KR20080111268A - Cleaning solution composition and cleaning method using the same - Google Patents
Cleaning solution composition and cleaning method using the same Download PDFInfo
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- KR20080111268A KR20080111268A KR1020070059453A KR20070059453A KR20080111268A KR 20080111268 A KR20080111268 A KR 20080111268A KR 1020070059453 A KR1020070059453 A KR 1020070059453A KR 20070059453 A KR20070059453 A KR 20070059453A KR 20080111268 A KR20080111268 A KR 20080111268A
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- South Korea
- Prior art keywords
- ammonium
- ether
- cleaning
- liquid composition
- cleaning liquid
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims abstract description 78
- 239000000203 mixture Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims description 37
- -1 ammonium salt compound Chemical class 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- WFSMVVDJSNMRAR-UHFFFAOYSA-N 2-[2-(2-ethoxyethoxy)ethoxy]ethanol Chemical compound CCOCCOCCOCCO WFSMVVDJSNMRAR-UHFFFAOYSA-N 0.000 claims abstract description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 5
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 claims abstract description 5
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 5
- 150000007530 organic bases Chemical class 0.000 claims abstract description 5
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 150000003868 ammonium compounds Chemical class 0.000 claims abstract description 4
- 150000003867 organic ammonium compounds Chemical class 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 40
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 34
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 6
- 239000004254 Ammonium phosphate Substances 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 6
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 4
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 4
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 3
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 3
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 3
- QWOZZTWBWQMEPD-UHFFFAOYSA-N 1-(2-ethoxypropoxy)propan-2-ol Chemical compound CCOC(C)COCC(C)O QWOZZTWBWQMEPD-UHFFFAOYSA-N 0.000 claims description 2
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 2
- 229960001231 choline Drugs 0.000 claims description 2
- JVOPCCBEQRRLOJ-UHFFFAOYSA-M tetrapentylazanium;hydroxide Chemical compound [OH-].CCCCC[N+](CCCCC)(CCCCC)CCCCC JVOPCCBEQRRLOJ-UHFFFAOYSA-M 0.000 claims description 2
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 claims 2
- 239000002245 particle Substances 0.000 abstract description 24
- 238000005260 corrosion Methods 0.000 abstract description 21
- 230000007797 corrosion Effects 0.000 abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 19
- 239000011521 glass Substances 0.000 abstract description 16
- 239000000243 solution Substances 0.000 abstract description 10
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 4
- 239000003637 basic solution Substances 0.000 abstract 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000356 contaminant Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- ZMANZCXQSJIPKH-UHFFFAOYSA-O triethylammonium ion Chemical compound CC[NH+](CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-O 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229940043376 ammonium acetate Drugs 0.000 description 2
- 235000019257 ammonium acetate Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011146 organic particle Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011242 organic-inorganic particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DVUVKWLUHXXIHK-UHFFFAOYSA-N tetraazanium;tetrahydroxide Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[OH-].[OH-].[OH-].[OH-] DVUVKWLUHXXIHK-UHFFFAOYSA-N 0.000 description 1
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
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- 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
-
- 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
-
- C11D2111/22—
Abstract
Description
본 발명은 금속 배선의 손상 없이 기판 상에 잔류하는 유기 오염물 및 파티클을 효과적으로 제거할 수 있는 세정액 조성물 및 이를 이용한 세정 방법에 관한 것으로서, 특히, 액정표시장치, 플라즈마 표시장치 및 유기전계발광소자 등의 평판표시장치에 이용되는 세정액 조성물 및 이를 이용한 세정 방법에 관한 것이다. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cleaning liquid composition capable of effectively removing organic contaminants and particles remaining on a substrate without damaging metal wiring, and to a cleaning method using the same. A cleaning liquid composition used in a flat panel display device and a cleaning method using the same.
액정표시장치, 플라즈마 표시장치 및 유기전계발광소자 등의 평판표시장치(Flat Panel Display Device)는 반도체 장치와 같이, 성막, 노광, 현상, 배선 식각 등의 공정을 거쳐 제품이 제조된다.Flat panel display devices, such as liquid crystal display devices, plasma display devices, and organic light emitting display devices, are manufactured like a semiconductor device through a process such as film formation, exposure, development, and wiring etching.
