every time, so that the post-processing area is the same each time, and the online microscope is always aligned with the pump laser irradiating the sample to be tested. Position, used for real-time detection of the state of the measured sample, absorbing layer and constraining layer during post-processing;
⑺设定用于激光冲击波处理的泵浦激光器的初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,选用光斑尺寸为2mm、搭接率为90%、扫描区域大小为10×10mm,要求E0和Em小于激光冲击波作用时使薄膜元件不发生破坏的最大激光能量;并标记S为小于等于(Em-E0)/ΔE的最大整数;令i=1;⑺Set the initial incident laser energy E 0 , maximum incident laser energy E m and laser energy incremental gradient ΔE of the pump laser used for laser shock wave processing, choose the spot size as 2mm, the overlap rate as 90%, and the scanning area size as 10×10mm, E 0 and E m are required to be less than the maximum laser energy that prevents the film element from being damaged when the laser shock wave acts; and mark S as the largest integer less than or equal to (E m -E 0 )/ΔE; let i=1;
⑻令实际入射激光能量E=E0+ΔE*i;(8) Let the actual incident laser energy E=E 0 +ΔE*i;
⑼采用光栅扫描方式对样品进行一次激光冲击波扫描处理,使得薄膜元件表面微结构发生变化;⑼Using the raster scanning method to scan the sample with a laser shock wave, so that the microstructure of the surface of the thin film element changes;
⑽去除薄膜样品表面残留的吸收层和约束层,并对薄膜样品进行喷淋和超声清洗;⑽Remove the residual absorbing layer and constraining layer on the surface of the film sample, and spray and ultrasonically clean the film sample;
⑾经过激光冲击波后处理的薄膜样品,再次利用波面干涉仪获得样品残余应力Ri,利用纳米划痕仪测量样品膜层与基底的临界附着力Ai,膜层临界界面结合力Bi和硬度Hi,获得激光冲击波后处理后m个不同脉冲辐照数目下的初始损伤阈值F0i和损伤生长阈值G0i;⑾After the laser shock wave post-treatment of the thin film sample, the residual stress R i of the sample is obtained by the wave surface interferometer again, and the critical adhesion force A i between the sample film and the substrate, the critical interface bonding force B i and the hardness of the film layer are measured by a nano-scratch instrument H i , obtain the initial damage threshold F0 i and damage growth threshold G0 i under m different pulse irradiation numbers after laser shock wave post-processing;
⑿令i=i+1;判断i是否小于等于S,若是,转入步骤(5),若否,进入步骤(13);⑿ Make i=i+1; judge whether i is less than or equal to S, if so, go to step (5), if not, go to step (13);
⒀通过被测样品相同区域在泵浦激光器不同能量下的辐照,完成了对该实验样品多个能量梯度的激光冲击波后处理,并获得了S次激光冲击波后处理后薄膜元件力学性能变化特性,包括残余应力R1~RS、临界附着力A1~AS、临界界面结合力B1~BS、硬度H1~HS和m个不同脉冲辐照数目下的初始损伤阈值F01~F0S和损伤生长阈值G01~G0S;⒀By irradiating the same area of the tested sample under different energies of the pump laser, the laser shock wave post-processing of the experimental sample with multiple energy gradients was completed, and the mechanical properties of the film element after S laser shock wave post-processing were obtained. , including residual stress R 1 ~ RS , critical adhesion force A 1 ~ AS , critical interfacial bonding force B 1 ~B S , hardness H 1 ~ HS and initial damage threshold F0 1 under m different pulse irradiation numbers ~F0 S and damage growth threshold G0 1 ~G0 S ;
⒁改变初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,重复步骤⑸~⒀;以未进行激光冲击波后处理时薄膜元件的力学特性R0、A0、B0、H0和抗激光损伤能力F0、G0为基准,分别获得E0、Em和ΔE对S次激光冲击波处理后样品力学性能RS、AS、BS、HS和抗激光损伤能力FS、GS的影响规律;⒁Change the initial incident laser energy E 0 , the maximum incident laser energy E m and the laser energy incremental gradient ΔE, and repeat steps ⑸ to ⒀; the mechanical properties of the film element R 0 , A 0 , B 0 , Based on H 0 and laser damage resistance F0 and G0, the mechanical properties R S , A S , B S , H S and laser damage resistance F S of samples after S laser shock wave treatment were obtained by E 0 , E m and ΔE, respectively. , the influence law of G S ;
