KR102246300B1 - Rinse Compositon for Process of Manufacturing Semiconductor and Display - Google Patents
Rinse Compositon for Process of Manufacturing Semiconductor and Display Download PDFInfo
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- KR102246300B1 KR102246300B1 KR1020210036156A KR20210036156A KR102246300B1 KR 102246300 B1 KR102246300 B1 KR 102246300B1 KR 1020210036156 A KR1020210036156 A KR 1020210036156A KR 20210036156 A KR20210036156 A KR 20210036156A KR 102246300 B1 KR102246300 B1 KR 102246300B1
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/2082—Polycarboxylic acids-salts thereof
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Abstract
Description
본 발명은 반도체 및 디스플레이 제조공정용 세정제 조성물에 대한 것으로, 보다 상세하게는 기판의 부식을 방지할 수 있으며, 금속 오염물을 제거할 뿐만 아니라 파티클의 재부착을 방지할 수 있는, 반도체 및 디스플레이 제조공정용 세정제 조성물에 관한 것이다.The present invention relates to a cleaning agent composition for a semiconductor and display manufacturing process, and more particularly, can prevent corrosion of a substrate, remove metal contaminants, as well as prevent re-adhesion of particles, a semiconductor and display manufacturing process It relates to a cleaning agent composition.
정보화 기술의 급속한 진전에 따라 대규모 집적회로(LSI, ULSI, VLSI)의 미세화, 고밀도화, 고집적화가 이루어지고, 배선의 다층화에 의한 기술개발이 행해지고 있다. 배선의 다층화를 달성하기 위해서는 배선 피치폭의 축소 및 배선간 용량의 저감 등을 행하는 것이 필요로 되고, 이를 위해 최근에는 저항률이 낮은 구리(Cu)를 배선재료로 사용하고 있다.With the rapid progress of information technology, large-scale integrated circuits (LSI, ULSI, VLSI) have been miniaturized, high-densified, and highly integrated, and technology development is being carried out by multi-layered wiring. In order to achieve a multilayered wiring, it is necessary to reduce the wiring pitch width and the capacity between wirings, and for this purpose, recently, copper (Cu) having a low resistivity is used as a wiring material.
반도체 장치의 제조과정에 발생하는 파티클, 금속원자, 유기물 등의 오염을 제거하여 장치의 신뢰성을 향상시키기 위하여 세정과정을 거친다. 이러한 세정과정 중에서는 구리가 부식되거나 역흡착되는 문제가 있는데 이러한 문제를 방지하면서 파티클이나 유기 오염물질을 제거하는 기능을 향상시키는 것은 종래 세정제 조성물로서는 달성하기 어려운 문제이다.A cleaning process is performed to improve the reliability of the device by removing contamination of particles, metal atoms, organic substances, etc. generated in the manufacturing process of a semiconductor device. There is a problem in that copper is corroded or adsorbed backwards in the cleaning process. However, improving the function of removing particles or organic contaminants while preventing such a problem is a problem that is difficult to achieve with the conventional cleaning composition.
이에 따라서 금속 오염물과 파티클을 제거하고 구리 부식을 방지하는 것과 함께 역흡착을 방지할 수 있는 pH 8 내지 13의 알칼리 수계의 세정제 조성물이 제안되고 있지만, 이 조성물은 유기 파티클 제거능력과 특정 막질의 무기 파티클 제거능력이 떨어지는 문제가 여전히 존재하고 있다.Accordingly, an alkaline aqueous detergent composition having a pH of 8 to 13 has been proposed that can remove metal contaminants and particles, prevent copper corrosion, and prevent reverse adsorption, but this composition has organic particle removal ability and specific film quality inorganic The problem of poor particle removal still exists.
대한민국공개특허공보 제10-2016-0092128호(2016.08.04.)에는 반도체 및 디스플레이 제조공정용 세정제 조성물이 개시되어 있다.Korean Laid-Open Patent Publication No. 10-2016-0092128 (2016.08.04.) discloses a cleaning agent composition for a semiconductor and display manufacturing process.
상기 반도체 및 디스플레이 제조공정용 세정제 조성물은 금속 오염물 및 유·무기 파티클을 동시에 제거하는 장점이 있지만 파티클의 재부착을 방지할 수 있는 기능이 미흡한 단점이 있다. The cleaning agent composition for semiconductor and display manufacturing processes has the advantage of simultaneously removing metal contaminants and organic/inorganic particles, but has a disadvantage in that the function of preventing re-adhesion of particles is insufficient.
