CN101665910A - Method for cleaning SiO* substrate used in alloy films made by vacuum evaporation - Google Patents
Method for cleaning SiO* substrate used in alloy films made by vacuum evaporation Download PDFInfo
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- CN101665910A CN101665910A CN200810120429A CN200810120429A CN101665910A CN 101665910 A CN101665910 A CN 101665910A CN 200810120429 A CN200810120429 A CN 200810120429A CN 200810120429 A CN200810120429 A CN 200810120429A CN 101665910 A CN101665910 A CN 101665910A
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- substrate
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- cleaning
- deionized water
- ultrasonic wave
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- 239000000758 substrate Substances 0.000 title claims abstract description 46
- 238000004140 cleaning Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000956 alloy Substances 0.000 title claims abstract description 15
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 15
- 238000007738 vacuum evaporation Methods 0.000 title claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 238000005498 polishing Methods 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims description 10
- 230000002000 scavenging effect Effects 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- 238000009835 boiling Methods 0.000 abstract 2
- 238000007740 vapor deposition Methods 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 12
- 238000000151 deposition Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- -1 argon ion Chemical class 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to a method for cleaning a SiO* substrate used in alloy films made by vacuum vapor deposition. The cleaning method comprises the following steps: (1) polishing a substrate by polishing powder; (2) putting the polished substrate in cleaning solution of ammonia, hydrogen peroxide and deionized water in a ratio of 1-1.2:2-3:5-6, boiling the solution for 10 to 20 minutes and thenwashing the substrate by using deionized water; (3) putting the substrate in cleaning solution of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 1-1.2:2-3:8-10 in a container,boiling the solution for 10 to 12 minutes and then washing the substrate by deionized water; (4) putting the substrate in an ultrasonic cleaner to carry out ultrasonic polishing cleaning and non-ultrasonic polishing cleaning for 3 to 10 minutes by adopting deionized water as cleaning medium at normal temperature or 50 to 75 DEG C; (5) putting and drying the substrate in a nitrogen furnace for later use; and (6) bombarding the surface of the substrate for 5 to 10 minutes by an ion gun inside a vacuum chamber before vapor deposition. Thus, the SiO2 substrate cleaned in the way ensures that a prepared FeSiB film is uniform, stable and firm.
Description
Technical field
The invention belongs to the optical thin film preparing technical field, specifically is a kind of used in alloy films made by vacuum evaporation SiO
2Matrix cleaning method.
Technical background
At present, multilayer alloy firm (as: FeSiB, Cu, FeSiB multilayer film) with good giant magnetic effect is generally had an optimistic view of, and can produce far-reaching influence to sensing Study on Theory and applied research field to its reduction of production cost and the further research of giant magnetic effect feature.But the common fault for preparing this multilayer film at present is: ply adhesion is weak, compactness and lack of homogeneity, and this shortcoming shows especially obviously when vacuum evaporation especially.According to relevant reported in literature, the sputter coating method can be improved the weak problem of sticking power, but the sputter coating machine costs an arm and a leg, at present domestic enterprise or the research unit's overwhelming majority that has coating equipment all is to adopt vacuum vapour deposition (common vapour deposition method and electron beam evaporation plating method), so explore this kind multilayer film that utilizes the vacuum vapour deposition preparation can overcome above common fault very important meaning arranged.But, present ubiquity SiO during the evaporation alloy
2Problem such as substrate surface poor adhesive force, film forming are insecure, tracing it to its cause is SiO
2Substrate surface treatment does not reach requirement.
Summary of the invention
The object of the present invention is to provide a kind of can make the FeSiB film that makes evenly, stable, firm used in alloy films made by vacuum evaporation SiO
2Matrix cleaning method.
The technical scheme that realizes the object of the invention is such:
(1) substrate is polished with polishing powder from rare earth.