하지만, 이러한 공정에 의해서 기판 표면에 각종의 유기물이나 무기물 등의 파티클이나 부착 오염이 발생한다. 이러한 오염물을 부착한 채로, 다음의 공정 처리를 실시했을 경우에는 막의 핀 홀이나 피트, 배선의 단선이나 브리지를 발생시켜, 제품 수율이 저하되는 문제점이 발생한다.However, by such a process, particles such as various organic matters and inorganic matters or adhesion contamination occur on the substrate surface. In the case where the following process treatment is carried out with these contaminants attached, a problem arises in that pinholes, pits, and wire breakage or bridge of the film are generated, resulting in a decrease in product yield.
상기와 같은 문제에 대해 이러한 오염물을 제거하기 위한 세정이 각 공정 간에 행해져 각종 오염물에 대한 세정액에 대해서도 많은 제안이 나와 있다.In order to solve such a problem, cleaning to remove such contaminants is performed between the respective processes, and many proposals have been made for cleaning liquids for various contaminants.
종래에는 세정액 조성물로서 반도체 장치에 이용되는 세정액 조성물을 평판표시장치에 그대로 적용하는 경우가 많이 있었다. 일본 특허공개공보 2005-154558에서는 H3PO4, HF, 암모니아 및/또는 아민을 함유 하는 세정액 조성물을 개시하고 있다. 하지만 상기 특허는 반도체 장치용 세정액 조성물에 관한 것이다. 만약 상기 반도체 장치용 세정액 조성물을 평판표시장치에 그대로 적용한다면, 평판표시장치에 이용되는 가장 대표적인 기판인 유리 기판이나, 가장 대표적인 배선 재료인 Al을 격렬하게 식각하는 HF를 포함하기 때문에, 평판표시장치의 세정액 조성물로 이용하기에는 부적합한 문제점이 있다.Conventionally, the cleaning liquid composition used for a semiconductor device as a cleaning liquid composition has often been applied to a flat panel display as it is. Japanese Patent Laid-Open No. 2005-154558 discloses a cleaning liquid composition containing H 3 PO 4 , HF, ammonia and / or amines. However, the patent relates to a cleaning liquid composition for a semiconductor device. If the cleaning liquid composition for a semiconductor device is applied to a flat panel display device as it is, the flat panel display device includes a glass substrate which is the most representative substrate used for the flat panel display device or HF which intensively etches Al which is the most representative wiring material. There is a problem that is not suitable for use as a cleaning liquid composition.
한편, 세정 또는 레지스트 박리공정 중 세정액 조성물 또는 레지스트 박리액 조성물로 인한 반도체 장치 또는 평판표시장치에 형성된 금속의 부식을 방지하기 위하여 부식방지기능이 추가된 조성물도 많이 개시되고 있다. 예를 들면, 일본국 특허공개공보 2000-232063호에는 인산과 인산 암모늄을 부식방지로 이용하는 조성물이 개시되었다. 하지만 상기 조성물은 레지스트 잔사 제거제에 관한 것이다. 또한, 이 레지스트 잔사 제거제를 평판표시장치에 세정액 조성물로서 이용한다면, 레지스트 잔사 제거제의 pH가 산성범위이므로 세정 초기의 단계에 기본적 특성인 침전물의 용해성과 알루미늄 배선의 부식성과의 양립이 불충분하여, 평판표시장치에 적용하기에는 부적합한 문제점이 있다.On the other hand, in order to prevent the corrosion of the metal formed in the semiconductor device or the flat panel display due to the cleaning liquid composition or the resist stripping liquid composition during the cleaning or resist stripping process, there are also many compositions added with a corrosion protection function. For example, Japanese Patent Laid-Open No. 2000-232063 discloses a composition using phosphoric acid and ammonium phosphate as corrosion protection. However, the composition relates to a resist residue remover. In addition, if the resist residue remover is used as a cleaning liquid composition in a flat panel display device, since the pH of the resist residue remover is in the acidic range, both the solubility of the precipitate which is a basic characteristic at the initial stage of cleaning and the corrosion resistance of the aluminum wiring are insufficient. There is a problem that is not suitable for application to a display device.