본 발명의 목적은 금속 오염물을 제거할 뿐만 아니라 파티클의 재부착을 방지할 수 있는, 반도체 및 디스플레이 제조공정용 세정제 조성물을 제공하는 것이다. An object of the present invention is to provide a cleaning agent composition for semiconductor and display manufacturing processes, which can prevent re-adhesion of particles as well as removing metal contaminants.
본 발명의 다른 목적은 기판의 부식을 방지할 수 있는, 반도체 및 디스플레이 제조공정용 세정제 조성물을 제공하는 것이다.Another object of the present invention is to provide a cleaning agent composition for semiconductor and display manufacturing processes that can prevent corrosion of a substrate.
상기 목적을 달성하기 위하여 본 발명은 다음과 같은 수단을 제공한다.In order to achieve the above object, the present invention provides the following means.
본 발명은, 에틸렌디아민테트라아세트산(ethylenediaminetetraacetic acid) 1~5중량%, 락트산 알킬 에스테르(lactic acid alkyl ester) 0.1~1중량%, 디이소프로판올아민 1~5중량%, 과산화수소 0.1~1중량%, 폴리스티렌술폰산 0.1~1중량%, 테트라에틸암모늄 하이드록사이드(tetraethylammonium hydroxide) 0.1~1중량%, 폴리옥시에틸렌노닐페닐에테르 1~5중량%, 폴리옥시부틸렌 실록산 1~3중량% 및 초순수 80~85중량%를 포함하는, 반도체 및 디스플레이 제조공정용 세정제 조성물을 제공한다.The present invention, ethylenediaminetetraacetic acid (ethylenediaminetetraacetic acid) 1-5% by weight, lactic acid alkyl ester (lactic acid alkyl ester) 0.1-1% by weight, diisopropanolamine 1-5% by weight, hydrogen peroxide 0.1-1% by weight, polystyrene 0.1 to 1% by weight of sulfonic acid, 0.1 to 1% by weight of tetraethylammonium hydroxide, 1 to 5% by weight of polyoxyethylene nonylphenyl ether, 1 to 3% by weight of polyoxybutylene siloxane, and 80 to 85 of ultrapure water It provides a cleaning agent composition for a semiconductor and display manufacturing process, including weight percent.
상기 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 세정력향상제 0.1~1중량부를 추가적으로 포함하되, 상기 세정력향상제는 불화테트라메틸암모늄 40~50중량%, 디에틸렌글리콜모노메틸에테르 20~30중량%, 디메틸아세트아미드 10~20중량%, 석신산(succinic acid) 10~20중량% 및 트리플루오로아세트산(trifluoroacetic acid) 1~5중량%를 포함한다.An additional 0.1 to 1 part by weight of a cleaning power improving agent is included in 100 parts by weight of the cleaning composition for the semiconductor and display manufacturing process, wherein the cleaning power improving agent is 40-50% by weight of tetramethylammonium fluoride, 20-30% by weight of diethylene glycol monomethyl ether, Dimethylacetamide 10-20 wt%, succinic acid 10-20 wt%, and trifluoroacetic acid 1-5 wt%.
상기 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 부식방지제 0.1~1중량부를 추가적으로 포함하되, 상기 부식방지제는 벤조트리아졸(1,2,3-benzotriazol) 40~50중량%, 피로갈롤(Pyrogallol) 20~30중량%, 티오글리세롤 10~20중량%, 폴리아미노설폰 5~15중량% 및 5-아미노 테트라졸(5-amino-1H-Tetrazole) 0.1~1중량%를 포함한다.An additional 0.1 to 1 part by weight of a corrosion inhibitor is included in 100 parts by weight of the cleaning composition for the semiconductor and display manufacturing process, wherein the corrosion inhibitor is 40 to 50% by weight of benzotriazol, and Pyrogallol ) 20 to 30% by weight, 10 to 20% by weight of thioglycerol, 5 to 15% by weight of polyaminosulfone, and 0.1 to 1% by weight of 5-amino-tetrazole (5-amino-1H-Tetrazole).
상기 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 하부막보호제 0.1~1중량부를 추가적으로 포함하되, 상기 하부막보호제는 벤조트리졸(benzotrizole) 50~60중량%, 메틸 글리콜(methyl glycol) 20~30중량%, 메틸트리부틸암모늄 하이드록사이드 10~20중량% 및 히드로퀴논 1~5중량%를 포함한다.An additional 0.1 to 1 part by weight of a lower film protector is included in 100 parts by weight of the cleaning composition for the semiconductor and display manufacturing process, wherein the lower film protectant is 50 to 60% by weight of benzotrizole and 20 to of methyl glycol. 30 wt%, methyltributylammonium hydroxide 10-20 wt%, and hydroquinone 1-5 wt%.
