KR101399502B1 - Remover composition for removing Thermosetting resin of TFT-LCD - Google Patents
Remover composition for removing Thermosetting resin of TFT-LCD Download PDFInfo
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- KR101399502B1 KR101399502B1 KR1020080091951A KR20080091951A KR101399502B1 KR 101399502 B1 KR101399502 B1 KR 101399502B1 KR 1020080091951 A KR1020080091951 A KR 1020080091951A KR 20080091951 A KR20080091951 A KR 20080091951A KR 101399502 B1 KR101399502 B1 KR 101399502B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 49
- 239000011347 resin Substances 0.000 title abstract description 10
- 229920005989 resin Polymers 0.000 title abstract description 10
- 229920001187 thermosetting polymer Polymers 0.000 title abstract description 9
- -1 alkylene glycol ether Chemical compound 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 14
- 230000007797 corrosion Effects 0.000 claims abstract description 14
- 238000005260 corrosion Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000005210 alkyl ammonium group Chemical group 0.000 claims abstract description 5
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 42
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002798 polar solvent Substances 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- CKFGINPQOCXMAZ-UHFFFAOYSA-N methanediol Chemical compound OCO CKFGINPQOCXMAZ-UHFFFAOYSA-N 0.000 claims description 4
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 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
- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 claims description 3
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 3
- KUFNEMCYFOJAGR-UHFFFAOYSA-N 4-benzyl-2h-triazole Chemical compound C=1C=CC=CC=1CC1=CNN=N1 KUFNEMCYFOJAGR-UHFFFAOYSA-N 0.000 claims description 3
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 2
- BQCCJWMQESHLIT-UHFFFAOYSA-N 1-propylsulfinylpropane Chemical compound CCCS(=O)CCC BQCCJWMQESHLIT-UHFFFAOYSA-N 0.000 claims description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-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
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 2
- CCAFPWNGIUBUSD-UHFFFAOYSA-N diethyl sulfoxide Chemical compound CCS(=O)CC CCAFPWNGIUBUSD-UHFFFAOYSA-N 0.000 claims description 2
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 2
- 235000019256 formaldehyde Nutrition 0.000 claims description 2
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 2
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims description 2
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 claims description 2
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 11
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000002950 deficient Effects 0.000 abstract description 2
- 229920001721 polyimide Polymers 0.000 description 21
- 239000004642 Polyimide Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005536 corrosion prevention Methods 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 229940093476 ethylene glycol Drugs 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08L61/04, C08L61/18 and C08L61/20
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/34—Imagewise removal by selective transfer, e.g. peeling away
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
-
- C11D2111/22—
Abstract
본 발명은 티에프티 엘시디의 제조공정에서 티에프티 엘시디의 열경화성 수지 형성공정 중 발생하는 불량의 기판을 재사용하기 위한 박리액 조성물에 관한 것으로, (a) 암모늄 하이드록사이드 또는 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드 화합물 0.5 내지 15 중량부; (b) 탄소수 1 내지 4의 알킬기를 갖는 알킬렌글리콜에테르 9 내지 89 중량부; (c) 글리콜 화합물 10 내지 40 중량부; (d) 부식방지제 0.01 내지 5 중량부; 및 (e) 물 0.1 내지 5 중량부를 포함하는 열경화성 수지 박리액 조성물에 관한 것이다.The present invention relates to a release liquid composition for reusing defective substrates generated during a process for forming a thermosetting resin of a TEFLICHIDYI in a process for producing TEFLICIDYDIA. The present invention relates to a release liquid composition comprising (a) ammonium hydroxide or an alkyl group having 1 to 4 carbon atoms 0.5 to 15 parts by weight of an alkyl ammonium hydroxide compound; (b) 9 to 89 parts by weight of an alkylene glycol ether having an alkyl group having 1 to 4 carbon atoms; (c) 10 to 40 parts by weight of a glycol compound; (d) 0.01 to 5 parts by weight of a corrosion inhibitor; And (e) 0.1 to 5 parts by weight of water.
본 발명의 박리액 조성물은 칼라 레지스트뿐 아니라, 네가티브 및 포지티브 유기절연막를 하부막질인 무기절연막 및 각종 금속 배선에 손상을 주지 않고 단시간에 제거하여 칼라필터 기판 및 티에프티 기판을 재사용할 수 있도록 한다.The stripping liquid composition of the present invention enables not only the color resist but also the negative and positive organic insulating films to be removed in a short time without damaging the inorganic insulating film and the various metal wirings as the underlying film to enable the reuse of the color filter substrate and the TiOFT substrate.