따라서 이 분야에서 이러한 문제점을 해결하기 위하여 평판표시장치 전용 의 새로운 세정액 조성물의 개발이 요구되고 있다.Therefore, in order to solve such a problem in this field, the development of a new cleaning liquid composition for flat panel display devices is required.
상기와 같은 종래기술의 문제점을 해결하고자, 본 발명은 유리기판 상의 유기 오염물이나 파티클 제거에 적합하고, 알루미늄 또는 알루미늄 합금 배선의 부식을 방지하는 세정액 조성물 및 이를 이용한 세정 방법을 제공하는 것을 목적으로 한다.In order to solve the problems of the prior art as described above, an object of the present invention is to provide a cleaning liquid composition suitable for removing organic contaminants or particles on a glass substrate, and to prevent corrosion of aluminum or aluminum alloy wiring and a cleaning method using the same. .
본 발명의 상기 목적을 실현하기 위하여, 본 발명은 염기성 수용액; 암모늄염 화합물; 알킬렌글리콜 모노알킬에테르 화합물; 및 물을 포함하는 것을 특징으로 하는 세정액 조성물을 제공한다.In order to realize the above object of the present invention, the present invention is a basic aqueous solution; Ammonium salt compounds; Alkylene glycol monoalkyl ether compounds; And it provides a cleaning liquid composition comprising water.
또한 본 발명은 상기 세정액 조성물을 이용한 세정방법을 제공한다.The present invention also provides a cleaning method using the cleaning liquid composition.
이하, 본 발명에 대해 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명의 세정액 조성물에 포함되는 염기성 수용액은 유기 오염물을 용해시키는 작용을 수행하며, 또한 파티클이나 유기 오염물의 기판 또는 금속 배선과의 접착력을 약화시켜 이들을 세정하는 역할을 수행한다. The basic aqueous solution contained in the cleaning liquid composition of the present invention performs a function of dissolving organic contaminants, and also weakens adhesion to the substrate or metal wiring of particles or organic contaminants to clean them.
상기 염기성 수용액의 구체적인 예로는 무기염기의 수용액, 유기염기의 수 용액 등을 들 수 있다. 상기 무기염기의 예로는 수산화 암모늄, 수산화 나트륨, 수산화 칼륨 등을 들 수 있고, 상기 유기염기의 예로는 테트라메틸암모늄 히드록시드, 테트라 에틸 암모늄 히드록시드, 테트라부틸 암모늄 히드록시드, 테트라펜틸암모늄 히드록시드 및 콜린 등을 들 수 있다. 이 중에서 수산화 암모늄 및 테트라암모늄 히드록시드를 이용하는 것이 바람직하다.Specific examples of the basic aqueous solution include an aqueous solution of an inorganic base, an aqueous solution of an organic base, and the like. Examples of the inorganic base include ammonium hydroxide, sodium hydroxide, potassium hydroxide and the like, and examples of the organic base include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutyl ammonium hydroxide, tetrapentylammonium Hydroxide, choline and the like. It is preferable to use ammonium hydroxide and tetraammonium hydroxide among these.
상기 염기성 수용액은 전체 조성물에 대하여 0.05 내지 5중량%로 포함되는 것이 바람직하며, 더욱 바람직하게는 0.1 내지 1 중량%이다. 상기 염기성 수용액이 0.05 내지 5 중량%로 포함되면, 유기 오염물 등을 용해시켜 충분한 세정력을 구현할 수 있고, 금속, 특히 알루미늄 또는 알루미늄 합금 배선에 대한 부식이 방지되는 이점이 있다. 또한, 이와 같은 이점으로 인해 제조 수율이 향상되는 이점도 있다. The basic aqueous solution is preferably contained in 0.05 to 5% by weight based on the total composition, more preferably 0.1 to 1% by weight. When the basic aqueous solution is contained in 0.05 to 5% by weight, it is possible to implement a sufficient cleaning power by dissolving organic contaminants and the like, there is an advantage that corrosion to metal, in particular aluminum or aluminum alloy wiring is prevented. In addition, there is an advantage that the manufacturing yield is improved due to such advantages.
