CN102980844B - Method for detecting washed surface of optical substrate used for laser thin film element - Google Patents
Method for detecting washed surface of optical substrate used for laser thin film element Download PDFInfo
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- CN102980844B CN102980844B CN201210526581.3A CN201210526581A CN102980844B CN 102980844 B CN102980844 B CN 102980844B CN 201210526581 A CN201210526581 A CN 201210526581A CN 102980844 B CN102980844 B CN 102980844B
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Abstract
The invention relates to a method for detecting the washed surface of an optical substrate used for a laser thin film element, belonging to the technical field of optics. A detection procedure process comprises the following steps of: calibrating the visibility of a white light surface detection lamp by using man-made silicon oxide globules of 5 microns and 10 microns in size; carrying out scale contrast on residual grains after the substrate is washed by using silicon oxide globules of 5 microns to 50 microns in size; counting the scale and the number of the residual grains, so as to realize the semi-quantitative detection on micrometer-scale grains on the surface of the substrate with the naked eye; scanning the surface of the substrate by using a weak absorption instrument; counting the number of points of which the absorption is larger than 20ppm and less than 100ppm and the absorption value is larger than 100ppm on the surface of the substrate, thereby realizing the precise evaluation on the washing and elimination efficiency of nano-scale metal oxide powder grains on the surface of the substrate; and measuring the depth and the surface roughness of the scratch on the surface of the substrate by using an atomic force microscope, measuring and recording the number of pocking marks of which the diameters are larger than 20nm, so as to realize the quantitative evaluation on the defects on the surface of the substrate. The method has the advantages that the quantitative detection on the washed surface of the optical substrate is realized, data support is provided for the improvement of the substrate washing process, and the requirements on laser damage after the substrate is plated with films are met.
Description
Technical field
The present invention relates to the surface inspecting method after a kind of optical substrate cleans, particularly optics base-plate cleaning rear surface detection method for a kind of laser film.
Background technology
Laser film is the key element in high power laser system, is one of the key factor that realizes the optical property of system.Film is again the weak link of easy damaged in laser system, and film damage not only reduces the output quality of laser, and easily causes the damage of other optical element in system, thereby gives the destruction of whole bringing on a disaster property of optical system.Affect the many factors of film damage threshold, from processing and the cleaning of substrate, to the design of film system and preparation and follow-up laser pre-treated etc.And the primary operation that base-plate cleaning is prepared as Laser Films will directly determine the final resisting laser damage ability of element.Substrate surface pollutant after general polishing mainly includes machine pollution, solid particle pollution, solubility pollution etc.On-chip these residual contaminants will significantly reduce substrate and the film interface ability to bear to high power laser light, and residue easily produces such as the such film defects of plethora in follow-up thin-film-coating process, interaction at these fault location laser and film can be exaggerated, and what defect became damage brings out source and short slab.
Therefore optical substrate needs effectively to clean before plated film, and conventional cleaning method has wipe method, RCA ablution, ultrasonic cleaning process at present.These three kinds of methods respectively have quality, and wherein wipe method is more effective to large scale particle more than micron, and are difficult to remove the particle of nanoscale; RCA cleans and belongs to chemical cleaning, can reduce the absorption affinity between particle and substrate, if still control the concentration of improper chemical solution, can cause the heavy corrosion of substrate, causes the increase of surfaceness; Ultrasonic Cleaning can efficiently be removed the particle of substrate surface various yardsticks from micron to sub-micron by the selection of frequency, yet when ultrasonic frequency selection is improper or ultrasonic time is long, can produce cut, pit etc., causes the physical damnification of substrate surface.