열경화성수지, 유기절연막, 박리액, 티에프티 엘시디 A thermosetting resin, an organic insulating film, a peeling liquid,
Description
본 발명은 티에프티 엘시디(TFT-LCD)용 열경화성 수지 박리액 조성물에 관한 것으로서, 보다 상세하게는 열경화성 수지 공정 중에서 발생하는 불량 기판의 유전체층, 유기보호층, 절연층, 배향막, 컬러필터 등의 제거효과가 우수하고 하부막층을 재사용할 수 있는 티에프티 엘시디의 칼라 레지스트, 네가티브 및 포지티브 유기절연막용 박리액 조성물에 관한 것이다.The present invention relates to a thermosetting resin stripper composition for a TFT-LCD, and more particularly, to a thermosetting resin stripper composition for a TFT-LCD which eliminates removal of a dielectric layer, an organic protective layer, an insulating layer, And a peeling liquid composition for a negative resist and a positive organic insulating film of a TEFLICHIDI, which is excellent in the effect and can reuse the lower film layer.
현재 유기보호층 하부막질로 무기 절연막 및 금속이 존재하는 공정에서 발생되는 불량 기판의 경우, 하부막질에 손상을 주지 않고 유기절연막을 제거하는 것이 어려운 것으로 알려져 있다.It is known that it is difficult to remove the organic insulating film without damaging the underlying film in the case of the defective substrate which is generated in the process in which the inorganic insulating film and the metal exist in the organic film under the organic protective layer.
기존의 공정은 일반적으로 네가티브형 레지스트이기 때문에 포지티브형에 비해 박리가 어려워 강력한 박리성능이 요구되었다. 이러한 강력한 박리성능을 얻기 위해서 높은 pH를 갖도록 유기계 또는 무기계 박리액이 제안되어 있다. 예를 들면, 유기계 박리액으로 한국공개특허공개 제2005-0006980호 및 일본특허 공개공보 소51-72503 및 유럽특허 공보 제 0119337호에 개시되어 있다.Since the conventional process is generally a negative type resist, it is difficult to peel off from the positive type and strong peeling performance is required. In order to obtain such a strong peeling performance, an organic or inorganic peeling solution has been proposed to have a high pH. For example, Korean Patent Laid-Open Publication No. 2005-0006980, Japanese Patent Laid-Open Publication No. 51-72503, and European Patent Publication No. 0119337 disclose an organic peeling solution.
하지만, 상기 유기계 박리액의 경우 높은 pH로 인해 하부의 무기절연막 및 금속배선에 심각한 손상을 초래할 수 있으며, pH를 낮추기 위해 약한 알칼리 화합물을 적용할 경우 금속배선에는 손상을 주지 않지만 유기절연막이 제거되지 않는 문제점이 있다.However, in the case of the organic peeling solution, a high pH may seriously damage the lower inorganic insulating film and the metal wiring. When the weak alkaline compound is applied to lower the pH, the organic insulating film is not removed, There is no problem.
또한, 포지티브 및 네가티브 유기절연막의 경우 기존에 일반적으로 사용되며 한국공개특허 제1998-0003889 호에서 개시된 엘시디용 레지스트 박리액이 있다. G하지만, 상기 방법은 장시간 처리하여도 잔막이 존재하고 있으며, 녹지 않고 액 중 부유하는 현상이 관찰되었다.Further, in the case of positive and negative organic insulating films, there is a resist stripping solution for LCD, which has been generally used and disclosed in Korean Patent Laid-Open No. 1998-0003889. G However, the above method has a residual film even after prolonged treatment, and a phenomenon of floating in a liquid without melting has been observed.
이와 같이, 종래의 칼라레지스트 및 폴리이미드 또는 유기절연막 제거방법으로는 안정적으로 대량의 칼라레지스트 및 폴리이미드 또는 유기절연막을 제거하는 것이 곤란하거나, 하부막질의 손상이 심하여 기판의 재사용이 불가능하며, 생산성 또는 수율이 떨어지는 문제점이 있다.As described above, in the conventional color resist and polyimide or organic insulating film removing method, it is difficult to stably remove a large amount of color resist and polyimide or organic insulating film, or the damage of the lower film is severe and the substrate can not be reused. Or the yield is low.
