CN101748002A - Fluorine-containing composition and application thereof - Google Patents
Fluorine-containing composition and application thereof Download PDFInfo
- Publication number
- CN101748002A CN101748002A CN200810203716A CN200810203716A CN101748002A CN 101748002 A CN101748002 A CN 101748002A CN 200810203716 A CN200810203716 A CN 200810203716A CN 200810203716 A CN200810203716 A CN 200810203716A CN 101748002 A CN101748002 A CN 101748002A
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- China
- Prior art keywords
- containing composition
- fluoro
- polysilicon
- fluorine
- monomer
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Classifications
-
- 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
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic compounds
-
- 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
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a fluorine-containing composition, which contains fluoride, a polyvinylpyrrolidone-type polymer and a carrier. The invention overcomes the defect of the high polysilicon corrosion rate of the prior fluorine-containing composition, provides the fluorine-containing composition effectively inhibiting polysilicon corrosion rate by adding the polyvinylpyrrolidone-type polymer which is screened out to apply to fluorine-containing systems and serves as a polysilicon corrosion inhibitor, and further widens the application range of the fluorine-containing composition in the fields of semiconductor wafer cleaning, polysilicon mechanical polishing and wet etching, solar batteries and the like. The invention also discloses the application of the fluorine-containing composition in semiconductor wafer cleaning.
Description
Technical field
The present invention relates to a kind of fluoro-containing composition and application thereof, be specifically related to fluoro-containing composition and application thereof in the semiconductor fabrication process.
Background technology
Polycrystalline silicon material is to be raw material reaches certain purity after the series of physical chemical reaction is purified electronic material with silicon, be very important intermediates in the silicon product industrial chain, being the main raw material of making silicon polished, solar cell and HIGH-PURITY SILICON goods, is information industry and the most basic starting material of new forms of energy industry.In field of semiconductor manufacture, polysilicon is widely used, as utilizes polysilicon to make grid (Gate) and through hole (Contact) etc.In the semiconductor components and devices manufacturing processed, the coating of photoresist layer, exposure and imaging are necessary process steps to the pattern manufacturing of components and parts.Before last (promptly after coating, imaging, ion implantation and the etching at photoresist layer) of patterning carried out next processing step, the residue of photoresist layer material need thoroughly be removed.In this process, can only remove residual polymkeric substance photoresist layer and inorganics, and can not attack infringement grid (Gate) and through hole material therefor such as polysilicon etc.
Fluoro-containing composition is to use more a kind of composition in wafer cleaning field.Fluorine element is owing to its bigger electronegativity, and atomic radius is little, usually can attack polysilicon, especially doped polysilicon (dopedpoly).And this usually can cause the change of semi-conductive characteristic dimension, and causes yield to descend.Therefore, in fluorine-containing composition, add suitable polysilicon corrosion inhibitor and seem necessary.Though US2007/0175104A1 has pointed out the polysilicon polish etch inhibitor that some use in polished semiconductor liquid, as polyacrylamide and derivative, polyoxyethylene glycol, contain the pure and mild polyvinylpyrrolidone of alkynyl; These corrosion inhibitors are mainly used under the alkaline condition, prevent the attack of hydroxide radical group to polysilicon, and this system only contains abrasive grains, water and alkali simultaneously, does not contain fluorochemical.And according to the characteristic (big as electronegativity, atomic radius is little) of fluorine, its corrosion and hydroxide radical group to polysilicon is then incomplete same to the mechanism of corrosion of polysilicon, can't determine that also can these a few class corrosion inhibitors be applicable in the system that contains fluorochemical.Therefore, seek the polysilicon corrosion inhibitor that a class is suitable in fluorine-containing system, the Application Areas scope for widening fluoro-containing composition has stronger realistic meaning and industrial requirements.