So how to obtain can be by base-plate cleaning totally and substrate smooth surface is damaged to minimum cleaning, needing has objective and accurate detection determination methods to the substrate surface situation after cleaning.At present for micrometer size granule, conventional detection method is to detect lamp check with the white light surface of 100W, yet this method is granularity size quantitatively, and bulb brightness is depended in the accuracy of check, and the brightness of bulb is affected by a lot of extraneous factors in actual use, such as on time, bulb total service time etc., if therefore in use will guarantee accuracy and the consistance of check, just must possess effects on surface and detect the method that lamp is calibrated.In addition substrate surface also has size such as the metal oxide particle of tens nanoscales, because yardstick is very little, although these particulates detect under lamp and cannot see on surface, but under laser irradiation, very easily cause the damage of substrate, and also lack effectively and detect at present for the such pollutant of substrate surface.Except aforesaid substrate pollutant, cleaning process can cause damage to a certain degree to substrate, produce surface scratch and pit, these beauty defects affect the damage threshold of element equally, so we also need the defect of substrate surface to carry out effectively and accurately detecting characterizing method.
Therefore, the present invention is directed to the problems referred to above, propose the detection method of optics base-plate cleaning rear surface quality for a kind of laser film element, for the cleaning of optical substrate, research and develop technical support is provided.
Summary of the invention
The object of the invention is to propose optics base-plate cleaning rear surface detection method for a kind of laser film element.
Optics base-plate cleaning rear surface detection method for the laser film element that the present invention proposes, concrete steps are as follows:
(1) on the fused quartz optical substrate of surface cleaning, the diameter of the homogeneous of spin coating size is respectively 5 μ m, 10 μ m monox beads, use white light surface to detect the fused quartz optical substrate that lamp observation scribbles monox bead, confirmation tester naked eyes can be seen the monox bead of fused quartz optical substrate adsorption, and can differentiate the scale size of bead, the visibility of confirming white light surface detection lamp reaches the standard that micrometer size granule is detected, and starts to carry out the detection of residual particles to cleaning rear fused quartz optical substrate surface;
(2) in fused quartz optical substrate testing process, when tester observes after residual particles, respectively by the standard oxygen SiClx bead contrast of 5～50 μ m yardsticks on this particle and standard film, obtain the range scale of this residual particles, number and the yardstick information of the residual particles on statistics fused quartz optical substrate surface;
(3) will after cleaning, under white light surface detection lamp, confirm the fused quartz optical substrate without visible particle, use the weak absorption value of weak absorption apparatus scanning survey substrate surface, record the average weak absorption value that fused quartz optical substrate cleans rear full surface, add up absorption on whole fused quartz optical substrate surface and higher than 20ppm, be less than the absorption point of 100ppm, and the number that is greater than the absorption point of 100ppm, confirm the cleaning removal degree that nanoscale metal oxide powder pollutes;
(4) fused quartz optical substrate after the cleaning by above-mentioned detection is detected as atomic force microscope, scan size is 10 μ m, 3～6 test points of each random selection in fused quartz optical substrate surface, the degree of depth of cut in search coverage, the roughness on fused quartz optical substrate surface in measured zone, and survey record diameter surpasses the pit number of 20nm.
In the present invention, in described step (1), the bulb power of white light surface detection lamp is 80～150W.
In the present invention, described step (2) Plays monox bead is of a size of 50 μ m, 30 μ m, in 10 μ m or 5 μ m any; The distribution density of standard oxygen SiClx bead is controlled at 10～20/mm
2.
In the present invention, in described step (3), the weak resolution absorbing is 10
-6 ..
In the present invention, the longitudinal frame of described step (4) Atom force microscope is 0.1nm.
Core of the present invention is the calibration that the artificial monox micron bead of utilization size homogeneous has been realized dialogue optical surface detection lamp, reach the with the naked eye semidefinite of effects on surface micro-meter scale residual particles and quantize check, use weak absorption tester to detect the removal effect of the metal oxide particle of nanoscale, use atomic force microscope to detect the variation of base-plate cleaning rear surface cut, roughness, pit, thereby realize the accurate detection to the cleaning performance of optical substrate.
