CN102179390A - Method for cleaning ultra-smooth surface - Google Patents
Method for cleaning ultra-smooth surface Download PDFInfo
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- CN102179390A CN102179390A CN2010105646286A CN201010564628A CN102179390A CN 102179390 A CN102179390 A CN 102179390A CN 2010105646286 A CN2010105646286 A CN 2010105646286A CN 201010564628 A CN201010564628 A CN 201010564628A CN 102179390 A CN102179390 A CN 102179390A
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- washing lotion
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Abstract
The invention discloses a method for cleaning an ultra-smooth surface. The method sequentially comprises the following steps of: performing ultrasonic cleaning on a substrate to be cleaned by using N-methylpyrrolidone cleansing solution, performing ultrasonic cleaning by using APG0810 cleansing solution, performing megasonic cleaning by using alcohol and acetone mixed cleansing solution, performing soak cleaning by using concentrated HNO3 and H2O2 mixed cleansing solution, performing megasonic cleaning by using pure water, dehydrating and drying by using a high-speed centrifugal machine, and cleaning any one or mixture of any two of oxygen, nitrogen, and argon by using a radio frequency plasma cleaner. By the method, particulate fouling of which the size is less than submicron on the ultra-smooth surface can be removed, so that the highly cleaning ultra-smooth surface can be obtained.
Description
Technical field
The present invention relates to a kind of smooth surface cleaning method, be applied to the cleaning of super-smooth surface adhesion of particles such as quartz glass, K9 glass.
Background technology
Along with the development of Ultraprecision Machining, the application of super-smooth surface is increasingly extensive, and is also more and more higher to the requirement of super-smooth surface.It is a very important operation in the manufacture process of semiconductor, microelectronic component and optical element that super-smooth surface cleans.Studies show that high-quality ultra-smooth substrate surface stains fine impurity can cause that device performance descends.Such as: on the optical base-substrate surface during residual submicron order impurity, to make substrate surface produce serious scattering, when this optical base-substrate was applied to superpower laser, these impurity not only can increase the absorption of optical element to laser, cause the loss of light, and can reduce laser damage threshold; In laser gyro was made, the crudy of super-smooth surface directly influenced the optical property of plated film back mirror and then influences the precision of gyro; When on the semi-conductor silicon chip surface, having the impurity of 0.2 μ m, will cause the fatefulue defective of chip.
The method that is applied to the substrate cleaning at present is a lot, scouring method, infusion method, microcorrosion method and ultrasonic method etc. are arranged, but these cleaning methods are because of the restriction of its cleansing power, can't remove impurity below the micron order from substrate surface, as dust, polishing powder and produce the polishing agent etc. of chemical reaction.Therefore, the surface that utilizes existing cleaning method to clean, the cleanliness factor requirement that has not reached the ultra-smooth substrate surface.
Summary of the invention
Can't remove the deficiency of the following impurity of micron order from substrate surface in order to overcome prior art, the invention provides a kind of super-smooth surface cleaning method, not only can reach the cleaning performance of existing cleaning method, and, can remove the following particle of submicron order in conjunction with after mega sonic wave cleaning machine and the plasma cleaner cleaning.
The technical solution adopted for the present invention to solve the technical problems may further comprise the steps:
(1) utilizes N-methyl pyrrolidone washing lotion that substrate to be cleaned is carried out ultrasonic wave (supersonic frequency 40KHz) and clean 15～35min, mainly remove the protective paint of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2～5 times;
(2) utilize that the pH value is 7～10, mass concentration is that 0.2%～0.8% APG0810 (C8～C10 APG) washing lotion is carried out ultrasonic wave (supersonic frequency 80KHz) to substrate and cleaned 10～25min, remove organic dirt of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2～5 times;
(3) (mixing the washing lotion volume ratio is alcohol: acetone 1: 1～1: 3) substrate is carried out million (frequency is 1MHz) and clean 5～10min, go on foot operation through changing over to down after the pure water rinsing 2～5 times to utilize alcohol acetone to mix washing lotion;
(4) under 70～75 ℃, utilize dense HNO
3With H
2O
2(mixing the washing lotion volume ratio is dense HNO to mix washing lotion
3: H
2O
2: H
2O=1: 1: 1～1: 1: 3) substrate is carried out soaking and washing 1～2h, remove residual polishing powder and the polishing fluid of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2～5 times;
(5) adopting pure water mega sonic wave (frequency is 1MHz) to clean 10～20min down at 90～100 ℃ finally washes substrate;
(6) (rotating speed is 2000～3000rpm) substrate to be dehydrated 5～10min to utilize supercentrifuge;
(7) using power is the radio frequency plasma cleaning machine of 50～180w, and purge gas is that any one or any two kinds mist in oxygen, nitrogen, the argon gas cleans 2～10min, removes the substrate surface residual particles.