根据力学性能和抗激光损伤能力的提升情况,对初始激光能量E0、能量递增梯度ΔE和最大激光能量Em进行优化,当薄膜元件力学性能和抗激光损伤能力不再提升,且满足实验样品的要求时,停止循环,完成薄膜元件力学性能后处理;此时认为达到最佳激光冲击波后处理效果,对应的即为最优激光冲击波后处理工艺参数;所述最优激光冲击波后处理工艺,包括初始激光能量、能量递增梯度、最大激光能量和光斑搭接率等。According to the improvement of the mechanical properties and the ability to resist laser damage, the initial laser energy E 0 , the energy incremental gradient ΔE and the maximum laser energy E m are optimized. When the requirements are met, stop the cycle and complete the post-treatment of the mechanical properties of the thin film element; at this time, it is considered that the best laser shock wave post-treatment effect is reached, and the corresponding parameters are the optimal laser shock wave post-treatment process parameters; the optimal laser shock wave post-treatment process, Including initial laser energy, energy increasing gradient, maximum laser energy and spot overlapping rate, etc.
实施例2Example 2
一种基于激光冲击波提高光学元件力学性能的后处理方法,包括如下步骤:A post-processing method for improving the mechanical properties of optical elements based on laser shock waves, comprising the following steps:
⑴采用电子束蒸发镀制大小为φ30×3mm的532nm减反膜,利用波面干涉仪获得样品残余应力R0,并利用纳米划痕仪测量样品膜层与基底的临界附着力A0,膜层临界界面结合力B0和硬度H0;(2)任意选取10个激光能量台阶Fj(j=1,2,…,10),每个激光能量台阶对应20个测试点,设定每个测试点的辐照脉冲数目N1,通过在线监控系统对准泵浦激光辐照被测样品的位置来检测损伤的发生和生长,从而获得损伤点数目与所有测试点数目的百分比,以及获得损伤生长点数目与所有测试点数目的百分比,即获得被测样品在不同能量下的初始损伤几率和该脉冲数目下的损伤生长几率;并通过线性拟合的方式获得被测样品在辐照脉冲数目N1下的初始损伤阈值F01以及损伤生长阈值G01;⑴A 532nm anti-reflection coating with a size of φ30×3mm is produced by electron beam evaporation, and the residual stress R 0 of the sample is obtained by using a wave surface interferometer, and the critical adhesion A 0 between the sample film and the substrate is measured by a nano-scratch instrument. Critical interface bonding force B 0 and hardness H 0 ; (2) Randomly select 10 laser energy steps F j (j=1, 2,..., 10), each laser energy step corresponds to 20 test points, set each The number of irradiation pulses N 1 of the test point is used to detect the occurrence and growth of damage by aligning the position of the pump laser irradiating the sample under test with the online monitoring system, so as to obtain the percentage of the number of damage points to the number of all test points, and obtain the damage growth The percentage of the number of points to the number of all test points, that is, to obtain the initial damage probability of the tested sample under different energy and the damage growth probability under the pulse number; and obtain the tested sample at the irradiation pulse number N 1 by linear fitting Under the initial damage threshold F 01 and the damage growth threshold G 01 ;
(3)在步骤(1)中制作的一批光学薄膜元件中重新选取一个被测样品,将测试点的辐照脉冲数目改为Nk(Nk≠N1),按照步骤(2)的方法,获得被测样品在辐照脉冲数目Nk下的初始损伤阈值F0k和损伤生长阈值G0k;(3) Re-select a sample to be tested from a batch of optical thin film elements made in step (1), change the number of irradiation pulses at the test point to N k (N k ≠ N 1 ), follow the steps in (2) method, obtaining the initial damage threshold F 0k and the damage growth threshold G 0k of the tested sample under the irradiation pulse number N k ;