상기 염기성 수용액을 사용한 세정액 조성물의 pH는 바람직하게는 pH 6 내지 pH 13, 더욱 바람직하게는 pH 8 내지 pH 11의 범위이다. 상술한 범위내의 pH는 알루미늄 또는 알루미늄 합금 배선에 대한 부식을 방지하는 효과가 있다.The pH of the cleaning liquid composition using the basic aqueous solution is preferably in the range of pH 6 to pH 13, more preferably pH 8 to pH 11. PH within the above range has the effect of preventing corrosion to the aluminum or aluminum alloy wiring.
본 발명의 세정액 조성물에 포함되는 암모늄염 화합물은 알루미늄 또는 알루미늄 합금에 대한 부식방지에 우수한 작용을 한다. 좀 더 상세하게는, 상기 암모늄염 화합물의 음이온 성분은 산소기의 비공유 전자로 인한 금속과의 결합으로 금속표면에 부착되어 히드록시기에 의한 금속 부식을 억제한다. 또한 상기 암모늄염 화합물에 대한 암모늄 성분은 염기성 수용액의 히드록시기와 함께 유리기판 위의 유기오염물이나 파티클 제거에 우수한 효과가 있다. The ammonium salt compound included in the cleaning liquid composition of the present invention plays an excellent role in preventing corrosion to aluminum or aluminum alloy. More specifically, the anion component of the ammonium salt compound is attached to the metal surface by bonding with the metal due to the non-covalent electrons of the oxygen group to suppress metal corrosion by the hydroxyl group. In addition, the ammonium component with respect to the ammonium salt compound has an excellent effect in removing organic contaminants or particles on the glass substrate with the hydroxyl group of the basic aqueous solution.
상기 암모늄염 화합물은 무기암모늄 화합물 및 유기암모늄 화합물로 이루어진 군에서 선택되는 1종 또는 2종 이상을 사용하는 것이 바람직하다. 상기 무기암모늄염 화합물의 구체적인 예로는 질산암모늄, 인산암모늄, 붕산암모늄 및 황산암모늄 등을 들 수 있고, 상기 유기암모늄염 화합물의 구체적인 예로는 암모늄시트레이트, 암모늄옥살레이트, 암모늄포메이트, 암모늄카보네이트 및 암모늄아세테이트 등을 들 수 있다.The ammonium salt compound is preferably used one or two or more selected from the group consisting of inorganic ammonium compounds and organic ammonium compounds. Specific examples of the inorganic ammonium salt compound include ammonium nitrate, ammonium phosphate, ammonium borate and ammonium sulfate. Specific examples of the organic ammonium salt compound include ammonium citrate, ammonium oxalate, ammonium formate, ammonium carbonate and ammonium acetate. Etc. can be mentioned.
상기 암모늄염 화합물의 농도는 바람직하게는 0.01 내지 10중량%, 더욱 바람직하게는 0.1내지 2중량%이다. 상기 암모늄염 화합물이 0.01 내지 10중량%로 포함되면, 금속에 대한 부식방지력이 향상되고, 암모늄염이 유리기판 표면에 잔류하는 것을 방지할 수 있는 이점이 있다.The concentration of the ammonium salt compound is preferably 0.01 to 10% by weight, more preferably 0.1 to 2% by weight. When the ammonium salt compound is included in an amount of 0.01 to 10% by weight, corrosion resistance to metal is improved, and the ammonium salt compound can be prevented from remaining on the surface of the glass substrate.