상기 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 거품제거제 0.1~1중량부를 추가적으로 포함하되, 상기 거품제거제는 헥산올 50~60중량%, 폴리에틸렌글리콜 20~30중량%, 트리이소부틸포스페이트 10~20중량% 및 과불소화노난올(CF3(CF2)8OH) 1~5중량%를 포함한다. An additional 0.1 to 1 part by weight of a defoaming agent is included in 100 parts by weight of the cleaning composition for the semiconductor and display manufacturing process, wherein the defoaming agent is hexanol 50 to 60% by weight, polyethylene glycol 20 to 30% by weight, triisobutyl phosphate 10 to 20% by weight and perfluorinated nonanol (CF 3 (CF 2 ) 8 OH) 1-5% by weight.
상기 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 재흡착방지제 0.1~1중량부를 추가적으로 포함하되, 상기 재흡착방지제는 수산화세슘(Cesium hydroxide) 50~60중량%, 폴리옥시에틸렌도데실페닐에테르 20~30중량%, 테트라부틸암모늄 하이드록사이드(TBAH) 10~20중량%, 수산화칼륨(KOH) 1~5중량% 및 풀빅산 발효물 0.1~1중량%를 포함하며, 상기 풀빅산 발효물은 바이오세라믹 스톤 정제수 50~70중량%, 복합효소액 10~30중량% 및 풀빅산 분말 15~25중량%를 혼합한 혼합물을 20~25℃에서 72~74시간 동안 호기발효한 발효물을 사용하며, 상기 바이오세라믹 스톤 정제수는 물 100중량부에 바이오세라믹 스톤 1~5중량부를 넣고 10~14시간 동안 방치하여 수득하며, 상기 바이오세라믹 스톤은 진주석 40~50중량%, 견운모 25~35중량% 및 황토 20~30중량%를 포함하는 혼합물을 물에 넣고 혼련한 후 숙성시킨 다음, 1,300~1,400℃의 온도에서 1~2시간 동안 소성시키며, 상기 복합효소액은 효소활성보조제 100중량부에 미생물혼합균주 1~10중량부, 생리활성화물질 20~30중량부 및 부식산 1~5중량부를 포함하며, 상기 효소활성보조제는 육류 세척수 100중량부에 바실러스 낫토균 0.1~1중량부를 가하고 5~7일 동안 혐기 발효하고, 40~42일 동안 폭기하여 호기 발효하며, 상기 미생물혼합균주는 홍국균 40~50중량%, 고초균 20~30중량%, 효모 10~20중량% 및 누룩균 5~15중량%를 포함하며, 상기 생리활성화물질은 유기질 100중량부에 상기 효소활성보조제 1~5중량부 및 물 10~20중량부를 혼합 후 10~20일 동안 혐기 발효시킨 후, 1~3일 동안 호기 발효시킨 발효물질 100중량부에 물 500~600중량부를 넣어 2~5일 동안 폭기조에서 발효시킨 후 이를 정치 및 침전시켜 분리한 상등액을 사용한다.An additional 0.1 to 1 part by weight of a re-adsorption inhibitor is additionally included in 100 parts by weight of the cleaning composition for the semiconductor and display manufacturing process, wherein the re-adsorption inhibitor is 50 to 60% by weight of cesium hydroxide, polyoxyethylene dodecylphenyl ether 20 -30% by weight, tetrabutylammonium hydroxide (TBAH) 10-20% by weight, potassium hydroxide (KOH) 1-5% by weight and 0.1-1% by weight of fulvic acid fermented product, and the fulvic acid fermented product is A mixture of 50 to 70% by weight of purified bioceramic stone, 10 to 30% by weight of complex enzyme solution, and 15 to 25% by weight of fulvic acid powder is used as a fermented product aerobic fermented at 20 to 25°C for 72 to 74 hours, The bioceramic stone purified water is obtained by adding 1 to 5 parts by weight of bioceramic stone to 100 parts by weight of water and leaving it for 10 to 14 hours, and the bioceramic stone is 40 to 50% by weight of pearl stone, 25 to 35% by weight of sericite and A mixture containing 20 to 30% by weight of loess is put in water, kneaded, then aged, and then calcined at a temperature of 1,300 to 1,400°C for 1 to 2 hours, and the complex enzyme solution is a microorganism mixed strain in 100 parts by weight of an enzyme activity supplement. 1 to 10 parts by weight, 20 to 30 parts by weight of a physiologically active substance, and 1 to 5 parts by weight of humic acid, and the enzyme activity adjuvant is added 0.1 to 1 part by weight of Bacillus natto bacteria to 100 parts by weight of meat washing water for 5 to 7 days. Anaerobic fermentation, aeration for 40 to 42 days, aerobic fermentation, the microorganism mixture strain contains 40-50% by weight of honggukgyun, 20-30% by weight of Bacillus bacillus, 10-20% by weight of yeast, and 5-15% by weight of koji bacteria, , The physiologically activating material is 100 parts by weight of the organic substance, after mixing 1 to 5 parts by weight of the enzyme activation aid and 10 to 20 parts by weight of water, anaerobic fermentation for 10 to 20 days, and then aerobic fermentation for 1 to 3 days. Add 500 to 600 parts by weight of water, ferment in an aeration tank for 2 to 5 days, settle and settle, and use the separated supernatant.
