CN107838117A - The processing method for substrate of improving laser damage threshold - Google Patents
The processing method for substrate of improving laser damage threshold Download PDFInfo
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- CN107838117A CN107838117A CN201710931656.9A CN201710931656A CN107838117A CN 107838117 A CN107838117 A CN 107838117A CN 201710931656 A CN201710931656 A CN 201710931656A CN 107838117 A CN107838117 A CN 107838117A
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- substrate
- minutes
- ultrasonic
- substrate surface
- deionized water
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
Using heat treatment and it is cleaned by ultrasonic the technology being combined, proposes a kind of processing method for substrate for lifting substrate surface and transmiting class thin-film component laser damage threshold.The impurity particle of substrate sub-surface is separated out to substrate surface using heat treatment technics, is then removed and is separated out to the impurity particle of substrate surface by ultrasonic cleaning technique.The present invention can increase adhesion of thin film while (Asia) surface impurity particle is removed, and lift substrate surface and transmit the laser damage threshold of class thin-film component.
Description
Technical field
The present invention relates to field of optical films, is a kind of processing method for substrate for improving laser damage threshold.
Background technology
Laser damage threshold is one of important parameter of optical thin film element performance, and can concern thin-film component in high power
Applications well is obtained in laser system.There are some researches show impurity defect is the root of induced laser damage：On the one hand, in laser
During irradiation, the local temperature at impurity defect is increased sharply, and damage from laser is produced under Thermal-mechanical Coupling effect；On the other hand, base
The impurity on piece (Asia) surface is in coating process because thermophoresis effect in substrate surface forms larger sized impurity particle and film
Coupling effect occurs for layer, causes the damage threshold of thin-film component to be far below the intrinsic damage threshold value of film, even below substrate table
The damage threshold in face.Therefore for coated element, the clean-up performance of substrate is the key for influenceing coated product quality
One of factor.High power laser system, as China's God Light equipment series, American National igniter (NIF), French LMJ devices,
The large-scale device of high power laser such as Japanese LFEX and GEKKO devices propose very high to the resisting laser damage performance of thin-film component
It is required that so that the cleaning of substrate must more strict and specification before plated film.Conventional substrate cleaning include organic solvent clean with
It is cleaned by ultrasonic：The former efficiency is low and is easily influenceed in the operating process of reality by operating personnel；The latter can remove substrate surface
Pollution, but can not effectively remove substrate process residual sub-surface impurity defect.National thin film technique is academic within 2015
Space technology physics Institute in Lanzhou delivers in seminar meeting paper (《Optical thin film substrate cleaning research》) propose
Ultrasonic wave+alkaline cleaning fluid cleaning, deionized water hydro-peening and rinsing, the method for the combination of nitrogen dried and clean, but this method
In used nitrogen dries up process, if nitrogen is of low quality, dirt can be also left on substrate.Even more important
It is that above processing mode is the removing to the pollution of substrate surface impurity, does not consider the influence of substrate sub-surface impurity particle.
The content of the invention
The technical problem to be solved in the present invention is to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of improving laser damage
The processing method for substrate of threshold value, the present invention can increase adhesion of thin film while (Asia) surface impurity particle is removed, carry
Rise substrate surface and transmit the laser damage threshold of class thin-film component.
The technical solution of the present invention
A kind of processing method for substrate for lifting substrate surface and transmiting class thin-film component laser damage threshold, its feature exist
In this method comprises the following steps：
1) substrate surface pollution is removed using ultrasonic cleaning method, concretely comprised the following steps：
1. deionized water sprays 3-30 minutes；2. alkali lye is cleaned by ultrasonic 3-10 minutes, supersonic frequency 40KHz, cleaning temperature
Spend for 60 DEG C；3. deionized water sprays, minute time 3-30, the cleaning agent of residual is rinsed；4. deionized water is cleaned by ultrasonic 3-10
Minute, supersonic frequency 40KHz, cleaning temperature is 60 DEG C；5. substrate is proposed from rinse bath；6. infrared baking in super-clean environment
Substrate more than 5 minutes.