Summary of the invention
Technical problem to be solved by this invention is to have overcome the big defective of polysilicon erosion rate that existing fluoro-containing composition exists, a kind of fluoro-containing composition of effective inhibition polysilicon erosion rate is provided, further widened fluoro-containing composition in semiconductor wafer cleaning, polysilicon mechanical polishing and wet etching, the range of application in fields such as solar cell.The invention also discloses fluoro-containing composition and cleaning the semiconductor wafer Application for Field.
Fluoro-containing composition of the present invention, it contains fluorochemical, polyvinylpyrrolidone--type polymer and carrier.
Among the present invention, the effect of described polyvinylpyrrolidone--type polymer is a corrosion inhibitor, can effectively reduce the erosion rate of fluoro-containing composition to polysilicon.Polyvinylpyrrolidone--type polymer can be a homopolymer, also can be multipolymer.What wherein, described multipolymer was preferable is the multipolymer of vinyl pyrrolidone and other vinyl monomers except that it; Better is the binary or the terpolymer of vinyl pyrrolidone and other vinyl monomers except that it.Wherein, described vinyl monomer is the monomer that contains vinyl, one or more that preferable is in ethene, propylene, vinylbenzene, acrylamide, vinyl cyanide, acrylic monomer, methacrylic monomer, propylene esters monomer and the methacrylic esters monomer.What wherein, described acrylic monomer was preferable is vinylformic acid; What described methacrylic monomer was preferable is methacrylic acid; What described propylene esters monomer was preferable is methyl acrylate and/or Hydroxyethyl acrylate; What described methacrylic esters monomer was preferable is methyl methacrylate and/or hydroxyethyl methylacrylate.Wherein, the size of described polymericular weight suppresses efficient not obviously influence to the polysilicon corrosive to it in fluorine-containing combination liquid, the preferable polymkeric substance that can dissolve and reach following preferred content scope in the fluoro-containing composition system of selecting for use.What the content of described polymkeric substance was preferable is 0.001～5%, and better is 0.001～3%, and best is 0.01～1%, and per-cent is mass percent.
Among the present invention, described fluorochemical is to be the conventional fluorochemical that uses in the fluoro-containing composition of this area.Described fluorochemical preferably is hydrogen fluoride, ammonium bifluoride (NH
4HF
2) and the salt that forms of hydrogen fluoride and alkali in one or more; Described alkali is preferable is in ammoniacal liquor, quaternary ammonium hydroxide and the hydramine one or more; That described fluorochemical is better is hydrogen fluoride, ammonium bifluoride (NH
4HF
2), Methanaminium, N,N,N-trimethyl-, fluoride (N (CH
3)
4F) and trihydroxyethyl Neutral ammonium fluoride (N (CH
2OH)
3HE) one or more in.What the content of described fluorochemical was preferable is mass percent 0.1～40%.
Among the present invention, described carrier can be water, also can be the aqueous solution of organic solvent.Described organic solvent is the conventional organic solvent that uses in this area, preferable is selected from sulfoxide, sulfone, imidazolidone, pyrrolidone, imidazolone, alcohol, ether and the acid amides one or more.That wherein, described sulfoxide is preferable is C
1～C
4Sulfoxide and/or C
7～C
10The aryl sulfoxide, better is dimethyl sulfoxide (DMSO); That described sulfone is preferable is C
1～C
4Sulfone and/or C
7～C
10Aryl sulfone, better is tetramethylene sulfone; What described imidazolidone was preferable is 1,3-dimethyl-2-imidazolidone; What described pyrrolidone was preferable is N-Methyl pyrrolidone and/or hydroxyethyl-pyrrolidone; What described imidazolone was preferable is 1,3-dimethyl-2-imidazolone (DMI); That described alcohol is preferable is C
1～C
4Alkyl alcohol and/or C
7～C
10Aryl alcohol, better is propylene glycol and/or Diethylene Glycol; That described ether is preferable is C
3～C
20Ether, better is propylene glycol monomethyl ether and/or dipropylene glycol monomethyl ether; That described acid amides is preferable is C
1～C
6Alkylamide, better is dimethyl formamide and/or N,N-DIMETHYLACETAMIDE.The content of water is no less than 5% in the aqueous solution of described organic solvent, preferably is 10～90%; More preferably be 15～70%, per-cent is mass percent.