(4)重复执行步骤(3),获得m个不同脉冲辐照数目下的初始损伤阈值F0(F0={F01,F02,F03……F0m}和损伤生长阈值G0(G0={G01,G 02,G03……G0m};要求脉冲辐照数目m不小于激光重复频率的200倍,例如重复频率为5Hz的话,测试的最大脉冲数目要不小于1000;(4) Repeat step (3) to obtain the initial damage threshold F0 (F0={F 01 , F 02 , F 03 ... F 0m } and damage growth threshold G0 (G0={ G 01 , G 02 , G 03 ... G 0m }; the number m of pulse irradiation is required to be not less than 200 times the laser repetition frequency, for example, if the repetition frequency is 5Hz, the maximum number of pulses to be tested should be not less than 1000;
⑸在步骤(1)中制作的一批光学薄膜元件中重新选取一组薄膜元件,在薄膜元件膜面粘贴吸收层,吸收层选用市场购买的以黑漆为材料的柔性贴膜,吸收层的厚度为150μm,吸收层厚度波动为8nm,面积覆盖整个样品表面;之后在吸收层的表面放置约束层,本实施例中选用去离子水为约束层,去离子水在吸收层表面上形成稳定的厚度为3mm的均匀水膜,形成激光冲击波后处理的实验样品;(5) Reselect a group of thin film elements from a batch of optical thin film elements produced in step (1), and paste an absorbing layer on the film surface of the thin film element. The absorbing layer is a flexible film made of black paint purchased in the market. The thickness of the absorbing layer is 150 μm, and the thickness fluctuation of the absorbing layer is 8nm, and the area covers the entire sample surface; then, a constrained layer is placed on the surface of the absorbing layer. In this embodiment, deionized water is selected as the constraining layer, and the deionized water forms a stable thickness A uniform water film of 3mm forms an experimental sample after laser shock wave treatment;
⑹将被测样品放置在电动平移台上,同时要保证同一样品每次放置的位置都相同,从而使得每次后处理的区域均相同,在线显微镜始终对准泵浦激光辐照被测样品的位置,用以实时检测后处理过程中被测样品、吸收层和约束层的状态;⑹ Place the sample to be tested on the electric translation stage, and at the same time, ensure that the position of the same sample is the same every time, so that the post-processing area is the same each time, and the online microscope is always aligned with the pump laser irradiating the sample to be tested. Position, used for real-time detection of the state of the measured sample, absorbing layer and constraining layer during post-processing;
⑺设定用于激光冲击波处理的泵浦激光器的初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,选用光斑尺寸为1mm、搭接率为90%、扫描区域大小为10×10mm,要求E0和Em小于激光冲击波作用时使薄膜元件不发生破坏的最大激光能量;并标记S为小于等于(Em-E0)/ΔE的最大整数;令i=1;⑺Set the initial incident laser energy E 0 , maximum incident laser energy E m and laser energy incremental gradient ΔE of the pump laser used for laser shock wave processing, choose a spot size of 1mm, an overlap rate of 90%, and a scanning area size of 10×10mm, E 0 and E m are required to be less than the maximum laser energy that prevents the film element from being damaged when the laser shock wave acts; and mark S as the largest integer less than or equal to (E m -E 0 )/ΔE; let i=1;
⑻令实际入射激光能量E=E0+ΔE*i;(8) Let the actual incident laser energy E=E 0 +ΔE*i;
⑼采用光栅扫描方式对样品进行一次激光冲击波扫描处理,使得薄膜元件表面微结构发生变化;⑼Using the raster scanning method to scan the sample with a laser shock wave, the microstructure of the surface of the thin film element changes;
⑽去除薄膜样品表面残留的吸收层和约束层,并对薄膜样品进行喷淋和超声清洗;⑽Remove the residual absorbing layer and constraining layer on the surface of the film sample, and spray and ultrasonically clean the film sample;
