CN105710066A - Method for removing polishing residual reagents of solar monocrystalline germanium slice - Google Patents
Method for removing polishing residual reagents of solar monocrystalline germanium slice Download PDFInfo
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- CN105710066A CN105710066A CN201610151254.2A CN201610151254A CN105710066A CN 105710066 A CN105710066 A CN 105710066A CN 201610151254 A CN201610151254 A CN 201610151254A CN 105710066 A CN105710066 A CN 105710066A
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- Prior art keywords
- germanium wafer
- abluent
- turnover box
- polishing
- medicament
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000005498 polishing Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910052732 germanium Inorganic materials 0.000 title abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 title abstract 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 19
- 238000012805 post-processing Methods 0.000 claims abstract description 7
- 230000007306 turnover Effects 0.000 claims description 36
- 239000003814 drug Substances 0.000 claims description 27
- 230000004087 circulation Effects 0.000 claims description 13
- 238000002161 passivation Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims 1
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 abstract description 12
- 239000003640 drug residue Substances 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 239000012459 cleaning agent Substances 0.000 abstract 7
- 238000011010 flushing procedure Methods 0.000 abstract 1
- 230000002045 lasting effect Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 8
- 230000017531 blood circulation Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a method for removing polishing residual reagents of a solar monocrystalline germanium slice. The method comprises the following steps: preparing a cleaning agent: dissolving oxalic acid into deionized water to prepare an oxalic acid cleaning agent with concentration being 0.05-0.15mol/L, adding 10-20 L of the cleaning agent into a cleaning tank with a liquor circulating system, and keeping circulating of the cleaning agent; preliminarily cleaning a polished surface of germanium wafer; cleaning a transfer box by use of the cleaning agent: soaking the transfer box containing the germanium wafer into the prepared cleaning agent, swinging the transfer box by 5-30 seconds in a direction parallel to the surface of the germanium wafer, and enabling the transfer box to stand for 5-30 seconds in the cleaning agent; and post-processing. According to the method provided by the invention, an oxalic acid dilute solution is introduced to react residual hypochlorite, and flushing is carried out, so that follow-up product badness caused by lasting corrosion of hypochlorite reagent residues to the polished surface of the germanium wafer is solved, the drug residue probability on the chemically and mechanically polished surface of the germanium wafer is greatly reduced, and the rejection rate/ reworking rate caused by reagent residues is reduced to 0.4% from 11.8%.
Description
Technical field
The invention belongs to germanium material processing technique field, be specifically related to a kind of method removing solar energy single germanium wafer polishing residual medicament.
Background technology
Germanium belongs to rare scattered rare metal, it is important semi-conducting material and strategic resource, possess many-sided special nature, have extensive and important application in fields such as quasiconductor, Aero-Space observing and controlling, nuclear physics detecting, fiber optic communication, infrared optics, solaode, chemical catalyst, biomedicines.
Solar energy single germanium wafer is mainly used as space flight GaAs photovoltaic cell substrate material, and it is prepared through processing such as section, grinding, chemically mechanical polishing, Cleaning and Passivation by the satisfactory germanium single crystal of electrical property and crystal defect.Due on single germanium wafer polished surface by crystalline film such as direct epitaxial growth GaAs, its polished surface quality directly influences epitaxial wafer and final photovoltaic cell quality.Current technique polished surface after chemically mechanical polishing will be made directly cleaning organics removal and granule, dispatch from the factory then through packaging after Passivation Treatment.Single germanium wafer CMP process polishing fluid adds the oxidant such as sodium hypochlorite or lithium hypochlorite to obtain the polished surface of high-quality, but these medicaments remain in polished silicon wafer on a small quantity by unavoidably having after polishing terminates, especially polish the Waffer edge and back that cannot be flushed to when terminating bottom sheet bath.Find that part germanium wafer medicament residual forms non-uniform corrosion the most at last at polished surface edge by long term production, affect the Cleaning and Passivation effect after germanium wafer polished surface, cause product quality fluctuation of dispatching from the factory.And do not see the solution for this problem about in single germanium wafer processing technique bibliographical information at present..
Summary of the invention
Goal of the invention: present invention aim at for the deficiencies in the prior art, it is provided that a kind of cleaning performance is good, and the method removing solar energy single germanium wafer polishing residual medicament that after cleaning, product quality is high, stability is high.
Technical scheme: a kind of method removing solar energy single germanium wafer polishing residual medicament of the present invention, comprises the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.05~0.15mol/L, and adds the above-mentioned abluent of 10~20L in the rinse bath with medicament blood circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to the germanium wafer burnishing surface deionized water rinsing in polishing disk, with vacuum WAND, germanium wafer is taken out from polishing disk afterwards, and be sequentially inserted into turnover box, and ensure that burnishing surface is in the same direction;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in step (1) rinse bath got ready, and swings turnover box 5~30S along the parallel direction on germanium wafer surface, after turnover box stood in overflow launder 5~30S;
(4) post processing: turnover box is taken out from rinse bath, tilt 5~50 ° clockwise, first to the polished surface of germanium wafer deionized water rinsing 5~50S, another mistake hour hands tilt 5~50 ° of non-polished surface deionized water rinsing 5~50S to germanium wafer, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
Preferably, described turnover box is 5~15 on chip.