2) impurity particle of substrate sub-surface is made to separate out to substrate surface using heat treatment：
Place the substrate in and be heat-treated in an oven, heat treatment temperature：200~800 DEG C (are not higher than for K9 glass
300℃)；Heat treatment time：2~8 hours；Heat-treating atmosphere：Atmospheric environment.After substrate naturally cools to room temperature in an oven
Take out substrate
3) removed and separated out to the foreign-matter contamination of substrate surface using ultrasonic cleaning method, concretely comprised the following steps：
1. deionized water sprays 5-30 minutes；2. alkali lye is cleaned by ultrasonic 3-10 minutes, supersonic frequency 40KHz, cleaning temperature
Spend for 60 DEG C；3. deionized water sprays, minute time 5-30, the cleaning agent of residual is rinsed；4. deionized water is cleaned by ultrasonic 3-10
Minute, supersonic frequency 40KHz, cleaning temperature is 60 DEG C；5. substrate is proposed from rinse bath；6. infrared baking in super-clean environment
Substrate more than 5 minutes.
Compared with prior art, technique effect of the invention is as follows：
1st, synthesis uses heat treatment technics and ultrasonic cleaning technique：Using heat treatment technics by the impurity of substrate sub-surface
Size separation goes out to substrate surface, and substrate (Asia) surface impurity particle is removed by ultrasonic cleaning technique.
2nd, can solve the problems, such as caused by substrate (Asia) surface impurity that Laser-induced damage threshold reduces, will not be to substrate
On the premise of producing chemical attack effect, increase adhesion of thin film while removing part sub-surface impurity particle, so as to carry
Rise substrate surface and transmit the laser damage threshold of class thin-film component.
3rd, method is simple and easy, has the characteristics of with strong points and efficiency high.It is adapted to cleaning to be used for large-scale high power laser light
The high-precision thin-film component substrate of system.
Brief description of the drawings
Fig. 1 is substrate surface AFM shape appearance figure, only at ultrasonic cleaning technique processing (left side) and the inventive method
Manage on (right side)
Fig. 2 is that only ultrasonic cleaning technique processing and the laser damage using the inventive method processing meron surface is respectively adopted
Hinder probability graph, optical maser wavelength is respectively 1064nm (left side) and 355nm (right side)
Fig. 3 is that only ultrasonic cleaning technique processing and the laser damage using coated element after the inventive method processing is respectively adopted
Hinder probability graph
Embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
Exemplified by size to be divided into the component of A, B, C, D tetra- is φ 50mm × 5mm K9 glass substrates, illustrate present invention use
In lifting substrate surface and the processing method for substrate of transmission class thin-film component laser damage threshold.Specific embodiment is as follows:
Embodiment 1
1st, A groups remove substrate surface pollution using the method for only ultrasonic cleaning technique processing, concretely comprise the following steps：
1. deionized water sprays 10 minutes；2. alkali lye is cleaned by ultrasonic 8 minutes, supersonic frequency 40KHz, cleaning temperature 60
℃；3. deionized water sprays, 10 minutes time, the cleaning agent of residual is rinsed；4. deionized water is cleaned by ultrasonic 8 minutes, supersonic frequency
Rate is 40KHz, and cleaning temperature is 60 DEG C；5. substrate is proposed from rinse bath；6. infrared baking substrate 25 minutes in super-clean environment.
2nd, B groups are concretely comprised the following steps using the inventive method processing substrate (Asia) surface contamination：
1) substrate surface pollution is removed using ultrasonic cleaning method, step is：1. deionized water sprays 10 minutes；2. alkali lye
It is cleaned by ultrasonic 8 minutes, supersonic frequency 40KHz, cleaning temperature is 60 DEG C；3. deionized water sprays, 10 minutes time, rinse residual
The cleaning agent stayed；4. deionized water is cleaned by ultrasonic 8 minutes, supersonic frequency 40KHz, cleaning temperature is 60 DEG C；5. from rinse bath
Middle proposition substrate；6. infrared baking substrate 25 minutes in super-clean environment.