The invention has the beneficial effects as follows: above-mentioned cleaning combines ultrasonic wave, mega sonic wave and the plasma cleaner of different frequency cleans workpiece, utilizes their different cleaning principles that the attachment of surface of the work is removed from big to small; In conjunction with various washing lotion grease, ion and the atom level particle of surface of the work are removed one by one simultaneously.In sum, this cleaning method can be removed the following particulate fouling of super-smooth surface submicron order, thereby obtains high clean super-smooth surface.
The present invention is further described below in conjunction with embodiment.
The specific embodiment
Example one, concrete cleaning process are as follows:
1, utilizes N-methyl pyrrolidone washing lotion to carry out ultrasonic wave (supersonic frequency 40KHz) and clean 15min, mainly remove the protective paint of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2 times;
2, pH=8, mass concentration are that 0.3% APG0810 (C8 ~ C10 APG) washing lotion is carried out ultrasonic wave (supersonic frequency 80KHz) and cleaned 10min, remove organic dirt of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2 times;
3, utilize the alcohol acetone of preparation in 1: 1 by volume to mix washing lotion and workpiece is carried out million (frequency is 1MHz) clean 5min, go on foot operation through changing over to down after the pure water rinsing 2 times;
4, under 70 ℃, utilize dense HNO
3With H
2O
2(volume ratio is dense HNO to mix washing lotion
3: H
2O
2: H
2O=1: 1: 1) carries out soaking and washing 1h, remove residual polishing powder and the polishing fluid of substrate surface, go on foot operation through changing over to down after the pure water rinsing 2 times;
5,90 ℃ of pure water mega sonic waves (frequency is 1MHz) clean 10min, and substrate is finally washed;
6, utilize the supercentrifuge of rotating speed, substrate is dehydrated 10min for 3000rpm;
7, use radio frequency (13.56MHz) plasma cleaner of power, utilize argon gas that substrate surface is cleaned 10min simultaneously, remove the nano-scale particle of remained on surface as 50w.
Cleaning performance is as follows:
To the detection of taking pictures of substrate surface before and after cleaning, can remove the submicron particles of substrate surface 95% by laser confocal microscope and super depth of field digit microscope after the cleaning.
Example two, concrete cleaning process are as follows:
1, utilizes N-methyl pyrrolidone washing lotion to carry out ultrasonic wave (supersonic frequency 40KHz) and clean 20min, mainly remove the protective paint of substrate surface, go on foot operation through changing over to down after the pure water rinsing 3 times;
2, pH=9, mass concentration are that 0.4% APG0810 (C8 ~ C10 APG) washing lotion is carried out ultrasonic wave (supersonic frequency 80KHz) and cleaned 15min, remove organic dirt of substrate surface, go on foot operation through changing over to down after the pure water rinsing 3 times;
3, utilizing is that the alcohol acetone of preparation in 1: 2 mixes washing lotion and workpiece is carried out million (frequency is 1MHz) cleans 15min by volume, goes on foot operation through changing over to down after the pure water rinsing 3 times;
4, under 72 ℃, utilize dense HNO
3With H
2O
2(volume ratio is dense HNO to mix washing lotion
3: H
2O
2: H
2O=1: 1: 1.5) carries out soaking and washing 1.5h, remove residual polishing powder and the polishing fluid of substrate surface, go on foot operation through changing over to down after the pure water rinsing 3 times;
5,95 ℃ of pure water mega sonic waves (frequency is 1MHz) clean 15min, and substrate is finally washed;
6, utilize the supercentrifuge of rotating speed, substrate is dehydrated 7min for 2500rpm;
7, use radio frequency (13.56MHz) plasma cleaner of power, utilize oxygen that substrate surface is cleaned 6min simultaneously, remove the nano-scale particle of remained on surface as 120w.