따라서, 칼라레지스트 및 폴리이미드 또는 유기절연막를 안전한 방법을 통해 대량으로 제거하는 방법이 요구되고 있는 실정이다.Therefore, there is a demand for a method of removing a large amount of color resist and polyimide or organic insulating film through a safe method.
본 발명은 상기한 종래 문제점을 해결하기 위하여, 티에프티 엘시디의 제조공정 중에 사용되는 칼라레지스트 및 폴리이미드 또는 유기절연막을 안전하게 다량으로 제거하기 위한 박리액 조성물을 제공하는 것을 목적으로 한다.SUMMARY OF THE INVENTION It is an object of the present invention to provide a release liquid composition for removing a large amount of color resist and polyimide or organic insulation film safely used in the manufacturing process of TiFTC.
상기 목적을 달성하기 위하여, 본 발명은In order to achieve the above object,
(a) 암모늄 하이드록사이드 또는 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드 화합물 0.5 내지 15 중량부; (b) 탄소수 1 내지 4의 알킬기를 갖는 알킬렌글리콜에테르 9 내지 89 중량부; (c) 글리콜 화합물 10 내지 40 중량부; (d) 부식방지제 0.01 내지 5 중량부; 및 (e) 물 0.1 내지 5 중량부를 포함하는 것을 특징으로 하는, 박리액 조성물을 제공한다.(a) 0.5 to 15 parts by weight of ammonium hydroxide or an alkylammonium hydroxide compound having an alkyl group having 1 to 4 carbon atoms; (b) 9 to 89 parts by weight of an alkylene glycol ether having an alkyl group having 1 to 4 carbon atoms; (c) 10 to 40 parts by weight of a glycol compound; (d) 0.01 to 5 parts by weight of a corrosion inhibitor; And (e) 0.1 to 5 parts by weight of water.
상기 박리액 조성물은 전체 조성물 100 중량부에 대하여 극성용제 1 내지 50 중량부를 더 포함할 수 있다.The release liquid composition may further comprise 1 to 50 parts by weight of a polar solvent based on 100 parts by weight of the total composition.
이하에서 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 종래보다 칼라레지스트 및 폴리이미드 또는 유기절연막의 재사용하기 위한 연구를 거듭한 결과, 특정 조성을 가진 박리액 조성물을 이용하면 하부막질에 손상을 주지 않으면서 칼라레지스트 및 폴리이미드 또는 유기절연막의 용이하게 제거할 수 있음을 발견하고 본 발명을 완성하기에 이르렀다.As a result of repeated researches for reusing a color resist and a polyimide or an organic insulating film than the conventional one, it has been found that the use of a release liquid composition having a specific composition is advantageous in that a color resist and polyimide or an organic insulating film And the present invention has been accomplished.
이러한 본 발명의 박리액 조성물은 (a) 암모늄 하이드록사이드 또는 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드 화합물; (b) 탄소수 1 내지 4의 알킬기를 갖는 알킬렌글리콜에테르; (c) 글리콜 화합물; (d) 부식방지제; 및 (e) 물을 포함한다. 특히, 본 발명의 조성물은 기존보다 물의 함량을 최소한으로 사용하여도 우수한 제거효과를 나타낼 수 있다.Such a releasing solution composition of the present invention comprises (a) ammonium hydroxide or an alkylammonium hydroxide compound having an alkyl group having 1 to 4 carbon atoms; (b) an alkylene glycol ether having an alkyl group having 1 to 4 carbon atoms; (c) a glycol compound; (d) a corrosion inhibitor; And (e) water. In particular, the composition of the present invention can exhibit an excellent removal effect even when the water content is minimized.