본 발명에 따른 반도체 및 디스플레이 제조공정용 세정제 조성물은 금속 오염물을 제거할 뿐만 아니라 파티클의 재부착을 방지할 수 있는 장점이 있다. The cleaning agent composition for semiconductor and display manufacturing processes according to the present invention has the advantage of not only removing metal contaminants, but also preventing re-adhesion of particles.
본 발명의 반도체 및 디스플레이 제조공정용 세정제 조성물은 기판의 부식을 방지할 수 있는 장점이 있다.The cleaning agent composition for a semiconductor and display manufacturing process of the present invention has an advantage of preventing corrosion of a substrate.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
먼저, 본 발명에 따른 반도체 및 디스플레이 제조공정용 세정제 조성물을 설명한다.First, a cleaning agent composition for a semiconductor and display manufacturing process according to the present invention will be described.
본 발명의 반도체 및 디스플레이 제조공정용 세정제 조성물은,The detergent composition for a semiconductor and display manufacturing process of the present invention,
에틸렌디아민테트라아세트산(ethylenediaminetetraacetic acid) 1~5중량%, 락트산 알킬 에스테르(lactic acid alkyl ester) 0.1~1중량%, 디이소프로판올아민 1~5중량%, 과산화수소 0.1~1중량%, 폴리스티렌술폰산 0.1~1중량%, 테트라에틸암모늄 하이드록사이드(tetraethylammonium hydroxide) 0.1~1중량%, 폴리옥시에틸렌노닐페닐에테르 1~5중량%, 폴리옥시부틸렌 실록산 1~3중량% 및 초순수 80~85중량%를 포함한다.Ethylenediaminetetraacetic acid 1 to 5% by weight, lactic acid alkyl ester 0.1 to 1% by weight, diisopropanolamine 1 to 5% by weight, hydrogen peroxide 0.1 to 1% by weight, polystyrene sulfonic acid 0.1 to 1 Including wt%, tetraethylammonium hydroxide 0.1 to 1 wt%, polyoxyethylene nonylphenyl ether 1 to 5 wt%, polyoxybutylene siloxane 1 to 3 wt%, and ultrapure water 80 to 85 wt% do.
상기 에틸렌디아민테트라아세트산(ethylenediaminetetraacetic acid)는 금속 오염물을 제거시키는 역할을 수행한다.The ethylenediaminetetraacetic acid serves to remove metal contaminants.
상기 에틸렌디아민테트라아세트산(ethylenediaminetetraacetic acid)는 1~5중량% 포함되는 것이 바람직하며, 1중량% 미만 포함되면 금속 오염물 제거 효과가 떨어지는 문제가 있고, 5중량% 초과 포함되면 피세정물이 부식될 수 있다. The ethylenediaminetetraacetic acid (ethylenediaminetetraacetic acid) is preferably contained in 1 to 5% by weight, if it is contained less than 1% by weight, there is a problem that the effect of removing metal contaminants decreases, and if it is contained in excess of 5% by weight, the object to be cleaned may be corroded. have.
상기 락트산 알킬 에스테르(lactic acid alkyl ester)는 파티클을 제거시키는 역할을 수행한다.The lactic acid alkyl ester serves to remove particles.
상기 락트산 알킬 에스테르(lactic acid alkyl ester)는 0.1~1중량% 포함되는 것이 바람직하며, 0.1중량% 미만 포함되면 파티클 제거 효과가 떨어지는 문제가 있고, 1중량% 초과 포함되면 피세정물을 부식시킬 수 있는 문제가 있다.The lactic acid alkyl ester is preferably contained in an amount of 0.1 to 1% by weight, and if it is contained in less than 0.1% by weight, there is a problem that the particle removal effect is deteriorated, and if it is contained in an amount exceeding 1% by weight, the object to be cleaned may be corroded. There is a problem.
상기 디이소프로판올아민은 세정 효과를 상승시키는 역할을 수행한다.The diisopropanolamine serves to increase the cleaning effect.