2) impurity particle of substrate sub-surface is made to separate out to substrate surface using heat treatment：
Place the substrate in and be heat-treated in an oven, heat treatment temperature：220℃；Heat treatment time：8 hours；Heat treatment
Atmosphere：Atmospheric environment.Substrate is taken out after substrate naturally cools to room temperature in an oven.
3) remove to separate out to the foreign-matter contamination of substrate surface, step using ultrasonic cleaning method and be：1. deionized water is sprayed
Leaching 10 minutes；2. alkali lye is cleaned by ultrasonic 8 minutes, supersonic frequency 40KHz, cleaning temperature is 60 DEG C；3. deionized water sprays, when
Between 10 minutes, rinse the cleaning agent of residual；4. deionized water is cleaned by ultrasonic 8 minutes, supersonic frequency 40KHz, cleaning temperature is
60℃；5. substrate is proposed from rinse bath；6. infrared baking substrate 25 minutes in super-clean environment.
3rd, (A groups) after the processing of only ultrasonic cleaning technique is measured respectively using AFM and by the present invention
(B groups) substrate surface pattern after method processing.Fig. 1 is substrate surface AFM shape appearance figures, only ultrasonic cleaning technique processing (left side) and
The inventive method handles (right side).
4th, two groups of substrate surface damage threshold measurements of A, B are carried out：
Testing standard：ISO21254, pulse width：12ns, incident angle：0 °, separate unit rank number of sampling：20.Fig. 2 is
The damage from laser probability graph on meron surface, optical maser wavelength are handled and handled using the inventive method using only ultrasonic cleaning technique
Respectively 1064nm (left side) and 355nm (right side).
Embodiment 2
1st, the substrate C groups using the processing of only ultrasonic cleaning technique are obtained with reference to the step 1 in embodiment 1.
2nd, it is coated with film layer according to required design on C group substrates.
3rd, obtained with reference to the step 2 in embodiment 1 using the inventive method processing substrate D groups.
4th, it is coated with D group substrates and identical film layer in step 2.
5th, the performance test of two groups of coated elements of C, D is carried out：
1. element spectrum property is tested after plated film：Incident angle uses 56 °, measures p-component transmissivity>98%.
2. element Laser-induced damage threshold measures after plated film:Testing standard：ISO21254, test wavelength：1064nm, arteries and veins
Rush width：12ns, incident angle：56 °, separate unit rank number of sampling：20, polarization state：P-component.Fig. 3 is to use only to be cleaned by ultrasonic
The damage from laser probability graph of coated element after technical finesse and the inventive method processing.
Many experiments show：The present invention is separated out the impurity particle of substrate sub-surface to substrate table by heat treatment technics
Face, then effectively removed and separated out to the impurity particle of substrate surface by ultrasonic cleaning technique.The present invention is will not be to substrate
On the premise of producing chemical attack effect, can effectively solve Laser-induced damage threshold caused by substrate (Asia) surface impurity reduces
The problem of, while increase adhesion of thin film, lift substrate surface and transmit the laser damage threshold of class thin-film component.
Claims (4)
- A kind of 1. processing method for substrate for lifting substrate surface and transmiting class thin-film component laser damage threshold, it is characterised in that This method comprises the following steps:Step 1) removes substrate surface pollution using ultrasonic cleaning method, is specially：1. deionized water sprays 3-30 minutes；2. alkali lye is cleaned by ultrasonic 3-10 minutes, supersonic frequency 40KHz；3. deionized water Spray, minute time 3-30, rinse the cleaning agent of residual；4. deionized water is cleaned by ultrasonic 3-10 minutes, supersonic frequency is 40KHz；5. substrate is proposed from rinse bath；6. infrared baking substrate more than 5 minutes in super-clean environment；Step 2) makes the impurity particle of substrate sub-surface separate out to substrate surface using heat treatment technics：Place the substrate in and be heat-treated in an oven, heat treatment temperature：200~800 DEG C；Heat treatment time：2~8 hours；Heat Handle atmosphere：Atmospheric environment；Substrate is taken out after substrate naturally cools to room temperature in an oven；Step 3) is removed using ultrasonic cleaning method to be separated out to the foreign-matter contamination of substrate surface, is specially：1. deionized water sprays 5-30 minutes；2. alkali lye is cleaned by ultrasonic 3-10 minutes, supersonic frequency 40KHz；3. deionized water Spray, minute time 5-30, rinse the cleaning agent of residual；4. deionized water is cleaned by ultrasonic 3-10 minutes, supersonic frequency is 40KHz；5. substrate is proposed from rinse bath；6. infrared baking substrate more than 5 minutes in super-clean environment.