본 발명의 박리액 조성물에 사용되는 하이드록사이드 화합물은 암모늄 하이드록 사이드 또는 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드를 사용할 수 있으며, 바람직하게는 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드를 사용한다. 상기 하이드록사이드 화합물의 함량은 전체 조성물에 대하여 0.5 내지 15 중량부로 사용하는 것이 바람직하며, 그 함량이 0.5 중량부 미만이면 폴리이미드를 구성하는 고분자 성분으로의 침투 능력이 떨어져 폴리이미드를 완전하게 제거하기 어렵고, 15 중량부를 초과하면 기타 용제의 성분 비율이 떨어져 오히려 제거 시간이 길어지는 악영향을 끼치게 된다.The hydroxide compound used in the release agent composition of the present invention may be ammonium hydroxide or an alkylammonium hydroxide having an alkyl group having 1 to 4 carbon atoms, preferably an alkylammonium salt having an alkyl group having 1 to 4 carbon atoms Hydroxides are used. The content of the hydroxide compound is preferably 0.5 to 15 parts by weight based on the total composition. If the amount of the hydroxyl compound is less than 0.5 part by weight, penetration into the polymer component constituting the polyimide is poor and the polyimide is completely removed If the amount is more than 15 parts by weight, the component ratio of the other solvent is lowered, and the removal time becomes longer.
상기 탄소수 1 내지 4의 알킬기를 갖는 알킬 암모늄 하이드록사이드는 테트라에틸 암모늄 하이드록사이드(tetraethyl ammonium hydroxide), 테트라메틸 암모늄 하이드록사이드(tetramethyl ammonium hydroxide), 테트라부틸 암모늄 하이드록사이드(tetrabutyl ammonium hydroxide), 및 이들의 혼합물로 이루어진 군으로부터 선택되는 것이 바람직하다.The alkylammonium hydroxide having an alkyl group having 1 to 4 carbon atoms is preferably selected from the group consisting of tetraethyl ammonium hydroxide, tetramethyl ammonium hydroxide, tetrabutyl ammonium hydroxide, , And a mixture thereof.
또한, 상기 탄소수 1 내지 4의 알킬기를 갖는 알킬렌 글리콜 에테르(alkyleneglycol ether)는 칼라레지스트 또는 유기절연막에 대한 용해력과 표면 장력을 저하시키는 능력이 뛰어나서 들떠있는 고분자와 유리면 사이에 작용하는 표면장력을 저하시켜 손쉽게 열경화성 수지가 박리되도록 한다. 또한, 상기 알킬렌 글리콜 에테르는 박리된 열경화성수지의 바인더나 폴리머 등을 용해하는 기능을 한다. 상기 알킬렌 글리콜 에테르의 사용량은 전체 조성물에 대하여 잔량으로 포함되며, 바람직하게 9 내지 89 중량부가 사용될 수 있다. 이때 그 함량이 9 중량부 미만이면 들떠있는 폴리이미드가 완전히 제거하기 어렵고, 89 중량부를 초과하면 박리액의 극성이 떨어져 칼라레지스트 또는 유기절연막의 고분자 재료인 아크릴 수지나 폴리이미드 수지를 용해하는 성능이 떨어져 막질이 액중에서 부유하는 단점이 있다. 본 발명에서 사용하는 알킬렌 글리콜 에테르는 에틸렌글리콜모노부틸에테르(ethyleneglycol monobutylether), 디에틸렌글리콜모노부틸에테르(diethylene glycol monobutylether), 트리에틸렌글리콜모노부틸에테르(triethyleneglycol monobutylether), 에틸렌글리콜모노메틸에테르(ethyleneglycol monomethylether), 디에틸렌글리콜모노메틸에테르(diethyleneglycol monomethylether), 트리에틸렌글리콜모노메틸에테르(triethyleneglycol monomethylether), 에틸렌글리콜모노에틸에테르(ethyleneglycol monoethylether) 및 이들의 혼합물로 이루어진 군으로부터 선택되는 것을 사용하는 것이 바람직하다.The alkyleneglycol ether having an alkyl group having 1 to 4 carbon atoms is excellent in the ability to dissolve the color resist or the organic insulating film and to lower the surface tension, thereby lowering the surface tension acting between the excited polymer and the glass surface So that the thermosetting resin is easily peeled off. The alkylene glycol ether functions to dissolve the binder, the polymer, and the like of the peeled thermosetting resin. The amount of the alkylene glycol ether to be used is included as a balance with respect to the total composition, preferably 9 to 89 parts by weight. If the content is less than 9 parts by weight, the exfoliating polyimide is difficult to completely remove. If the amount exceeds 89 parts by weight, the polarity of the exfoliating liquid is lowered and the performance of dissolving the acrylic resin or polyimide resin as the polymer material of the color resist or the organic insulating film There is a disadvantage that it floats off in the liquid. The alkylene glycol ethers used in the present invention include ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, triethyleneglycol monobutyl ether, ethyleneglycol monomethyl ether, it is preferable to use one selected from the group consisting of monomethylether, diethyleneglycol monomethylether, triethyleneglycol monomethylether, ethyleneglycol monoethylether and mixtures thereof .