상기 디이소프로판올아민은 1~5중량% 포함되는 것이 바람직하며, 1중량% 미만 포함되면 세정효과가 저하되는 문제가 있고, 5중량% 초과 포함되면 기판을 손상할 수 있는 문제가 있다. The diisopropanolamine is preferably contained in an amount of 1 to 5% by weight, and if it is contained in less than 1% by weight, there is a problem that the cleaning effect is deteriorated, and if it is contained in an amount exceeding 5% by weight, there is a problem that the substrate may be damaged.
상기 과산화수소는 금속불순물의 세정효과를 향상시키는 역할을 수행한다. The hydrogen peroxide serves to improve the cleaning effect of metallic impurities.
상기 과산화수소는 0.1~1중량% 포함되는 것이 바람직하며, 0.1중량% 미만 포함되면 금속불순물의 세정효과가 떨어지는 문제가 있고, 1중량% 초과 포함되면 금속을 부식시킬 수 있는 문제가 있다. The hydrogen peroxide is preferably contained in an amount of 0.1 to 1% by weight, and if it is contained in an amount of less than 0.1% by weight, there is a problem that the cleaning effect of metallic impurities is deteriorated, and if it is contained in more than 1% by weight, there is a problem that the metal may be corroded.
상기 폴리스티렌술폰산은 미립자 제거성을 향상시키는 역할을 수행한다.The polystyrene sulfonic acid serves to improve particulate removal.
상기 폴리스티렌술폰산은 0.1~1중량% 포함되는 것이 바람직하며, 0.1중량% 미만 포함되면 미립자 제거효과가 떨어지는 문제가 있고, 1중량% 초과 포함되면 피세정물을 부식시킬 수 있는 문제가 있다. The polystyrene sulfonic acid is preferably contained in an amount of 0.1 to 1% by weight, and if it is contained in less than 0.1% by weight, there is a problem in that the particle removal effect is inferior, and if it is contained in more than 1% by weight, there is a problem that the object to be cleaned may be corroded.
상기 테트라에틸암모늄 하이드록사이드(tetraethylammonium hydroxide)는 오염물에 대해 세정하는 역할을 수행한다.The tetraethylammonium hydroxide serves to cleanse contaminants.
상기 테트라에틸암모늄 하이드록사이드(tetraethylammonium hydroxide)는 0.1~1중량% 포함되는 것이 바람직하며, 0.1중량% 미만 포함되면 오염물에 대해 세정하는 효과가 떨어지는 문제가 있고, 1중량% 초과 포함되면 하부막에 대한 손상을 발생시킬 수 있다.The tetraethylammonium hydroxide is preferably contained in an amount of 0.1 to 1% by weight, and if it is contained less than 0.1% by weight, there is a problem that the cleaning effect for contaminants is inferior, and if it is contained in excess of 1% by weight, the lower film is It may cause damage to the.
상기 폴리옥시에틸렌노닐페닐에테르는 금속표면으로의 재흡착 방지 역할을 수행한다.The polyoxyethylene nonylphenyl ether serves to prevent re-adsorption to the metal surface.
상기 폴리옥시에틸렌노닐페닐에테르는 1~5중량% 포함되는 것이 바람직하며, 1중량% 미만 포함되면 금속표면으로의 재흡착 방지 효과가 떨어지는 문제가 있고, 5중량% 초과 포함되면 거품이 발생하는 문제가 발생될 수 있다.The polyoxyethylene nonylphenyl ether is preferably contained in 1 to 5% by weight, and if it is contained in less than 1% by weight, there is a problem that the effect of preventing re-adsorption to the metal surface decreases, and if it is contained in more than 5% by weight, foaming occurs. May occur.
상기 폴리옥시부틸렌 실록산은 거품을 제거하는 역할을 수행한다. The polyoxybutylene siloxane serves to remove bubbles.
상기 폴리옥시부틸렌 실록산은 1~3중량% 포함되는 것이 바람직하며, 1중량% 미만 포함되면 거품을 제거하는 효과가 떨어지는 문제가 있고, 3중량% 초과 포함되면 세정력을 떨어뜨리는 문제가 있다.The polyoxybutylene siloxane is preferably contained in an amount of 1 to 3% by weight, and if it is contained in less than 1% by weight, there is a problem that the effect of removing bubbles is inferior, and if it is contained in excess of 3% by weight, there is a problem of lowering the cleaning power.
상기 초순수는 80~85중량% 포함되는 것이 바람직하다. It is preferable that the ultrapure water is contained in an amount of 80 to 85% by weight.
물은 통상의 이온교환수지를 통한 초순수를 사용하는 것이 바람직하다. It is preferable to use ultrapure water through a conventional ion exchange resin.