The present invention especially realizes the quantification that optical substrate surface is detected, for the improvement of base-plate cleaning technique provides data supporting, avoided substrate inner and surperficial because overclean produces defect, guarantee that substrate has high damage threshold, have that detection speed is fast, testing result is directly perceived, accuracy of detection advantages of higher simultaneously.
Accompanying drawing explanation
Fig. 1: 10 μ m bead images under optical microscope.
Fig. 2: the weak absorption image in optical substrate surface.
Fig. 3: optical substrate surface scratch, pit atomic force microscope images.
Embodiment
Below in conjunction with accompanying drawing and example, the present invention is elaborated.
Embodiment 1:
Detection after cleaning with BK7 optical substrate:
Difference spin coating size homogeneous 10 μ m, 5 μ m beads on clean φ 30mm fused quartz optical substrate, the distribution density of bead is controlled at 10～20/mm
2, after drying as standard film.Utilizing enlargement factor is size and the distribution density of the light field microscope demarcation bead of 50 times, as shown in accompanying drawing one.Before starting substrate detection, turn on white light surface and detect lamp, after preheating in 5 minutes, use 10 μ m, 5 μ m beads to observe under detection lamp, confirmation can be seen the bead of substrate surface absorption, and can differentiate the two scale size, thereby the visibility state of confirming to detect lamp be normally, can start cleaning the particle detection of rear optical substrate.
In substrate testing process, when tester observes after residual particles, respectively by the standard oxygen SiClx bead contrast of 5 to 50 μ m yardsticks on this particle and standard film, thereby obtain the range scale of this residual particles, and with the method, count number and the yardstick information of the residual particles of substrate surface, if be greater than 10 μ m residual particles outnumber 10, need the dynamics of improve cleaning.
By detect observation under lamp after cleaning on surface, confirm the optical substrate without visible particle, use weak absorption apparatus to measure the weak absorption value of substrate surface, as shown in accompanying drawing two, after confirming base-plate cleaning, average weak absorption value is lower than 20ppm, and the absorption that is less than 100ppm higher than 20ppm on whole substrate is counted and is less than 5, on whole substrate, can not there is the idea that is greater than 100ppm, if meet above-mentioned each absorption value, do not illustrate that current cleaning way to the place to go dynamics of nanoscale metal oxide particle not enough, need to increase the concentration of cleaning solvent.
To cleaning metacoxal plate, do atomic force microscope detection, as shown in accompanying drawing three.Scan size is 10 μ m, each sample surfaces is random selects 3 to 6 above points to test, if in measured zone, the depth capacity of cut surpasses 2nm after detecting, substrate roughness is the twice before cleaning, the pit number that diameter surpasses 20nm is greater than 20, illustrate that cleaning force spends greatly, need to reduce solution acid alkalinity or ultrasonic echography time.
With the cleaning metacoxal plate of confirming by above-mentioned detection method, prepare 1064nm highly reflecting films, and carry out the laser damage threshold test of 1064nm wavelength, test mode is 1-on-1, and test result shows that the damage threshold of element is all higher than 30J/cm
2.
The above-mentioned description to embodiment is that object is that those skilled in the art can understand and apply the invention in order technological thought of the present invention and feature to be described.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, within the improvement of making for the present invention and modification are all encompassed in protection scope of the present invention.