또한, 상기 글리콜 화합물은 스트리퍼의 린스 능력을 향상시키는 역할을 한다. 상기 글리콜 화합물의 사용량은 전체 조성물에 대하여 10 내지 40 중량부로 사용할 수 있으며, 그 함량이 10 중량부 미만인 경우 린스 능력을 저하시키는 문제가 있고, 40 중량부를 초과하면 스트립 능력을 저하시키는 문제가 있다. 상기 글리콜 화합물로는 에틸렌 글리콜, 메틸렌 글리콜, 부틸렌글리콜 및 테트라에틸렌글리콜로 이루어진 군에서 선택되는 1종 이상을 사용할 수 있다. In addition, the glycol compound serves to improve the rinsing ability of the stripper. The amount of the glycol compound used may be 10 to 40 parts by weight based on the total composition. When the content is less than 10 parts by weight, the rinsing ability is lowered. When the amount is more than 40 parts by weight, the stripping ability is lowered. The glycol compound may be at least one selected from the group consisting of ethylene glycol, methylene glycol, butylene glycol, and tetraethylene glycol.
또한, 본 발명에서 부식방지제는 기판 금속층(Substrate metal layer)의 부식억제 역할을 한다. 상기 부식방지제의 함량은 전체 조성물에 대하여, 0.01 내지 5 중량부로 사용하며, 그 함량이 0.01 중량부 미만이면 부식억제효과 저하 문제가 있고, 5 중량부를 초과하면 린스 능력을 저하시키는 문제가 있다. 상기 부식방지제의 예를 들면, 아스코르브산, 벤질 트리아졸, 카테콜, 톨릴 트리아졸 및 이들의 혼합물로 이루어진 군에서 선택되는 것을 사용할 수 있다.In addition, in the present invention, the corrosion inhibitor plays a role of inhibiting the corrosion of the substrate metal layer. The corrosion inhibitor is used in an amount of 0.01 to 5 parts by weight based on the total composition. When the content is less than 0.01 part by weight, the corrosion inhibiting effect deteriorates. When the content is more than 5 parts by weight, the rinsing ability is deteriorated. Examples of the corrosion inhibitor include ascorbic acid, benzyltriazole, catechol, tolyltriazole, and mixtures thereof.
또한, 본 발명은 물의 사용량을 최소한으로 줄여 이전에 사용하였던 물의 역할을 탈피할 수 있다. 즉, 종래에는 일반적으로 물의 사용량이 많았지만, 본 발명은 특정함량의 하이드록사이드 와 부식방지제의 사용으로 최소한의 물의 양으로도 수지의 제거 및 부식방지의 효과를 극대화할 수 있다. 따라서, 본 발명에서는 물의 사용량을 전체 조성물에 1 내지 5 중량부로 사용할 수 있다. 상기 물의 함량이 1 중량부 미만이면 하이드록사이드의 활성도가 떨어져 공정시간 및 박리시간이 길어지며, 5 중량부를 초과하면 부식방지의 효과를 볼 수 없어 하부막 공정을 재사용 하는대 손실을 줄 수 있다. 또한, 본 발명에서 사용하는 물은 일반적으로 비저항이 18 (MΩ) 이상인 것을 사용한다.Further, the present invention can reduce the amount of water to be used to a minimum, thereby avoiding the previously used water. That is, although the amount of water used in the past is generally large, the present invention can maximize the effect of removing the resin and preventing corrosion even with a minimum amount of water by using a specific amount of the hydroxide and the corrosion inhibitor. Accordingly, in the present invention, the amount of water used may be 1 to 5 parts by weight based on the total composition. If the content of the water is less than 1 part by weight, the activity of the hydroxide is lowered and the process time and the peeling time are prolonged. If the water content is more than 5 parts by weight, the corrosion prevention effect can not be obtained. The water used in the present invention generally has a resistivity of 18 (M?) Or more.