Cleaning performance is as follows:
To the detection of taking pictures of substrate surface before and after cleaning, can remove the submicron particles of substrate surface 98% by laser confocal microscope and super depth of field digit microscope after the cleaning.
Example three, concrete cleaning process are as follows:
1, utilizes N-methyl pyrrolidone washing lotion to carry out ultrasonic wave (supersonic frequency 40KHz) and clean 30min, mainly remove the protective paint of substrate surface, go on foot operation through changing over to down after the pure water rinsing 4 times;
2, pH=10, mass concentration are that 0.6% APG0810 (C8 ~ C10 APG) washing lotion is carried out ultrasonic wave (supersonic frequency 80KHz) and cleaned 20min, remove organic dirt of substrate surface, go on foot operation through changing over to down after the pure water rinsing 4 times;
3, utilizing is that the alcohol acetone of preparation in 1: 3 mixes washing lotion and workpiece is carried out million (frequency is 1MHz) cleans 20min by volume, goes on foot operation through changing over to down after the pure water rinsing 4 times;
4, under 75 ℃, utilize dense HNO
3With H
2O
2(volume ratio is dense HNO to mix washing lotion
3: H
2O
2: H
2O=1: 1: 3) carries out soaking and washing 2h, remove residual polishing powder and the polishing fluid of substrate surface, go on foot operation through changing over to down after the pure water rinsing 4 times;
5,100 ℃ of pure water mega sonic waves (frequency is 1MHz) clean 20min, and substrate is finally washed;
6, utilize the supercentrifuge of rotating speed, substrate is dehydrated 5min for 2000rpm;
7, use radio frequency (13.56MHz) plasma cleaner of power, utilize oxygen and argon gas mist that substrate surface is cleaned 2min simultaneously, remove the nano-scale particle of remained on surface as 180w.
Cleaning performance is as follows:
To the detection of taking pictures of substrate surface before and after cleaning, can remove the submicron particles of substrate surface 97% by laser confocal microscope and super depth of field digit microscope after the cleaning.
Claims (1)
1. a super-smooth surface cleaning method is characterized in that comprising the steps:
(1) utilizes N-methyl pyrrolidone washing lotion that the ultrasonic wave that substrate to be cleaned carries out supersonic frequency 40KHz is cleaned 15～35min, go on foot operation through changing over to down after the pure water rinsing 2～5 times;
(2) utilize that the pH value is 7～10, mass concentration is that 0.2%～0.8% APG0810 washing lotion is cleaned 10～25min to the ultrasonic wave that substrate carries out supersonic frequency 80KHz, goes on foot operation through changing over to down after the pure water rinsing 2～5 times;
(3) utilize volume ratio to be alcohol: 1: 1～1: 3 alcohol acetone of acetone mixes washing lotion, and substrate is carried out frequency is that 5～10min are cleaned in million of 1MHz, goes on foot operation through changing over to down after the pure water rinsing 2～5 times;
(4) under 70～75 ℃, utilizing volume ratio is dense HNO
3: H
2O
2: H
2O=1: 1: 1～1: 1: 3 dense HNO
3With H
2O
2Mix washing lotion substrate is carried out soaking and washing 1～2h, go on foot operation through changing over to down after the pure water rinsing 2～5 times;
(5) the pure water mega sonic wave that is 1MHz 90～100 ℃ of following employing frequencies cleans 10～20min to substrate;
(6) utilizing rotating speed is that the supercentrifuge of 2000～3000rpm dehydrates 5～10min to substrate;
(7) using power is the radio frequency plasma cleaning machine of 50～180w, and purge gas is that any one or any two kinds mist in oxygen, nitrogen, the argon gas cleans 2～10min.