본 발명은, 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 세정력향상제 0.1~1중량부를 추가적으로 포함할 수 있다. In the present invention, 0.1 to 1 part by weight of a cleaning power improving agent may be additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 세정력향상제는 금속 오염물 세정 효과를 더욱 향상시킬 수 있는 장점이 있다.The cleaning power improving agent has the advantage of further improving the cleaning effect of metal contaminants.
상기 세정력향상제는 불화테트라메틸암모늄 40~50중량%, 디에틸렌글리콜모노메틸에테르 20~30중량%, 디메틸아세트아미드 10~20중량%, 석신산(succinic acid) 10~20중량% 및 트리플루오로아세트산(trifluoroacetic acid) 1~5중량%를 포함한다.The cleaning power improving agent is tetramethylammonium fluoride 40-50% by weight, diethylene glycol monomethyl ether 20-30% by weight, dimethylacetamide 10-20% by weight, succinic acid 10-20% by weight, and trifluoro It contains 1 to 5% by weight of acetic acid (trifluoroacetic acid).
본 발명은, 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 부식방지제 0.1~1중량부를 추가적으로 포함할 수 있다. In the present invention, 0.1 to 1 part by weight of a corrosion inhibitor may be additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 부식방지제는 금속막 등의 금속을 부식시키지 않는 효과를 상승시키는 역할을 수행한다.The corrosion inhibitor serves to increase the effect of not corroding metal such as a metal film.
상기 부식방지제는 벤조트리아졸(1,2,3-benzotriazol) 40~50중량%, 피로갈롤(Pyrogallol) 20~30중량%, 티오글리세롤 10~20중량%, 폴리아미노설폰 5~15중량% 및 5-아미노 테트라졸(5-amino-1H-Tetrazole) 0.1~1중량%를 포함한다.The corrosion inhibitor is benzotriazole (1,2,3-benzotriazol) 40 to 50% by weight, pyrogallol (Pyrogallol) 20 to 30% by weight, thioglycerol 10 to 20% by weight, polyaminosulfone 5 to 15% by weight and 5-amino tetrazole (5-amino-1H-Tetrazole) 0.1 to 1% by weight is included.
본 발명은, 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 하부막보호제 0.1~1중량부를 추가적으로 포함할 수 있다. In the present invention, 0.1 to 1 part by weight of a lower film protector may be additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 하부막보호제는 하부막의 손상을 방지할 수 있는 효과를 상승시키는 역할을 수행한다.The lower layer protective agent serves to increase the effect of preventing damage to the lower layer.
상기 하부막보호제는 벤조트리졸(benzotrizole) 50~60중량%, 메틸 글리콜(methyl glycol) 20~30중량%, 메틸트리부틸암모늄 하이드록사이드 10~20중량% 및 히드로퀴논 1~5중량%를 포함한다.The lower film protective agent includes 50 to 60% by weight of benzotrizole, 20 to 30% by weight of methyl glycol, 10 to 20% by weight of methyltributylammonium hydroxide, and 1 to 5% by weight of hydroquinone do.
본 발명은, 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 거품제거제 0.1~1중량부를 추가적으로 포함할 수 있다. In the present invention, 0.1 to 1 part by weight of a foam remover may be additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 거품제거제는 계면활성제로 인한 거품을 제거하는 역할을 수행한다.The foam remover serves to remove foam caused by the surfactant.
상기 거품제거제는 헥산올 50~60중량%, 폴리에틸렌글리콜 20~30중량%, 트리이소부틸포스페이트 10~20중량% 및 과불소화노난올(CF3(CF2)8OH) 1~5중량%를 포함한다. The defoaming agent contains 50 to 60% by weight of hexanol, 20 to 30% by weight of polyethylene glycol, 10 to 20% by weight of triisobutyl phosphate, and 1 to 5% by weight of perfluorinated nonanol (CF 3 (CF 2 ) 8 OH) Includes.
본 발명은, 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 재흡착방지제 0.1~1중량부를 추가적으로 포함할 수 있다. The present invention may additionally include 0.1 to 1 part by weight of a re-adsorption inhibitor to 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 재흡착방지제는 세정 후 파티클(particle)의 재흡착을 방지하는 효과를 상승시키는 역할을 수행한다.The anti-readsorption agent serves to increase the effect of preventing re-adsorption of particles after washing.
상기 재흡착방지제는 수산화세슘(Cesium hydroxide) 50~60중량%, 폴리옥시에틸렌도데실페닐에테르 20~30중량%, 테트라부틸암모늄 하이드록사이드(TBAH) 10~20중량%, 수산화칼륨(KOH) 1~5중량% 및 풀빅산 발효물 0.1~1중량%를 포함한다.The re-adsorption inhibitor is cesium hydroxide (Cesium hydroxide) 50-60% by weight, polyoxyethylene dodecylphenyl ether 20-30% by weight, tetrabutylammonium hydroxide (TBAH) 10-20% by weight, potassium hydroxide (KOH) It contains 1 to 5% by weight and 0.1 to 1% by weight of fulvic acid fermented product.