Preferably, the abluent in described rinse bath system often cleans 50 germanium wafer emptying replacings once.
Preferably, the concentration of described oxalic acid abluent is 0.1mol/L.
Preferably, in step (4), the angle of inclination clockwise of turnover box is 15~30 °.
Preferably, in step (4), the angle of inclination counterclockwise of turnover box is 15~30 °.
Beneficial effect: in (1) method provided by the invention, the oxalic acid weak solution of introducing reproducibility is rinsed well after being reacted away by residual hypochlorite again, overcoming in tradition the shortcoming that only cannot rinse out hypochlorite residual with deionized water completely, solving hypochlorite medicament residual, that germanium wafer burnishing surface is continued corrode the subsequent product caused is bad;(2) for avoiding the product of residual oxalic acid and oxalic acid and hypochlorite to remain on germanium wafer, burnishing surface is caused damage, first uses deionized water rinsing burnishing surface, it is ensured that the cleaning of burnishing surface;Then non-burnishing surface is cleaned again, it is ensured that the overall cleaning of germanium wafer;When angle of inclination is 15~30 °, cleaning effect is best;(3) use after the present invention, greatly reduce germanium wafer surface drug residual probability after chemically mechanical polishing, decrease and later process product quality is affected;(4) through statistics, use after the present invention removes polished silicon wafer process, because of medicament residual cause scrap/rework rate has been reduced to 0.4% by 11.8%, substantially increases yield rate and constant product quality.
Accompanying drawing explanation
Fig. 1 is the view not using present invention process wafer temperature;
Fig. 2 is the view using present invention process wafer temperature.
Detailed description of the invention
By the examples below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1: a kind of method removing solar energy single germanium wafer polishing residual medicament, comprises the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.1mol/L, and adds the above-mentioned abluent of 15L in the rinse bath with medicament blood circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to 4 germanium wafer burnishing surface deionized water rinsings in polishing disk, after with vacuum WAND, germanium wafer is taken out from polishing disk, and be sequentially inserted into turnover box, and ensureing that burnishing surface is in the same direction, dressing amount is 10;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in step (1) Overflow groove system got ready, and swings turnover box 20S along the parallel direction on germanium wafer surface, after turnover box stood in overflow launder 20S;
(4) post processing: turnover box is taken out from overflow launder, tilt 15 ° clockwise, polished surface deionized water rinsing 30S to germanium wafer, another mistake hour hands tilt 15 ° of non-polished surfaces to germanium wafer and wash away ionized water 30S, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
In treatment method, the abluent in described rinse bath system often cleans 50 germanium wafer emptying and changes once.
Embodiment 2: a kind of method removing solar energy single germanium wafer polishing residual medicament, comprises the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.05mol/L, and adds the above-mentioned abluent of 10L in the rinse bath with medicament blood circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to 4 germanium wafer burnishing surface deionized water rinsings in polishing disk, after with vacuum WAND, germanium wafer is taken out from polishing disk, and be sequentially inserted into turnover box, and ensureing that burnishing surface is in the same direction, dressing amount is 5;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in step (1) abluent got ready, and swings turnover box 5S along the parallel direction on germanium wafer surface, after turnover box stood in abluent 5S;
(4) post processing: turnover box is taken out from rinse bath, tilt 5 ° clockwise, first to the polished surface of germanium wafer deionized water rinsing 5S, another mistake hour hands tilt 5 ° of non-polished surfaces to germanium wafer and wash away ionized water 5S, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
In treatment method, the abluent in described rinse bath system often cleans 50 germanium wafer emptying and changes once.
Embodiment 3: a kind of method removing solar energy single germanium wafer polishing residual medicament, comprises the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.15mol/L, and adds the above-mentioned abluent of 20L in the rinse bath with medicament blood circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to 4 germanium wafer burnishing surface deionized water rinsings in polishing disk, after with vacuum WAND, germanium wafer is taken out from polishing disk, and be sequentially inserted into turnover box, and ensureing that burnishing surface is in the same direction, dressing amount is 15;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in step (1) abluent got ready, and swings turnover box 30S along the parallel direction on germanium wafer surface, after turnover box stood in rinse bath 30S;
(4) post processing: turnover box is taken out from rinse bath, tilt 50 ° clockwise, first to the polished surface of germanium wafer deionized water rinsing 50S, another mistake hour hands tilt 50 ° of non-polished surfaces to germanium wafer and wash away ionized water 50S, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
In treatment method, the abluent in described rinse bath system often cleans 50 germanium wafer emptying and changes once.