(2) substrate is positioned in glass or the quartz curette, adds proportioning and be: ammoniacal liquor: hydrogen peroxide: deionized water is 1～1.2: 2～3: 5～6 scavenging solution, be placed on the electric furnace heated and boiled 10～20 minutes, and rinse well with deionized water then.
(3) adding proportioning in cup is: hydrochloric acid: hydrogen peroxide: deionized water is 1～1.2: 2～3: 8～10 scavenging solution, boil equally after 10～12 minutes and rinse well with deionized water.
(4) substrate is put into the rinse bath of Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning 3～10 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean 3～5 minutes, unlatching ultrasonic wave, water temperature is controlled at 50 ℃～75 ℃, substrate is thrown moving the cleaning about 3～8 minutes, again substrate is thrown moving the cleaning 3～5 minutes after closing ultrasonic wave.Cleaning medium adopts deionized water.
(5) putting into nitrogen furnace dries stand-by.
(6) last cleaning is to carry out in vacuum chamber before the plating.With the surface that is placed on the ion gun bombardment substrate in the vacuum chamber 5～10 minutes.
Polishing powder in the described step (1) can be a cerium rouge.
Scavenging solution proportioning in the described step (2) can be ammoniacal liquor: hydrogen peroxide: deionized water is 1: 2～2.5: 5～6.
Scavenging solution proportioning in the described step (3) can be hydrochloric acid: hydrogen peroxide: deionized water is 1～1.2: 2～2.5: 8～10.
Described step (4) can be substrate to be put into the rinse bath of Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning 3～10 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean 3～5 minutes, unlatching ultrasonic wave, water temperature is controlled at 55 ℃～65 ℃, substrate is thrown moving the cleaning about 3～8 minutes, again substrate is thrown moving the cleaning 3～5 minutes after closing ultrasonic wave.Cleaning medium adopts deionized water.
Putting into the time that nitrogen furnace dries in the described step in (5) can be 10～20 minutes.
Used in alloy films made by vacuum evaporation SiO of the present invention
2Matrix cleaning method has solved SiO
2Problems such as the ubiquitous surface adhesion force of substrate is poor, film forming is insecure can make the FeSiB film that makes even, stable, firm.
Embodiment
Embodiment
Get used in alloy films made by vacuum evaporation SiO
2Substrate:
(1) substrate is polished with polishing powder, the polishing powder of polishing substrate should be used polishing powder from rare earth.Cerium rouge is used in suggestion, its fine size, and grinding force is strong, and polishing velocity is fast, good brightness and easy cleaning.Why cerium oxide is utmost point effective polishing compound, is because it can use decomposition and two kinds of forms of mechanical friction polishing substrate simultaneously.
(2) substrate is positioned in quartz or the glass cylinder, adding proportioning is: ammoniacal liquor: hydrogen peroxide: deionized water=1～1.2: 2～2.2: 5～6 scavenging solution, be placed on the electric furnace heated and boiled 10～20 minutes, rinse ammoniacal liquor then well with deionized water: hydrogen peroxide: the ratio of deionized water can be 1: 2: 5 or 1: 3: 6; Be placed on about the 15 minutes time of heated and boiled on the electric furnace, should not be less than 10 minutes, otherwise can impact effect.
(3) adding proportioning in cup is: hydrochloric acid: hydrogen peroxide: deionized water=1～1.2: 2～2.5: 8～10 scavenging solution, boil equally after 10～12 minutes and rinse hydrochloric acid with deionized water well: hydrogen peroxide: the ratio of deionized water can be 1: 2: 8 or 1: 3: 8; Be placed on about the 15 minutes time of heated and boiled on the electric furnace, should not be less than 10 minutes (with (2)).