- 2. lifting substrate surface according to claim 1 and the Substrate treatment side for transmiting class thin-film component laser damage threshold Method, it is characterised in that described substrate is optical glass or crystal.
- 3. lifting substrate surface according to claim 1 and the Substrate treatment side for transmiting class thin-film component laser damage threshold Method, it is characterised in that be not higher than 300 DEG C for K9 glass heat treatment temperature.
- 4. lifting substrate surface according to claim 1 and the Substrate treatment side for transmiting class thin-film component laser damage threshold Method, it is characterised in that cleaning temperature is 60 DEG C in step 1) and step 3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710931656.9A CN107838117A (en) | 2017-10-09 | 2017-10-09 | The processing method for substrate of improving laser damage threshold |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710931656.9A CN107838117A (en) | 2017-10-09 | 2017-10-09 | The processing method for substrate of improving laser damage threshold |
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| CN107838117A true CN107838117A (en) | 2018-03-27 |
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| CN201710931656.9A Pending CN107838117A (en) | 2017-10-09 | 2017-10-09 | The processing method for substrate of improving laser damage threshold |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111424317A (en) * | 2020-04-13 | 2020-07-17 | 电子科技大学 | Preparation method of single crystal garnet film with high laser-induced damage threshold |
| CN113248121A (en) * | 2021-06-18 | 2021-08-13 | 中国工程物理研究院激光聚变研究中心 | Post-processing method for improving damage threshold of fused quartz component |
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| CN105195487A (en) * | 2015-08-04 | 2015-12-30 | 航天科工惯性技术有限公司 | Quartz glass cleaning method |
| CN105925935A (en) * | 2016-05-17 | 2016-09-07 | 苏州市康普来表面处理科技有限公司 | Physical vapor deposition technology applied to communication system assembly for replacing water electroplating |
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Patent Citations (5)
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| JP2015023069A (en) * | 2013-07-17 | 2015-02-02 | 株式会社Ｓｃｒｅｅｎホールディングス | Substrate cleaning apparatus and substrate cleaning method |
| CN103639149A (en) * | 2013-12-09 | 2014-03-19 | 山东百利通亚陶科技有限公司 | Method for cleaning wafer |
| CN103885099A (en) * | 2014-02-13 | 2014-06-25 | 同济大学 | Transmission optical component damage threshold improvement method based on multi-iteration etching |
| CN105195487A (en) * | 2015-08-04 | 2015-12-30 | 航天科工惯性技术有限公司 | Quartz glass cleaning method |
| CN105925935A (en) * | 2016-05-17 | 2016-09-07 | 苏州市康普来表面处理科技有限公司 | Physical vapor deposition technology applied to communication system assembly for replacing water electroplating |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111424317A (en) * | 2020-04-13 | 2020-07-17 | 电子科技大学 | Preparation method of single crystal garnet film with high laser-induced damage threshold |
| CN111424317B (en) * | 2020-04-13 | 2021-08-06 | 电子科技大学 | Preparation method of single crystal garnet film with high laser-induced damage threshold |
| CN113248121A (en) * | 2021-06-18 | 2021-08-13 | 中国工程物理研究院激光聚变研究中心 | Post-processing method for improving damage threshold of fused quartz component |
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Application publication date: 20180327 |