상기 풀빅산 발효물은 바이오세라믹 스톤 정제수 50~70중량%, 복합효소액 10~30중량% 및 풀빅산 분말 15~25중량%를 혼합한 혼합물을 20~25℃에서 72~74시간 동안 호기발효한 발효물을 사용한다.The fulvic acid fermented product is a mixture of 50 to 70% by weight of purified bioceramic stone, 10 to 30% by weight of complex enzyme solution, and 15 to 25% by weight of fulvic acid powder by aerobic fermentation at 20 to 25°C for 72 to 74 hours. Use fermented products.
상기 바이오세라믹 스톤 정제수는 물 100중량부에 바이오세라믹 스톤 1~5중량부를 넣고 10~14시간 동안 방치하여 수득한다.The bioceramic stone purified water is obtained by adding 1 to 5 parts by weight of bioceramic stone to 100 parts by weight of water and leaving it for 10 to 14 hours.
상기 바이오세라믹 스톤은 진주석 40~50중량%, 견운모 25~35중량% 및 황토 20~30중량%를 포함하는 혼합물을 물에 넣고 혼련한 후 숙성시킨 다음, 1,300~1,400℃의 온도에서 1~2시간 동안 소성시켜 제조한다.The bioceramic stone is a mixture containing 40 to 50% by weight of pearlite, 25 to 35% by weight of silky mica, and 20 to 30% by weight of loess, mixed with water, and then aged, then 1 to 1 at a temperature of 1,300 to 1,400°C. It is prepared by firing for 2 hours.
상기 복합효소액은 효소활성보조제 100중량부에 미생물혼합균주 1~10중량부, 생리활성화물질 20~30중량부 및 부식산 1~5중량부를 포함한다. The complex enzyme solution contains 1 to 10 parts by weight of a microorganism mixed strain, 20 to 30 parts by weight of a physiologically active substance, and 1 to 5 parts by weight of humic acid in 100 parts by weight of an enzyme activity adjuvant.
상기 효소활성보조제는 육류 세척수 100중량부에 바실러스 낫토균 0.1~1중량부를 가하고 5~7일 동안 혐기 발효하고, 40~42일 동안 폭기하여 호기 발효하여 제조한다.The enzyme activity aid is prepared by adding 0.1 to 1 parts by weight of Bacillus natto bacteria to 100 parts by weight of meat washing water, anaerobic fermentation for 5 to 7 days, aeration for 40 to 42 days, and aerobic fermentation.
상기 바실러스 낫토균(Bacillus natto)은 짚에 존재하며, 짚 한 묶음에 약 1천만개가 붙어있으며 균의 크기는 길이 2.33마이크론, 폭은 1마이크론이고 종의 보존을 위해 포자를 형성하는 성질을 가지고 있다.The bacilli present in natto straw bacteria (Bacillus natto) is attached to the approximately 10 million at a straw bundle, and the size of the bacteria has a length 2.33 microns, a width of 1 micron and has a property to form spores for the preservation of the species .
상기 미생물혼합균주는 홍국균 40~50중량%, 고초균 20~30중량%, 효모 10~20중량% 및 누룩균 5~15중량%를 포함한다.The microorganism-mixed strain includes 40 to 50% by weight of honggukgyun, 20 to 30% by weight of Bacillus bacillus, 10 to 20% by weight of yeast, and 5 to 15% by weight of yeast.
상기 미생물혼합균주는 홍국균, 고초균, 효모 및 누룩균을 혼합하는 개념으로서, 이렇게 혼합하면 복합활성효소의 생성이 가능하다.The microorganism-mixed strain is a concept of mixing honggukgyun, Bacillus bacillus, yeast, and yeast, and when mixed in this way, it is possible to produce a complex active enzyme.