본 발명의 세정액 조성물에 있어서 알킬렌글리콜 모노알킬에테르 화합물은 유기오염물을 용해시키는 양자성 극성 용제역할을 한다. 또한 상기 알킬렌글리콜 모노알킬에테르 화합물은 용제로서의 기능 외에도 세정액의 표면장력을 저하시켜 유리기판에 대한 습윤성을 증가시켜 세정력을 향상시켜 준다. 또한 높은 비점으로 인해 약액 사용 시 휘발에 의한 약액 손실을 최소화 할 수 있다.In the cleaning liquid composition of the present invention, the alkylene glycol monoalkyl ether compound serves as a proton polar solvent for dissolving organic contaminants. In addition, the alkylene glycol monoalkyl ether compound, in addition to its function as a solvent, lowers the surface tension of the cleaning liquid, thereby increasing the wettability on the glass substrate, thereby improving the cleaning power. In addition, due to the high boiling point it is possible to minimize the loss of the chemical solution due to volatilization.
상기 알킬렌글리콜 모노알킬에테르 화합물로는 에틸렌글리콜모노부틸에테르(BG), 디에틸렌글리콜 모노메틸에테르(MDG), 디에틸렌글리콜 모노에틸에테르(carbitol), 디에틸렌글리콜 모노부틸에테르(BDG), 디프로필렌글리콜 모노메틸에 테르(DPM), 디프로필렌글리콜 모노에틸에테르(MFDG), 트리에틸렌글리콜 모노부틸에테르(BTG), 트리에틸렌글리콜 모노에틸에테르(MTG) 및 프로필렌글리콜 모노메틸에테르(MFG)로 이루어진 군으로부터 1종 이상 선택되는 화합물을 사용하는 것이 바람직하다.As the alkylene glycol monoalkyl ether compound, ethylene glycol monobutyl ether (BG), diethylene glycol monomethyl ether (MDG), diethylene glycol monoethyl ether (carbitol), diethylene glycol monobutyl ether (BDG), di Propylene glycol monomethyl ether (DPM), dipropylene glycol monoethyl ether (MFDG), triethylene glycol monobutyl ether (BTG), triethylene glycol monoethyl ether (MTG) and propylene glycol monomethyl ether (MFG) It is preferable to use a compound selected from one or more types from the group.
상기 알킬렌글리콜 모노알킬에테르의 농도는 바람직하게는 0.05 내지 50중량%, 더욱 바람직하게는 0.5 내지 40중량% 이다. 상기 알킬렌글리콜 모노알킬에테르가 0.05 내지 50중량%로 포함되면, 유기 오염물에 대한 용해력이 충분히 발휘되고, 세정액 조성물의 표면장력을 저하시켜 습윤성이 증가되어 세정력이 증대되는 이점이 있다. The concentration of the alkylene glycol monoalkyl ether is preferably 0.05 to 50% by weight, more preferably 0.5 to 40% by weight. When the alkylene glycol monoalkyl ether is contained in an amount of 0.05 to 50% by weight, the dissolving power to organic contaminants is sufficiently exerted, the surface tension of the cleaning liquid composition is lowered, and the wettability is increased to increase the cleaning power.
본 발명의 세정액 조성물에 포함되는 물은 특별히 한정되는 것은 아니나, 탈이온수가 바람직하다. 더욱 바람직하게는 물의 비저항 값(즉, 물속에 이온이 제거된 정도)이 18㏁/㎝이상인 탈이온수를 사용하는 것이다. Although the water contained in the cleaning liquid composition of this invention is not specifically limited, Deionized water is preferable. More preferably, deionized water having a specific resistance value of the water (that is, the degree to which ions are removed in the water) is 18 kW / cm or more is used .
상기와 같은 세정액을 이용하여 세정방법을 수행할 때, 스프레이(Spray)방식, 스핀(Spin)방식, 딥핑(Dipping)방 및 초음파를 이용한 딥핑 방식으로 이루어진 군에서 선택되는 어느 하나로 수행할 수 있다. 또한, 가장 우수한 세정 효과를 나타낼 수 있는 세정액 조성물의 온도는 20 내지 80℃이며, 바람직하게는 20 내지 50℃이다. 상기 세정방법이 습식공정일 때, 세정시간은 제거효율을 기대할 때 길게 하는 것이 유리하나 생산성을 고려해 볼 때 세정시간은 30초 내지 10분 정도가 바 람직하다.When the cleaning method is performed using the cleaning solution as described above, the cleaning method may be performed by any one selected from the group consisting of a spray method, a spin method, a dipping room, and a dipping method using ultrasonic waves. Moreover, the temperature of the cleaning liquid composition which can exhibit the most outstanding cleaning effect is 20-80 degreeC, Preferably it is 20-50 degreeC. When the cleaning method is a wet process, it is advantageous to lengthen the cleaning time when the removal efficiency is expected, but considering the productivity, the cleaning time is preferably about 30 seconds to 10 minutes.