Claims (5)
1. an optics base-plate cleaning rear surface detection method for laser film element, is characterized in that concrete steps are as follows:
(1) on the fused quartz optical substrate of surface cleaning, the diameter of the homogeneous of spin coating size is respectively 5 μ m, 10 μ m monox beads, use white light surface to detect the fused quartz optical substrate that lamp observation scribbles monox bead, confirmation tester naked eyes can be seen the monox bead of fused quartz optical substrate adsorption, and can differentiate the scale size of bead, the visibility of confirming white light surface detection lamp reaches the standard that micrometer size granule is detected, and starts to carry out the detection of residual particles to cleaning rear fused quartz optical substrate surface;
(2) in fused quartz optical substrate testing process, when tester observes after residual particles, respectively by the standard oxygen SiClx bead contrast of 5～50 μ m yardsticks on this particle and standard film, obtain the range scale of this residual particles, number and the yardstick information of the residual particles on statistics fused quartz optical substrate surface;
(3) will after cleaning, under white light surface detection lamp, confirm the fused quartz optical substrate without visible particle, use the weak absorption value of weak absorption apparatus scanning survey substrate surface, record the average weak absorption value that fused quartz optical substrate cleans rear full surface, add up absorption on whole fused quartz optical substrate surface and higher than 20ppm, be less than the absorption point of 100ppm, and the number that is greater than the absorption point of 100ppm, confirm the cleaning removal degree that nanoscale metal oxide powder pollutes;
(4) fused quartz optical substrate after the cleaning by above-mentioned detection is detected as atomic force microscope, scan size is 10 μ m, 3～6 test points of each random selection in fused quartz optical substrate surface, the degree of depth of cut in search coverage, the roughness on fused quartz optical substrate surface in measured zone, and survey record diameter surpasses the pit number of 20nm.
2. optics base-plate cleaning rear surface detection method for laser film element according to claim 1, is characterized in that: in described step (1), the bulb power of white light surface detection lamp is 80～150W.
3. optics base-plate cleaning rear surface detection method for laser film element according to claim 1, is characterized in that: described step (2) Plays monox bead is of a size of 50 μ m, 30 μ m, in 10 μ m or 5 μ m any; The distribution density of standard oxygen SiClx bead is controlled at 10～20/mm
2.
4. optics base-plate cleaning rear surface detection method for laser film element according to claim 1, is characterized in that: in described step (3), the resolution of weak absorption apparatus is 10
-6.
5. optics base-plate cleaning rear surface detection method for laser film element according to claim 1, is characterized in that: the longitudinal frame of described step (4) Atom force microscope is 0.1nm.
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| CN201210526581.3A CN102980844B (en) | 2012-12-10 | 2012-12-10 | Method for detecting washed surface of optical substrate used for laser thin film element |
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| CN201210526581.3A CN102980844B (en) | 2012-12-10 | 2012-12-10 | Method for detecting washed surface of optical substrate used for laser thin film element |
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| CN104316496B (en) * | 2014-11-05 | 2017-05-10 | 中国工程物理研究院激光聚变研究中心 | Grease pollutant monitoring device in high-power laser |
| CN105203503B (en) * | 2015-09-16 | 2017-12-26 | 同济大学 | A kind of Laser Films element ultra-smooth optical substrate surface inspecting method |
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| GB2326229A (en) * | 1997-06-13 | 1998-12-16 | Robert Jeffrey Geddes Carr | Detecting and analysing submicron particles |
| US8072597B2 (en) * | 2000-09-21 | 2011-12-06 | Hitachi, Ltd. | Method and its apparatus for inspecting particles or defects of a semiconductor device |
| WO2004025563A1 (en) * | 2002-09-12 | 2004-03-25 | Cyvera Corporation | Diffraction grating-based encoded micro-particles for multiplexed experiments |
| CN1298886C (en) * | 2004-09-28 | 2007-02-07 | 中国科学院上海光学精密机械研究所 | Film coating method for improving optical thin-film laser injure threshold |
| JP4755054B2 (en) * | 2006-09-01 | 2011-08-24 | 株式会社日立ハイテクノロジーズ | Surface inspection method and surface inspection apparatus |
| CN101955939B (en) * | 2009-04-28 | 2012-07-25 | 中国科学院化学研究所 | Aptamer for grouping different subtype non-small cell lung cancers and screening method thereof |
| CN102747328B (en) * | 2012-06-27 | 2014-01-29 | 同济大学 | Coating method capable of improving laser induced damage threshold of high-reflectivity film |
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