(4) substrate is put into the rinse bath of Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning 3～10 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean 3～5 minutes, unlatching ultrasonic wave, water temperature is controlled at 50 ℃～75 ℃, substrate is thrown moving the cleaning about 3～8 minutes, again substrate is thrown moving the cleaning 3～5 minutes after closing ultrasonic wave.Cleaning medium adopts deionized water glass to be put into the rinse bath of Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning about 5 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean about 5 minutes, unlatching ultrasonic wave, water temperature is controlled at about 60 ℃, substrate is thrown moving the cleaning about 5 minutes, close after the ultrasonic wave again to glass throw moving clean about 5 minutes, still keep about 60 ℃ of water temperatures, substrate is by drawing lifting gear to draw slowly slowly, and the time of drawing lifting slowly is about 5 minutes.
(5) it is stand-by to put into nitrogen furnace oven dry, and the time of oven dry is about 10 minutes.
(6) last cleaning is to carry out in vacuum chamber before the plating.With the surface that is placed on the ion gun bombardment substrate in the vacuum chamber 5～10 minutes, what pay special attention to was substrate to be put in the process in the vacuum chamber will avoid koniology and rubbish to be attached on lens surface again.Surface (using argon ion) with being placed on the ion gun bombardment substrate in the vacuum chamber makes the foreign matter of glass substrate surface absorption produce desorption or decomposition, is taken away by vacuum pump at last, reaches the cleaning purpose.
Claims (6)
1, a kind of used in alloy films made by vacuum evaporation SiO
2Matrix cleaning method is characterized in that comprising following operation and step:
(1) substrate is polished with polishing powder from rare earth;
(2) substrate is positioned in the container and adds proportioning and be: ammoniacal liquor: hydrogen peroxide: deionized water is 1～1.2: 2～3: 5～6 scavenging solution, and heated and boiled 10～20 minutes is rinsed well with deionized water then;
(3) place container adding proportioning to be again: hydrochloric acid: hydrogen peroxide: deionized water is 1～1.2: 2～3: 8～10 scavenging solution, boil equally after 10～12 minutes and rinse well with deionized water;
(4) substrate is put into the rinse bath of Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning 3～10 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean 3～5 minutes, unlatching ultrasonic wave, water temperature is controlled at 50 ℃～75 ℃, substrate is thrown moving the cleaning about 3～8 minutes, again substrate is thrown moving the cleaning 3～5 minutes after closing ultrasonic wave.Cleaning medium adopts deionized water;
(5) putting into nitrogen furnace dries stand-by;
(6) before the evaporation in vacuum chamber, with the surface of ion gun bombardment substrate 5～10 minutes.
2, used in alloy films made by vacuum evaporation SiO as claimed in claim 1
2Matrix cleaning method is characterized in that: the polishing powder in the step (1) is a cerium rouge.
3, used in alloy films made by vacuum evaporation SiO as claimed in claim 1 or 2
2Matrix cleaning method is characterized in that: the scavenging solution proportioning in the step (2) is an ammoniacal liquor: hydrogen peroxide: deionized water is 1: 2～2.5: 5～6.
4, used in alloy films made by vacuum evaporation SiO as claimed in claim 3
2Matrix cleaning method is characterized in that: the scavenging solution proportioning in the step (3) is a hydrochloric acid: hydrogen peroxide: deionized water is 1～1.2: 2～2.5: 8～10.
5, used in alloy films made by vacuum evaporation SiO as claimed in claim 4
2Matrix cleaning method, it is characterized in that: the rinse bath of in the step (4) substrate being put into Ultrasonic Cleaners, carrying out ultrasonic wave at normal temperatures throws moving cleaning 3～10 minutes, closes ultrasonic wave, under the normal temperature glass is continued to throw moving clean 3～5 minutes, unlatching ultrasonic wave, water temperature is controlled at 55 ℃～65 ℃, substrate is thrown moving the cleaning about 3～8 minutes, again substrate is thrown moving the cleaning 3～5 minutes after closing ultrasonic wave.Cleaning medium adopts deionized water.