Embodiment 4: a kind of method removing solar energy single germanium wafer polishing residual medicament, comprises the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.1mol/L, and adds the above-mentioned abluent of 15L in the rinse bath with medicament blood circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to 4 germanium wafer burnishing surface deionized water rinsings in polishing disk, after with vacuum WAND, germanium wafer is taken out from polishing disk, and be sequentially inserted into turnover box, and ensureing that burnishing surface is in the same direction, dressing amount is 10;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in step (1) abluent got ready, and swings turnover box 20S along the parallel direction on germanium wafer surface, after turnover box stood in abluent 20S;
(4) post processing: turnover box is taken out from rinse bath, tilt 30 ° clockwise, first to the polished surface of germanium wafer deionized water rinsing 30S, another mistake hour hands tilt 30 ° of non-polished surfaces to germanium wafer and wash away ionized water 30S, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
In treatment method, the abluent in described rinse bath system often cleans 50 germanium wafer emptying and changes once.
The inventive method with existing methodical scrap/rework wafers number statistical result is in Table 1;The problem picture of wafer before and after this method is wherein used to see accompanying drawing 1 and accompanying drawing 2;Contrasted it can be seen that after using this technique, Waffer edge drug residue rate substantially reduces by two figure;
Table 1 the inventive method scraps/rework wafers number statistical result with existing methodical
The improvement of the inventive method essentially consists in: add, in the developing technique after the chemically mechanical polishing of conventional germanium wafer processing terminates, the process technique removing drug residue, germanium wafer is put into and rare oxalic acid solution swings and stands the sufficient time, the sodium hypochlorite of germanium wafer remained on surface or lithium hypochlorite etc. have the medicament of Oxidation and are cleaned up by reaction, rinse well with deionized water afterwards, ensure that the germanium wafer surface drug residual entering Cleaning and Passivation operation is few, stabilize the Cleaning and Passivation operation quality of production.
Although as it has been described above, represented and described the present invention with reference to specific preferred embodiment, but it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention premise defined without departing from claims, it can be made in the form and details various change.
Claims (6)
1. the method removing solar energy single germanium wafer polishing residual medicament, it is characterised in that: comprise the steps:
(1) abluent prepares: be dissolved in deionized water by oxalic acid, is configured to the oxalic acid abluent that concentration is 0.05~0.15mol/L, and adds the above-mentioned abluent of 10~20L in the rinse bath with medicine liquid circulation, and abluent keeps circulation;
(2) tentatively clean: the polishing disk after being completed by polishing operation takes off, and to the germanium wafer burnishing surface deionized water rinsing in polishing disk, with vacuum WAND, germanium wafer is taken out from polishing disk afterwards, and be sequentially inserted into turnover box, and ensure that burnishing surface is in the same direction;
(3) abluent cleans: the turnover box being loaded into germanium wafer immerses in the abluent in step (1) rinse bath got ready, and swings turnover box 5~30S along the parallel direction on germanium wafer surface, after turnover box stood in abluent 5~30S;
(4) post processing: turnover box is taken out from rinse bath, tilt 5~50 ° clockwise, first to the polished surface of germanium wafer deionized water rinsing 5~50S, another mistake hour hands tilt 5~50 ° of non-polished surface deionized water rinsing 5~50S to germanium wafer, load circulation after drying in drier and arrive Cleaning and Passivation operation after having rinsed.
2. the method for removal solar energy single germanium wafer according to claim 1 residual polishing medicament, it is characterised in that: described turnover box is 5~15 on chip.
3. the method for removal solar energy single germanium wafer according to claim 1 residual polishing medicament, it is characterised in that: the abluent in described rinse bath system often cleans 50 germanium wafer emptying and changes once.
4. the method for removal solar energy single germanium wafer according to claim 1 residual polishing medicament, it is characterised in that: the concentration of described oxalic acid abluent is 0.1mol/L.
5. the method for removal solar energy single germanium wafer according to claim 1 residual polishing medicament, it is characterised in that: in step (4), the angle of inclination clockwise of turnover box is 15~30 °.
6. the method for removal solar energy single germanium wafer according to claim 1 residual polishing medicament, it is characterised in that: in step (4), the angle of inclination counterclockwise of turnover box is 15~30 °.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114082740A (en) * | 2022-01-19 | 2022-02-25 | 北京通美晶体技术股份有限公司 | Method for cleaning germanium wafer and application thereof |
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CN105047538A (en) * | 2015-07-31 | 2015-11-11 | 江苏奥能光电科技有限公司 | Silicon wafer cleaning method and cleaning device |
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US20020132745A1 (en) * | 1999-11-15 | 2002-09-19 | Arch Specialty Chemicals | Non-corrosive cleaning composition for removing plasma etching residues |
CN1885499A (en) * | 2005-06-22 | 2006-12-27 | 住友电气工业株式会社 | Method of surface treating substrates and method of manufacturing III-V compound semiconductors |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114082740A (en) * | 2022-01-19 | 2022-02-25 | 北京通美晶体技术股份有限公司 | Method for cleaning germanium wafer and application thereof |
CN114082740B (en) * | 2022-01-19 | 2022-04-08 | 北京通美晶体技术股份有限公司 | Method for cleaning germanium wafer and application thereof |
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