이하, 실시예를 들어 본 발명을 상세히 설명하지만, 본 발명은 하기 실시예로만 한정되는 것은 아니다. 하기 실시예는 본 발명의 바람직한 조성뿐만 아니라 본 발명의 조성물을 이용하기 위한 바람직한 방법을 제시한다.Hereinafter, although an Example is given and this invention is demonstrated in detail, this invention is not limited only to a following example. The following examples set forth preferred compositions as well as preferred methods for using the compositions of the invention.
실시예Example 1 내지 1 to 16 및 16 and 비교예Comparative example 1 내지 4: 세정액 조성물의 제조 1 to 4: Preparation of Cleaning Liquid Composition
표 1에 기재된 성분과 조성비로 혼합하고 교반하여 세정액 조성물을 제조하였다. The cleaning liquid composition was prepared by mixing and stirring the components shown in Table 1 and the composition ratio.
주) TMAH: 테트라메틸암모늄 히드록시드TMAH: tetramethylammonium hydroxide
TEAH: 테트라에틸암모늄 히드록시드TEAH: tetraethylammonium hydroxide
NH4OH: 수산화암모늄NH 4 OH: ammonium hydroxide
BDG: 디에틸렌글리콜 모노부틸에테르BDG: diethylene glycol monobutyl ether
BG: 에틸렌글리콜 모노부틸에테르BG: ethylene glycol monobutyl ether
MDG: 디에틸렌글리콜 모노메틸에테르 MDG: diethylene glycol monomethyl ether
카비톨(Carbitol): 디에틸렌글리콜 모노에틸에테르Carbitol: diethylene glycol monoethyl ether
시험예1Test Example 1 : 유기오염물 : Organic pollutants 제거력Removal 평가 evaluation
유리기판을 대기 중에 24시간 방치하여 대기중의 각종 유기물, 무기물, 파티클 등에 오염시킨 후 스프레이식 유리 기판 세정장치를 이용하여 2분 동안 40℃에서 상기의 수용액으로 세정후 초순수에 30초 세척한 후 질소로 건조하였다. 상기 유리기판 위에 0.5㎕의 초순수 방울을 떨어뜨려 세정후의 접촉각을 측정하여 표2에 기재하였다. After leaving the glass substrate in the air for 24 hours to contaminate various organic materials, inorganic materials, and particles in the air, and then using a spray-type glass substrate cleaning device, the glass substrate is washed with the aqueous solution at 40 ° C. for 2 minutes, and then washed in ultrapure water for 30 seconds Dried with nitrogen. 0.5 μl of ultrapure water was dropped on the glass substrate, and the contact angle after washing was measured.
시험예2Test Example 2 : 유기 Organic 파티클particle 제거력Removal 평가 evaluation
각각의 세정액 조성물을 가지고, 평균 입자 크기가 0.8㎛인 폴리스티렌라텍스(이하 PLS라 함) 파티클 솔루션으로 유리기판을 오염시킨 후 1분간 3,000rpm으로 스핀(spin) 드라이한 후 스프레이식 유리 기판 세정장치를 이용하여 2분 동안 40℃에서 각각의 세정액으로 세정 후 초순수에 30초 세척한 후 질소로 건조하였다. 이때 세정 전후의 파티클 수는 표면입자측정기(Surface scan)로 0.3㎛ 이상의 파티클 수를 측정하여 표2에 기재하였다.With each cleaning liquid composition, the glass substrate was contaminated with polystyrene latex (hereinafter referred to as PLS) particle solution having an average particle size of 0.8 μm, spin-dried at 3,000 rpm for 1 minute, and then the sprayed glass substrate cleaning device was After washing with each washing solution at 40 ℃ for 2 minutes using 30 seconds in ultrapure water and then dried with nitrogen. At this time, the number of particles before and after the cleaning is shown in Table 2 by measuring the particle number of 0.3㎛ or more with a surface scan (Surface scan).