Fluoro-containing composition of the present invention can also add other conventional additives as required, and as metal corrosion inhibitor etc., its content generally is no more than 10%.
Among the present invention, described fluoro-containing composition can be applicable to semiconductor wafer cleaning, polysilicon mechanical polishing and wet etching, fields such as solar cell, and semiconductor wafer is cleaned in preferable being applied to.Fluoro-containing composition of the present invention can effectively suppress the polysilicon erosion rate when being used as the semiconductor die chip detergent.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is: the present invention has overcome the big defective of polysilicon erosion rate that existing fluoro-containing composition exists, by the polysilicon corrosion inhibitor polyvinylpyrrolidone--type polymer that in fluorine-containing system, is suitable for that adding filters out, provide a kind of fluoro-containing composition of effective inhibition polysilicon erosion rate.This fluoro-containing composition has further been widened fluoro-containing composition in semiconductor wafer cleaning, polysilicon mechanical polishing and wet etching, the range of application in fields such as solar cell.The invention also discloses fluoro-containing composition and cleaning the semiconductor wafer Application for Field.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
Embodiment 1～22
Table 1 has provided the embodiment 1～22 of fluoro-containing composition of the present invention, by prescription in the table, each component is mixed, and can make the fluoro-containing composition of each embodiment.
Table 1 fluoro-containing composition embodiment 1～22 of the present invention
Effect embodiment
Press each component of table 2 prescription uniform mixing, preparation comparative example A～E and clean-out system 1～10.
Table 2 comparative example A～E and clean-out system 1～10 and 40 ℃ of erosion rates thereof
The polysilicon erosion rate testing method of solution:
1) utilize the Nanospec6100 thickness tester to test the thickness (T1) of 4 * 4cm polysilicon silicon chip;
2) this 4 * 4cm polysilicon silicon chip is immersed in advance in the solution of constant temperature to 40 ℃ 30 minutes;
3) take out this 4 * 4cm polysilicon silicon chip, use washed with de-ionized water, high pure nitrogen dries up, and utilizes the thickness (T2) of Nanospec6100 thickness tester test 4 * 4cm polysilicon silicon chip again;
4) by being input to suitable procedure, the variation of above-mentioned one-tenth-value thickness 1/10 and soak time can calculate its erosion rate.
From table 2, comparative example A and D are as can be seen, poly(oxyethylene glycol) 400 corrosion to polysilicon in fluorine-containing system does not have restraining effect, show simultaneously fluorine to hydroxide radical group among the corrosion of polysilicon and the patent US2007/0175104A1 to the mechanism of corrosion of polysilicon and incomplete same.Therefore the polysilicon corrosion inhibitor needs screening again in fluorine-containing system.Comparative Examples E shows that the solubleness of polyacrylamide base polymer in this system is little in the table 2.
Comparative example A and clean-out system 1 add polyvinylpyrrolidone (K30) and can suppress the corrosion of polysilicon in 2% ammonium fluoride aqueous solution effectively as can be seen in the table 2, and its erosion rate is reduced to 0.67A/min from 30.0A/min.
From Comparative Examples B and clean-out system 2 as can be seen, even the concentration of Neutral ammonium fluoride is elevated to 40% from 2%, add the corrosion that polyvinylpyrrolidone (K30) also can suppress polysilicon, promptly erosion rate is reduced to 26.7A/min from 54.8A/min.
From Comparative Examples C and clean-out system 3 as can be seen, add polyvinylpyrrolidone (K30) and can suppress the corrosion of polysilicon in water and solvent system effectively, promptly erosion rate is reduced to 14.5A/min from 81.8A/min.