6, used in alloy films made by vacuum evaporation SiO as claimed in claim 5
2Matrix cleaning method is characterized in that: putting into the time that nitrogen furnace dries in the step in (5) is 10～20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810120429A CN101665910A (en) | 2008-09-04 | 2008-09-04 | Method for cleaning SiO* substrate used in alloy films made by vacuum evaporation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810120429A CN101665910A (en) | 2008-09-04 | 2008-09-04 | Method for cleaning SiO* substrate used in alloy films made by vacuum evaporation |
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| Publication Number | Publication Date |
|---|---|
| CN101665910A true CN101665910A (en) | 2010-03-10 |
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|---|---|---|---|
| CN200810120429A Pending CN101665910A (en) | 2008-09-04 | 2008-09-04 | Method for cleaning SiO* substrate used in alloy films made by vacuum evaporation |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964067A (en) * | 2012-12-11 | 2013-03-13 | 天津耀皮工程玻璃有限公司 | SiO2 antireflection film for solar photovoltaic glass and preparation method thereof |
| CN102974565A (en) * | 2012-12-12 | 2013-03-20 | 天津中环领先材料技术有限公司 | Method for cleaning monocrystalline silicon polished wafer |
| 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 |
| CN104498887A (en) * | 2014-12-02 | 2015-04-08 | 中国航天科工集团第三研究院第八三五八研究所 | Method for preprocessing nodule defects of ultra-low-loss reflector coating substrate |
| CN105750266A (en) * | 2016-04-27 | 2016-07-13 | 芜湖真空科技有限公司 | ITO glass cleaning method |
| CN107686977A (en) * | 2017-09-01 | 2018-02-13 | 苏州云舒新材料科技有限公司 | A kind of preparation method of semiconductor molybdenum disulfide film material |
| CN108957599A (en) * | 2018-07-12 | 2018-12-07 | 贵州贵安新区众鑫捷创科技有限公司 | A kind of camera optical mirror slip slice process |
| CN109604244A (en) * | 2018-11-27 | 2019-04-12 | 上海申和热磁电子有限公司 | A kind of cleaning method of suitable ultra thin silicon wafers |
| CN111659665A (en) * | 2020-05-29 | 2020-09-15 | 徐州鑫晶半导体科技有限公司 | Silicon wafer cleaning method and silicon wafer cleaning equipment |
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2008
- 2008-09-04 CN CN200810120429A patent/CN101665910A/en active Pending
Cited By (11)
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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 |
| CN102964067A (en) * | 2012-12-11 | 2013-03-13 | 天津耀皮工程玻璃有限公司 | SiO2 antireflection film for solar photovoltaic glass and preparation method thereof |
| CN102964067B (en) * | 2012-12-11 | 2016-01-06 | 天津耀皮工程玻璃有限公司 | For the SiO of solar energy photovoltaic glass 2anti-reflection film and preparation method thereof |
| CN102974565A (en) * | 2012-12-12 | 2013-03-20 | 天津中环领先材料技术有限公司 | Method for cleaning monocrystalline silicon polished wafer |
| CN104498887A (en) * | 2014-12-02 | 2015-04-08 | 中国航天科工集团第三研究院第八三五八研究所 | Method for preprocessing nodule defects of ultra-low-loss reflector coating substrate |
| CN105750266A (en) * | 2016-04-27 | 2016-07-13 | 芜湖真空科技有限公司 | ITO glass cleaning method |
| CN107686977A (en) * | 2017-09-01 | 2018-02-13 | 苏州云舒新材料科技有限公司 | A kind of preparation method of semiconductor molybdenum disulfide film material |
| CN108957599A (en) * | 2018-07-12 | 2018-12-07 | 贵州贵安新区众鑫捷创科技有限公司 | A kind of camera optical mirror slip slice process |
| CN109604244A (en) * | 2018-11-27 | 2019-04-12 | 上海申和热磁电子有限公司 | A kind of cleaning method of suitable ultra thin silicon wafers |
| CN111659665A (en) * | 2020-05-29 | 2020-09-15 | 徐州鑫晶半导体科技有限公司 | Silicon wafer cleaning method and silicon wafer cleaning equipment |
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Application publication date: 20100310 |