시험예3Test Example 3 : 무기 : weapon 파티클particle 제거력Removal 평가 evaluation
각각의 세정액 조성물을 가지고, 입자 크기가 서브마이크론(Submicron)인 질화 실리콘 파티클 솔루션으로 유리기판을 오염시킨 후 1분간 3000rpm으로 스핀(spin) 드라이한 후 스프레이식 유리 기판 세정장치를 이용하여 2분 동안 40℃에서 각각의 세정액으로 세정 후 초순수에 30초 세척한 후 질소로 건조하였다. 이때 세정 전후의 파티클 수는 표면입자측정기(Surface scan)로 0.3㎛ 이상의 파티클 수를 측정하여 표2에 기재하였다.With each cleaning liquid composition, the glass substrate was contaminated with a silicon nitride particle solution having a particle size of submicron, followed by spin drying at 3000 rpm for 1 minute, followed by a spray glass substrate cleaning apparatus for 2 minutes. After washing with each washing solution at 40 ℃ 30 seconds in ultrapure water and then dried with nitrogen. At this time, the number of particles before and after the cleaning is shown in Table 2 by measuring the particle number of 0.3㎛ or more with a surface scan (Surface scan).
시험예4Test Example 4 : 알루미늄 : aluminum 부식력Corrosion 평가 evaluation
알루미늄이 2000Å 두께로 형성된 유리기판을 실시예 1내지 16 및 비교예 1내지 4의 세정액에 30분간 딥핑시켰다. 이때 세정액의 온도는 40℃이며 알루미늄 막의 두께는 딥핑 이전 및 이후에 측정하였고, 알루미늄막의 용해속도를 알루미늄 막의 두께 변화로부터 계산하여 측정하여 표2에 기재하였다.A glass substrate having a thickness of 2000 mm 3 was dipped into the cleaning solutions of Examples 1 to 16 and Comparative Examples 1 to 4 for 30 minutes. At this time, the temperature of the cleaning solution is 40 ℃ and the thickness of the aluminum film was measured before and after the dipping, and calculated by calculating the dissolution rate of the aluminum film from the thickness change of the aluminum film is shown in Table 2.
<접촉각 평가 기준><Contact angle evaluation standard>
30° 이하: 세정력 우수30 ° or less: excellent cleaning power
40° 이하: 세정력 양호40 ° or less: Good cleaning power
50° 이하: 세정력 미흡50 ° or less: insufficient cleaning power
50° 초과: 세정력 불량 (오염 시 접촉각 70~80°)Above 50 °: Poor cleaning power (Contact angle 70 ~ 80 ° in case of contamination)
<알루미늄 평가 기준><Aluminum evaluation standard>
◎: 알루미늄 부식량 50Å 이하/30분 ◎: Aluminum corrosion amount less than 50Å / 30 minutes
○: 알루미늄 부식량 100Å 이하/30분 ○: aluminum corrosion rate 100 kPa or less / 30 minutes
△: 알루미늄 부식량 300Å 이하/30분 △: aluminum corrosion amount less than 300 kPa / 30 minutes
×: 알루미늄 부식량 300Å 이상/30분 X: aluminum corrosion rate of 300 kPa or more / 30 minutes
<파티클 평가 기준><Particle Evaluation Criteria>
◎: 파티클 제거력 90% 이상◎: 90% or more of particle removal power
○: 파티클 제거력 80%이상 ○: more than 80% of particle removal
△: 파티클 제거력 70%이상△: more than 70% of particle removal power
×: 파티클 제거력 70%미만 ×: less than 70% of particle removal
실시예1 내지 16의 경우에는 모두 유기오염물의 제거력이 있음을 알 수 있다. 또한, 접촉각이 20°~40°를 가지게 되어 유기오염물의 제거력을 나타냄을 보여주며, 유기 파티클 및 무기 파티클이 80% 이상의 제거력을 나타내었다. 또한 실시예1 내지 15의 경우에는 암모늄염 화합물의 첨가로 알루미늄에 대한 부식방지 효과가 있었다. 그러나 비교예1과 2의 경우에는 암모늄염이 첨가되지 않거나 함량이 충분치 못하는 경우 알루미늄의 부식 현상이 관찰되었으며, 비교예3와 같이 암모늄염화합물의 양이 적정치를 초과하여 첨가되었을 경우에도 부식 현상이 관찰되었다. 