The molecular weight that clean-out system 3,4 and 5 shows polyvinylpyrrolidone is to the not obviously influence of its corrosion inhibition ability, and promptly the k value drops to 12 from 30, and its corrosion inhibition ability is under test condition, and is suitable substantially, is respectively 14.5,13.8 and 14.2A/min.
Clean-out system 5 and 9 shows that in the finite concentration scope, the consumption of polyvinylpyrrolidone is to the not obviously influence of its inhibitor efficiency.
Table 2 shows that simultaneously some binary of V-Pyrol RC and terpolymer have the polysilicon inhibitor efficiency suitable with the polyvinylpyrrolidone homopolymer.
Claims (17)
1. fluoro-containing composition, it contains fluorochemical, polyvinylpyrrolidone--type polymer and carrier.
2. fluoro-containing composition as claimed in claim 1 is characterized in that: described polyvinylpyrrolidone--type polymer is homopolymer and/or multipolymer.
3. fluoro-containing composition as claimed in claim 2 is characterized in that: described multipolymer is the multipolymer of vinyl pyrrolidone and other vinyl monomers except that it.
4. fluoro-containing composition as claimed in claim 3 is characterized in that: described multipolymer is the binary and/or the terpolymer of vinyl pyrrolidone and other vinyl monomers except that it.
5. as claim 3 or 4 described fluoro-containing compositions, it is characterized in that: described other vinyl monomers are one or more in ethene, propylene, vinylbenzene, acrylamide, vinyl cyanide, acrylic monomer, methacrylic monomer, propylene esters monomer and the methacrylic esters monomer.
6. fluoro-containing composition as claimed in claim 5 is characterized in that: described acrylic monomer is a vinylformic acid; Described methacrylic monomer is a methacrylic acid; Described propylene esters monomer is methyl acrylate and/or Hydroxyethyl acrylate; Described methacrylic esters monomer is methyl methacrylate and/or hydroxyethyl methylacrylate.
7. fluoro-containing composition as claimed in claim 1 is characterized in that: the content of described polyvinylpyrrolidone--type polymer is 0.001～5%, and per-cent is mass percent.
8. fluoro-containing composition as claimed in claim 1 is characterized in that: described fluorochemical is one or more in the salt that forms of hydrogen fluoride, ammonium bifluoride and hydrogen fluoride and alkali.
9. fluoro-containing composition as claimed in claim 8 is characterized in that: described alkali is one or more in ammoniacal liquor, quaternary ammonium hydroxide and the hydramine.
10. fluoro-containing composition as claimed in claim 8 is characterized in that: described fluorochemical is one or more in hydrogen fluoride, ammonium bifluoride, Methanaminium, N,N,N-trimethyl-, fluoride and the trihydroxyethyl Neutral ammonium fluoride.
11. fluoro-containing composition as claimed in claim 1 is characterized in that: the content of described fluorochemical is 0.1～40%, and per-cent is mass percent.
12. fluoro-containing composition as claimed in claim 1 is characterized in that: described carrier is the aqueous solution of water or organic solvent.
13. fluoro-containing composition as claimed in claim 12 is characterized in that: described organic solvent is one or more in sulfoxide, sulfone, imidazolidone, pyrrolidone, imidazolone, alcohol, ether and the acid amides.
14. fluoro-containing composition as claimed in claim 13 is characterized in that: described sulfoxide is C
1～C
4Sulfoxide and/or C
7～C
10The aryl sulfoxide; Described sulfone is C
1～C
4Sulfone and/or C
7～C
10Aryl sulfone; Described alcohol is C
1～C
4Alkyl alcohol and/or C
7～C
10Aryl alcohol; Described ether is C
3～C
20Ether; Described acid amides is C
1～C
6Alkylamide.