또한, 본 발명의 조성물은 극성용제를 더 포함할 수 있다. 상기 극성용제는 폴리이미드에 대한 침투력과 용해력이 뛰어나서 폴리이미드의 고분자 사이에 침투하여 팽윤현상을 일으킨다. 극성용제의 사용량은 전체 조성물 100 중량부에 대하여 1 내지 50 중량부가 바람직하며, 이때 그 함량이 1 중량부 미만이면 폴리이미드를 완전하게 제거하는데 현저히 시간이 늘어나고, 50 중량부를 초과하면 무기 알칼리 하이드록사이드 화합물과의 용해도를 저하하여 성능 향상이 기대되지 않는다. 본 발명에서 사용하는 극성용제는 디메틸설폭사이드(dimethylsulfoxide), 디에틸설폭사이드(diethylsulfoxide), 디프로필설폭사이드(dipropylsulfoxide), 설포란(sulfolane), n-메틸피롤리돈(N-Methyl-2-pyrrolidone), 피롤리돈(pyrrolidone), n-에틸피롤리돈(n-ethyl pyrrolidone) 및 이들의 혼합물로 이루어진 군으로부터 선택되는 것을 사용하는 것이 바람직하다.In addition, the composition of the present invention may further comprise a polar solvent. The polar solvent is excellent in penetration and dissolution power against polyimide, and penetrates between the polymers of polyimide to cause a swelling phenomenon. The amount of the polar solvent to be used is preferably 1 to 50 parts by weight based on 100 parts by weight of the total composition. If the amount is less than 1 part by weight, a considerable amount of time is required to completely remove the polyimide. When the amount is more than 50 parts by weight, The solubility with the side compound is lowered and the performance improvement is not expected. The polar solvent used in the present invention may be selected from the group consisting of dimethylsulfoxide, diethylsulfoxide, dipropylsulfoxide, sulfolane, N -methyl-2- pyrrolidone, pyrrolidone, n-ethyl pyrrolidone, and mixtures thereof. It is preferred to use a compound selected from the group consisting of pyrrolidone, pyrrolidone, n-ethyl pyrrolidone and mixtures thereof.
또한, 본 발명의 박리액 조성물의 제조방법은 본 발명이 속하는 기술분야에서 통상의 지식을 가진자에 의해 제조 가능하며, 그 방법이 특별히 한정되지는 않는다. 또한, 본 발명의 박리액 조성물은 일반적인 티에프티 엘시디 제조공정의 열경화성 수지인 칼라레지스트 및 폴리이미드 또는 유기절연막의 제거공정에 사용될 수 있다.The method for producing the release liquid composition of the present invention can be manufactured by a person having ordinary skill in the art to which the present invention belongs, and the method thereof is not particularly limited. In addition, the release liquid composition of the present invention can be used in a process of removing a color resist, a polyimide or an organic insulating film, which is a thermosetting resin in a general TiFTiCyDi manufacturing process.
이상과 같이, 본 발명의 박리액 조성물은 각 성분들의 상승효과에 의해 칼라레지스트 및 유기절연막를 단시간내에 쉽게 제거할 수 있으며 폴리이미드 기판를 재사용할 수 있도록 하므로, 경제적인 이점이 있다.As described above, the peeling liquid composition of the present invention can easily remove the color resist and the organic insulating film in a short time due to the synergistic effect of each component, and it is possible to reuse the polyimide substrate, which is economically advantageous.
이하 본 발명을 하기 실시예를 참조로 하여 보다 상세히 설명한다. 이들 실시예는 본 발명을 예시하기 위한 것일 뿐, 본 발명의 범위가 하기 실시예에 의하여 한정되는 것이 아님은 물론이다. 하기 실시예에 있어서 별도의 언급이 없으면 백분율 및 혼합비는 중량을 기준으로 한 것이다.Hereinafter, the present invention will be described in more detail with reference to the following examples. It is to be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. In the following examples, percentages and mixing ratios are based on weight unless otherwise specified.