또한, 비교예4는 알루미늄 부식방지 효과는 나타났으나, 세정력 및 파티클 제거력이 모두 불량인 것을 알 수 있다.In the case of Examples 1 to 16, it can be seen that all have the ability to remove organic contaminants. In addition, the contact angle has a 20 ° ~ 40 ° showing the removal power of organic contaminants, organic particles and inorganic particles showed a removal power of more than 80%. In addition, in Examples 1 to 15, there was an anticorrosion effect on aluminum by the addition of an ammonium salt compound. However, in the case of Comparative Examples 1 and 2, the corrosion phenomenon of aluminum was observed when the ammonium salt was not added or the content was insufficient, and the corrosion phenomenon was observed even when the amount of the ammonium salt compound was added in excess of the appropriate value as in Comparative Example 3. It became. In addition, Comparative Example 4 showed an aluminum corrosion protection effect, it can be seen that both the cleaning power and the particle removal power is poor.
이상에서 상술한 바와 같이, 본 발명의 세정액 조성물은 평판표시장치 기판 제조 시 성막 형성 전후의 유리기판 표면에 대한 유기물오염 및 파티클 제거력 이 우수한 효과가 있다. 또한, 평판표시장치 기판 상에 형성된 알루미늄 및 알루미늄 합금배선의 부식방지 효과가 우수하고, 다량의 탈이온수를 포함하고 있어 취급이 용이하며 환경적으로 유리한 효과가 있다.As described above, the cleaning liquid composition of the present invention has excellent effects of organic contamination and particle removal on the surface of the glass substrate before and after the film formation when the flat panel display substrate is manufactured. In addition, it is excellent in the corrosion protection effect of the aluminum and aluminum alloy wiring formed on the flat panel display device, and contains a large amount of deionized water, it is easy to handle and has an environmentally beneficial effect.
Claims (15)
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| KR1020070059453A KR20080111268A (en) | 2007-06-18 | 2007-06-18 | Cleaning solution composition and cleaning method using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011031092A3 (en) * | 2009-09-11 | 2011-08-04 | 동우 화인켐 주식회사 | Cleaning solution composition for substrate for preparation of flat panel display |
| CN102575201A (en) * | 2009-09-11 | 2012-07-11 | 东友Fine-Chem股份有限公司 | Cleaning solution composition for substrate for preparation of flat panel display |
| US8551575B1 (en) | 2008-09-08 | 2013-10-08 | Lam Research | Methods and solutions for preventing the formation of metal particulate defect matter upon a substrate after a plating process |
| KR20160038166A (en) * | 2014-09-29 | 2016-04-07 | 한경대학교 산학협력단 | Composition for removing black ink for recycling electronic part |
-
2007
- 2007-06-18 KR KR1020070059453A patent/KR20080111268A/en not_active Application Discontinuation
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8551575B1 (en) | 2008-09-08 | 2013-10-08 | Lam Research | Methods and solutions for preventing the formation of metal particulate defect matter upon a substrate after a plating process |
| WO2011031092A3 (en) * | 2009-09-11 | 2011-08-04 | 동우 화인켐 주식회사 | Cleaning solution composition for substrate for preparation of flat panel display |
| CN102575201A (en) * | 2009-09-11 | 2012-07-11 | 东友Fine-Chem股份有限公司 | Cleaning solution composition for substrate for preparation of flat panel display |
| CN102575201B (en) * | 2009-09-11 | 2014-07-09 | 东友Fine-Chem股份有限公司 | Cleaning solution composition for substrate for preparation of flat panel display |
| KR20160038166A (en) * | 2014-09-29 | 2016-04-07 | 한경대학교 산학협력단 | Composition for removing black ink for recycling electronic part |
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