⑾经过激光冲击波后处理的薄膜样品,再次利用波面干涉仪获得样品残余应力Ri,利用纳米划痕仪测量样品膜层与基底的临界附着力Ai,膜层临界界面结合力Bi和硬度Hi,并重复步骤⑵~⑷,获得激光冲击波后处理后m个不同脉冲辐照数目下的初始损伤阈值F0i和损伤生长阈值G0i;⑾After the laser shock wave post-treatment of the thin film sample, the residual stress R i of the sample is obtained by the wave surface interferometer again, and the critical adhesion force A i between the sample film and the substrate, the critical interface bonding force B i and the hardness of the film layer are measured by a nano-scratch instrument H i , and repeat steps (2) to (4) to obtain initial damage threshold F0 i and damage growth threshold G0 i under m different pulse irradiation numbers after laser shock wave post-treatment;
⑿令i=i+1;判断i是否小于等于S,若是,转入步骤(5),若否,进入步骤(13);⑿ Make i=i+1; judge whether i is less than or equal to S, if so, go to step (5), if not, go to step (13);
⒀通过被测样品相同区域在泵浦激光器不同能量下的辐照,完成了对该实验样品多个能量梯度的激光冲击波后处理,并获得了S次激光冲击波后处理后薄膜元件力学性能变化特性,包括残余应力R1~RS、临界附着力A1~AS、临界界面结合力B1~BS、硬度H1~HS和m个不同脉冲辐照数目下的初始损伤阈值F01~F0S和损伤生长阈值G01~G0S;⒀By irradiating the same area of the tested sample under different energies of the pump laser, the laser shock wave post-processing of the experimental sample with multiple energy gradients was completed, and the mechanical properties of the film element after S laser shock wave post-processing were obtained. , including residual stress R 1 ~ RS , critical adhesion force A 1 ~ AS , critical interfacial bonding force B 1 ~B S , hardness H 1 ~ HS and initial damage threshold F0 1 under m different pulse irradiation numbers ~F0 S and damage growth threshold G0 1 ~G0 S ;
⒁改变初始入射激光能量E0、最大入射激光能量Em和激光能量递增梯度ΔE,重复步骤⑸~⒀;以未进行激光冲击波后处理时薄膜元件的力学特性R0、A0、B0、H0和抗激光损伤能力F0、G0为基准,分别获得E0、Em和ΔE对S次激光冲击波处理后样品力学性能RS、AS、BS、HS和抗激光损伤能力FS、GS的影响规律;⒁Change the initial incident laser energy E 0 , the maximum incident laser energy E m and the laser energy incremental gradient ΔE, and repeat steps ⑸ to ⒀; the mechanical properties of the film element R 0 , A 0 , B 0 , Based on H 0 and laser damage resistance F0 and G0, the mechanical properties R S , A S , B S , H S and laser damage resistance F S of samples after S laser shock wave treatment were obtained by E 0 , E m and ΔE, respectively. , the influence law of G S ;
根据力学性能和抗激光损伤能力的提升情况,对初始激光能量E0、能量递增梯度ΔE和最大激光能量Em进行优化,当薄膜元件力学性能和抗激光损伤能力不再提升,且满足实验样品的要求时,停止循环,完成薄膜元件力学性能后处理;此时认为达到最佳激光冲击波后处理效果,对应的即为最优激光冲击波后处理工艺参数;所述最优激光冲击波后处理工艺,包括初始激光能量、能量递增梯度、最大激光能量和光斑搭接率等。According to the improvement of the mechanical properties and the ability to resist laser damage, the initial laser energy E 0 , the energy incremental gradient ΔE and the maximum laser energy E m are optimized. When the requirements are met, stop the cycle and complete the post-treatment of the mechanical properties of the thin film element; at this time, it is considered that the best laser shock wave post-treatment effect is reached, and the corresponding parameters are the optimal laser shock wave post-treatment process parameters; the optimal laser shock wave post-treatment process, Including initial laser energy, energy increasing gradient, maximum laser energy and spot overlapping rate, etc.
⒂改变镀膜参数(沉积速率、沉积温度等),重复步骤⑴~⒁,还可获得激光冲击波后处理对同一类型不同微结构的光学薄膜元件力学性能的提升规律。⒂Change the coating parameters (deposition rate, deposition temperature, etc.) and repeat the steps ⑴~⒁, and you can also obtain the improvement law of the mechanical properties of the same type of optical thin film elements with different microstructures after laser shock wave post-treatment.
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