[실시예 1-13 및 비교예 1-4][Examples 1-13 and Comparative Examples 1-4]
하기 표 1 및 2에 나타낸 비율로 각 성분을 혼합하여 각각 실시예 및 비교예의 칼라 레지스트 박리액 조성물을 제조하였다.(단위: 중량부)The respective components were mixed in the ratios shown in Tables 1 and 2 to prepare color resist stripping liquid compositions of Examples and Comparative Examples, respectively (unit: parts by weight)
[표 1][Table 1]
[표 2] [Table 2]
주) 상기 표 1 및 2에서,Note) In Tables 1 and 2 above,
(a): 하이드록사이드 화합물, (b): 알킬렌글리콜에테르, (c): 글리콜 (a): a hydroxyl compound, (b) an alkylene glycol ether, (c) a glycol
(d): 부식방지제, (e): 물, (f): 극성용제, (g) 아민류(d): corrosion inhibitor, (e): water, (f): polar solvent, (g)
TMAH: 테트라메틸암모늄하이드록사이드TMAH: tetramethylammonium hydroxide
MDG : 디에틸렌글리콜 메틸에테르MDG: diethylene glycol methyl ether
EG : 에틸렌글리콜 MEA: 모노에탄올아민EG: ethylene glycol MEA: monoethanolamine
ASA: 아스코르브산(Ascorbic acid)ASA: Ascorbic acid
BT: 벤질 트리아졸 TT: 톨릴 트리아졸BT: benzyltriazole TT: tolyltriazole
[실험예][Experimental Example]
상기 실시예 1-13 및 비교예 1-4에서 제조한 칼라레지스트 박리액 조성물에 대한 성능평가를 위해, 하기 공정의 칼라 필터 기판을 사용하여 다음과 같이 열경화성수지 제거 실험을 실시하였다.In order to evaluate the performance of the color resist stripping composition prepared in Examples 1-13 and 1-4, a thermosetting resin removing test was carried out as follows using a color filter substrate.
1. 시편 제조1. Specimen Manufacturing
(1) 시편 1(1) Psalm 1
하부에 Mo/Al/Mo 다중막이 증착되어 있고 패턴까지 만들어져 있는 글래스에 폴리이미드(PI)를 만들고, 범용적으로 사용되는 칼라 레지스트 조성물 (동진쎄미켐 사제, 상품명: DCR-725S)을 스핀 코팅하여 최종 막두께가 1.7 ㎛가 되도록 도포하였다. 이어서, 핫 플레이트에서 상기 레지스트막을 90 ℃에서 120초간 프리베이크(pre-bake)하였다. 계속해서, 노광하고 1% 수산화칼륨(KOH) 현상액으로 상온에서 60초 현상한 후, 상기 패턴이 형성된 시편을 220 ℃의 오븐에서 20분간 하드 베이크(hard-bake)하여 시편 1을 제조하였다.A polyimide (PI) was formed on a glass having a pattern of Mo / Al / Mo multilayer deposited thereon, and a color resist composition (DCR-725S, trade name: DCR-725S available from Dongjin Semichem Co., Ltd.) So as to have a film thickness of 1.7 mu m. Subsequently, the resist film was pre-baked on a hot plate at 90 DEG C for 120 seconds. Subsequently, the resist film was exposed to light and developed with 1% potassium hydroxide (KOH) developer at room temperature for 60 seconds. Then, the patterned specimen was hard-bake in an oven at 220 ° C for 20 minutes to prepare specimen 1.
(2) 시편 2(2) Psalm 2
또한, 폴리이미드가 도포된 시편을 만들기 위해, 하부에 Mo/Al/Mo 다중막이 증착되어 있고 패턴까지 만들어져 있는 글래스에 유기절연막 조성물(동진쎄미켐 사제, 상품명 SOJN-091)을 스핀코팅하여 최종 막두께가 4.0 ㎛가 되도록 도포하였다. 이어서, 핫 플레이트에서 상기 폴리이미드를 90 ℃에서 120 초간 소프트 베이크(soft-bake)를 실시하였다. 계속해서, 노광하고 2.38% TMAH 현상액으로 상온에서 70초 현상 후 전면 노광을 실시하고, 130 ℃에서 3분간 하드베이크 하여 시편 2를 제조하였다.In order to make polyimide-coated specimens, an organic insulating film composition (product name: SOJN-091, manufactured by Dongjin Semichem Co., Ltd.) was spin-coated on a glass substrate having a Mo / Al / Was 4.0 占 퐉. Then, the polyimide was subjected to soft-bake at 90 DEG C for 120 seconds on a hot plate. Subsequently, the resist film was exposed to light, developed with 2.38% TMAH developer for 70 seconds at room temperature, and then subjected to a front exposure, and hard baked at 130 캜 for 3 minutes to prepare a test piece 2.