15. fluoro-containing composition as claimed in claim 13, it is characterized in that: described organic solvent is dimethyl sulfoxide (DMSO), tetramethylene sulfone, 1,3-dimethyl-2-imidazolidone, N-Methyl pyrrolidone, hydroxyethyl-pyrrolidone, 1, one or more in 3-dimethyl-2-imidazolone, propylene glycol, Diethylene Glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, dimethyl formamide and the N,N-DIMETHYLACETAMIDE.
16. fluoro-containing composition as claimed in claim 12 is characterized in that: the content of water is for being no less than 5% in the aqueous solution of described organic solvent, and per-cent is mass percent.
17. as the application of each described fluoro-containing composition of claim 1～16 in cleaning semiconductor wafer.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810203716A CN101748002A (en) | 2008-11-28 | 2008-11-28 | Fluorine-containing composition and application thereof |
| PCT/CN2009/001282 WO2010060271A1 (en) | 2008-11-28 | 2009-11-19 | Fluorine contained composition and application thereof |
| CN200980148362.2A CN102227518B (en) | 2008-11-28 | 2009-11-19 | Fluorine contained composition and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810203716A CN101748002A (en) | 2008-11-28 | 2008-11-28 | Fluorine-containing composition and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101748002A true CN101748002A (en) | 2010-06-23 |
Family
ID=42225208
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810203716A Pending CN101748002A (en) | 2008-11-28 | 2008-11-28 | Fluorine-containing composition and application thereof |
| CN200980148362.2A Active CN102227518B (en) | 2008-11-28 | 2009-11-19 | Fluorine contained composition and application thereof |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200980148362.2A Active CN102227518B (en) | 2008-11-28 | 2009-11-19 | Fluorine contained composition and application thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (2) | CN101748002A (en) |
| WO (1) | WO2010060271A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531369A (en) * | 2014-12-31 | 2015-04-22 | 镇江市港南电子有限公司 | High-efficiency easily-cleaned silicon slice detergent |
| CN104745089A (en) * | 2013-12-25 | 2015-07-01 | 安集微电子（上海）有限公司 | Chemically mechanical polishing liquid for flattening barrier layer and use method thereof |
| CN105040108A (en) * | 2015-08-21 | 2015-11-11 | 浙江启鑫新能源科技股份有限公司 | Texture surface making method for polycrystalline silicon solar battery |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08292562A (en) * | 1995-04-25 | 1996-11-05 | Hitachi Chem Co Ltd | Antireflection film composition and production of pattern using the same |
| DE10131723A1 (en) * | 2001-06-30 | 2003-01-16 | Henkel Kgaa | Corrosion protection agents and corrosion protection processes for metal surfaces |
| US20050194562A1 (en) * | 2004-02-23 | 2005-09-08 | Lavoie Raymond L.Jr. | Polishing compositions for controlling metal interconnect removal rate in semiconductor wafers |
-
2008
- 2008-11-28 CN CN200810203716A patent/CN101748002A/en active Pending
-
2009
- 2009-11-19 WO PCT/CN2009/001282 patent/WO2010060271A1/en active Application Filing
- 2009-11-19 CN CN200980148362.2A patent/CN102227518B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104745089A (en) * | 2013-12-25 | 2015-07-01 | 安集微电子（上海）有限公司 | Chemically mechanical polishing liquid for flattening barrier layer and use method thereof |
| CN104531369A (en) * | 2014-12-31 | 2015-04-22 | 镇江市港南电子有限公司 | High-efficiency easily-cleaned silicon slice detergent |
| CN105040108A (en) * | 2015-08-21 | 2015-11-11 | 浙江启鑫新能源科技股份有限公司 | Texture surface making method for polycrystalline silicon solar battery |
| CN105040108B (en) * | 2015-08-21 | 2017-11-17 | 浙江启鑫新能源科技股份有限公司 | The etching method of polysilicon solar cell |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2010060271A1 (en) | 2010-06-03 |
| CN102227518B (en) | 2015-05-27 |
| CN102227518A (en) | 2011-10-26 |
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Open date: 20100623 |