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|---|---|---|---|
| CN 201010564628 CN102179390B (en) | 2010-11-25 | 2010-11-25 | Method for cleaning ultra-smooth surface |
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|---|---|---|---|
| CN 201010564628 CN102179390B (en) | 2010-11-25 | 2010-11-25 | Method for cleaning ultra-smooth surface |
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| CN102179390A true CN102179390A (en) | 2011-09-14 |
| CN102179390B CN102179390B (en) | 2013-05-08 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517594A (en) * | 2011-12-15 | 2012-06-27 | 西安北方捷瑞光电科技有限公司 | Method for cleaning cerium-based polishing solution residues |
| CN103191889A (en) * | 2012-01-06 | 2013-07-10 | 北方夜视技术股份有限公司 | Cleaning method for photocathode input window of low-light-level image intensifier |
| CN105170538A (en) * | 2015-08-03 | 2015-12-23 | 芜湖真空科技有限公司 | Surface cleaning method for LOW-E glass |
| CN105195465A (en) * | 2015-09-21 | 2015-12-30 | 同济大学 | Fully-automatic optical element cleaning device with ultrasonic-megasonic composite frequency |
| CN105251745A (en) * | 2015-10-09 | 2016-01-20 | 同济大学 | Cleaning method for optical elements after precise polishing |
| CN106216308A (en) * | 2016-08-08 | 2016-12-14 | 泉州市三星消防设备有限公司 | A kind of cleaning method of the optical element after polishing |
| CN109277359A (en) * | 2018-09-29 | 2019-01-29 | 中国电子科技集团公司第四十六研究所 | A kind of cleaning process of infrared lens germanium single crystal twin polishing piece |
| CN110711739A (en) * | 2019-09-29 | 2020-01-21 | 中国科学院长春光学精密机械与物理研究所 | CaF for deep ultraviolet2Method for cleaning optical substrate |
| CN113070273A (en) * | 2020-01-03 | 2021-07-06 | 中国科学院上海硅酸盐研究所 | Surface treatment method for improving laser damage threshold of calcium fluoride crystal optical element |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517594A (en) * | 2011-12-15 | 2012-06-27 | 西安北方捷瑞光电科技有限公司 | Method for cleaning cerium-based polishing solution residues |
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| CN103191889A (en) * | 2012-01-06 | 2013-07-10 | 北方夜视技术股份有限公司 | Cleaning method for photocathode input window of low-light-level image intensifier |
| CN103191889B (en) * | 2012-01-06 | 2015-08-26 | 北方夜视技术股份有限公司 | A kind of clean method for gleam image intensifier photocathode input window |
| CN105170538A (en) * | 2015-08-03 | 2015-12-23 | 芜湖真空科技有限公司 | Surface cleaning method for LOW-E glass |
| CN105195465B (en) * | 2015-09-21 | 2017-07-18 | 同济大学 | A kind of ultrasonic wave mega sonic wave combination frequency full-automatic optical element cleaning device |
| CN105195465A (en) * | 2015-09-21 | 2015-12-30 | 同济大学 | Fully-automatic optical element cleaning device with ultrasonic-megasonic composite frequency |
| CN105251745A (en) * | 2015-10-09 | 2016-01-20 | 同济大学 | Cleaning method for optical elements after precise polishing |
| CN105251745B (en) * | 2015-10-09 | 2017-05-24 | 同济大学 | Cleaning method for optical elements after precise polishing |
| CN106216308A (en) * | 2016-08-08 | 2016-12-14 | 泉州市三星消防设备有限公司 | A kind of cleaning method of the optical element after polishing |
| CN106216308B (en) * | 2016-08-08 | 2018-10-23 | 泉州市三星消防设备有限公司 | A kind of cleaning method of optical element after polishing |
| CN109277359A (en) * | 2018-09-29 | 2019-01-29 | 中国电子科技集团公司第四十六研究所 | A kind of cleaning process of infrared lens germanium single crystal twin polishing piece |
| CN109277359B (en) * | 2018-09-29 | 2021-08-31 | 中国电子科技集团公司第四十六研究所 | Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens |
| CN110711739A (en) * | 2019-09-29 | 2020-01-21 | 中国科学院长春光学精密机械与物理研究所 | CaF for deep ultraviolet2Method for cleaning optical substrate |
| CN113070273A (en) * | 2020-01-03 | 2021-07-06 | 中国科学院上海硅酸盐研究所 | Surface treatment method for improving laser damage threshold of calcium fluoride crystal optical element |
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