2. 제거 시험2. Removal test
(1) 제거시간 비교 시험(1) Removal time comparative test
상기 제조된 시편 1 및 2에 대하여 온도 70 ℃에서 칼라 레지스트 제거 및 폴리이미드 재료 제거를 위한 박리액 조성물에 침지하여 기판에서 칼라레지스트 또는 유기절연막이 완전히 박리되는 시간을 측정하였다. 계속하여, 상기 시편 1을 칼라레지스트 박리액 조성물로부터 꺼낸 후, 초순수로 수세하고 질소가스로 건조하고, 패턴내에 칼라레지스트가 잔류하는지 여부를 올림푸스 현미경으로 100배로 확대하여 검사하여 칼라 레지스트가 기판내 잔류하는지의 여부를 관찰하였다.The prepared specimens 1 and 2 were immersed in a peeling liquid composition for removing the color resist and removing the polyimide material at a temperature of 70 ° C to measure the time for completely peeling the color resist or the organic insulating film from the substrate. Subsequently, the specimen 1 was taken out from the color resist stripper composition, rinsed with ultrapure water, dried with nitrogen gas, and examined whether the color resist remained in the pattern was magnified 100 times with an Olympus microscope, Were observed.
(2) Al 막질 손상 정도 비교 시험(2) A comparative test of the degree of Al film damage
하부막질의 손상 여부를 관찰하기 위해 각 박리액 조성물에 칼라레지스트가 도포된 시편을 30분간 침지하여 SEM으로 손상 여부를 관찰하였다.In order to observe the damage of the lower film, the specimen coated with the color resist was dipped in each stripper solution for 30 minutes, and the damage was observed by SEM.
하기 표 3은 유기절연막재료 및 칼라레지스트가 완전히 박리되어 잔사가 발견되지 않는 시간을 측정하여 나타낸 결과이다.Table 3 below shows the results of measuring the time when the organic insulating film material and the color resist are completely peeled off and no residue is found.
[표 3][Table 3]
손상 정도Al film
Degree of damage
(폴리이미드)Psalm 1
(Polyimide)
(유기절연막)Psalm 2
(Organic insulating film)
주) 상기 표 3에서, < X : 배선이 완전히 없어짐, △ : Al 의 심각한 손상, ○ : 표면 피팅(Pitting) 발생, ◎ : 전혀 손상 없음>Note: In Table 3, < X: wiring completely disappeared,?: Serious damage of Al,?: Surface firing (Pitting)
상기 표 3에서 알 수 있듯이, 본원의 실시예는 칼라레지스트 제거성능 및 유기절연막의 제거 성능이 뛰어날 뿐만 아니라 하부막질의 손상이 전혀 없는 것을 알 수 있다. 또한, 본 발명은 부식방지제 및 하이드록실아민 등의 주요 성분들이 없는 비교예에 비해 칼라레지스트 제거 성능 및 부식방지 성능이 매우 우수함을 알 수 있다.As can be seen from Table 3, the embodiment of the present invention shows not only excellent performance of removing a color resist, removal performance of an organic insulating film, but also damage of the underlying film at all. In addition, it can be seen that the present invention has excellent color resist removal performance and corrosion prevention performance as compared with the comparative example in which no major components such as a corrosion inhibitor and a hydroxylamine are present.
본 발명에 따른 박리액 조성물은 칼라 레지스트 및 유기절연막을 짧은 시간 내에 용이하게 제거할 수 있으며, 후속의 린스 공정에서 이소프로필알콜, 디메틸설폭사이드와 같은 유기용제를 사용할 필요 없이 물만으로 린스할 수 있는 장점이 있고, 특히 레지스트 패턴의 제거가 가능하여 기판을 재사용할 수 있다.The peeling liquid composition according to the present invention can easily remove the color resist and the organic insulating film in a short time and can easily rinse with water without using an organic solvent such as isopropyl alcohol or dimethyl sulfoxide in a subsequent rinsing process In particular, the resist pattern can be removed and the substrate can be reused.
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