상기 홍국균은 자낭균문 모나스커스(Monascus)속에 속하는 붉은색의 사상균으로서, 쌀 등과 같은 곡류를 발효시키는 과정에서 각종 유익한 대사산물로 진한 빨간색의 색소 및 모나콜린 K 등을 생산한다. 이 균은 중국을 중심으로 동아시아의 여러 지역에서 천연의 식품 착색제나 가공품 및 소화 촉진과 혈류 개선의 소재로서 오랫동안 사용되어 왔다. 홍국균이 생성하는 2차 대사산물인 메비놀린은 콜레스테롤 생합성효소인 HMG-CoA(3-hydroxy-methyl-3-glutaryl-coenzyme) 환원효소를 강력하게 저해하여 혈중지질 농도를 감소시키고 콜레스테롤 합성을 억제하거나 항진균, 혈당상승의 억제, 혈압조절, 항비만, 항암 등과 같은 각종 기능성을 가진다. 또한, 홍국균은 적색계 색소(rubropuntain, monascorubin)와 황색계 색소(monascin, ankaflavin), 자색계 색소(rubropunctamine, monascorubramine) 등을 생성하며, 이와 같은 색소물질은 항균 및 항암효과가 있다.The honggukgyun is a red-colored filamentous fungus belonging to the genus Monascus, and produces dark red pigments and Monacholine K as various beneficial metabolites in the process of fermenting grains such as rice. This fungus has long been used as a natural food colorant or processed product in various regions of East Asia, mainly in China, as a material for promoting digestion and improving blood flow. Mebinoline, a secondary metabolite produced by Honggukbacteria, strongly inhibits the cholesterol biosynthetic enzyme HMG-CoA (3-hydroxy-methyl-3-glutaryl-coenzyme) reductase, thereby reducing blood lipid concentration and inhibiting cholesterol synthesis. It has various functions such as antifungal, suppression of blood sugar rise, blood pressure control, anti-obesity, and anti-cancer. In addition, honggukgyun produces red pigments (rubropuntain, monascorubin), yellow pigments (monascin, ankaflavin), purple pigments (rubropunctamine, monascorubramine), and the like, and such pigments have antibacterial and anticancer effects.
상기 홍국균은 모나스커스 필로서스(Monascus pilosus), 모나스커스 러버(Monascus ruber), 모나스커스 퍼프레우스(Monascus purpureus), 모나스커스 카올리앙(Monascus kaoliang), 모나스커스 바리케리(Monascus barykery) 및 모나스커스 안카(Monascus anka)로 이루어진 군에서 선택된 어느 하나를 사용할 수 있다.The honggukgyun is Monascus pilosus , Monascus ruber , Monascus purpureus , Monascus kaoliang , Monascus barykery , and Monascus barykery. Any one selected from the group consisting of Monascus anka may be used.
상기 고초균은 바실러스 섭틸리스(B. subtilis), 바실러스 리크네포르미스(B. lichneformis), 바실러스 메가테리움(B. megaterium), 바실러스 아밀로리퀘파시엔스(B. amyloliquefaciens), 바실러스 낫토(B. natto), 바실러스 안스라시스(B.antharcis), 바실러스렌투스(B.lentus), 바실러스 퍼미러스(B.pumilus), 바실러스 더링지엔시스(B.thuringiensis), 바실러스 알베이(B.alvei), 바실러스 아조토픽산스(B.azotofixans), 바실러스 매세란스(B.macerans), 바실러스 포리믹사(B.polymyxa), 바실러스 파필리에(B.popilliae), 바실러스 코아글란스(B.coagulans), 바실러스 스테아로더모필러스(B.stearothermophilus), 바실러스 파스퇴리(B.pasteurii), 바실러스 패리커스(B.sphaericus) 및 바실러스 패스티디오서스(B.fastidiosus)로 이루어진 군에서 선택된 어느 하나를 사용할 수 있다.The Bacillus subtilis is Bacillus subtilis (B. subtilis), Bacillus leakage four formate miss (B. lichneformis), Bacillus MEGATHERIUM (B. megaterium), Bacillus amyl Lowry Quebec Pacific Enschede (B. amyloliquefaciens), Bacillus natto (B natto ), B.antharcis , B.lentus , B.pumilus , B.thuringiensis , B.alvei ), Bacillus azo topic Sans (B.azotofixans), Bacillus maese lance (B.macerans), Bacillus Poly miksa (B.polymyxa), Bacillus papil Rie (B.popilliae), Bacillus core posts lance (B.coagulans), Bacillus stearate loader Russ a brush (B.stearothermophilus), may be used for Bacillus Pas toeri (B.pasteurii), Bacillus Parry coarse one selected from the group consisting of (B.sphaericus) and Bacillus Pastes video suspension (B.fastidiosus).
상기 효모는 사카로마이세스 루시(Saccharomyces rouxii), 사카로마이세스 세레비시아에(Saccharomyces cereviciae), 사카로마이세스 오비폴미스(Saccharomyces oviformis) 및 사카로마이세스 스테이네리(Saccharomyces steineri)로 이루어진 군에서 선택된 어느 하나를 사용할 수 있다. The yeast consists of Saccharomyces rouxii , Saccharomyces cereviciae , Saccharomyces oviformis , and Saccharomyces steineri . Any one selected from the group can be used.
상기 누룩균은 아스퍼질러스 오리제(Aspergillus oryzae) 및 아스퍼질러스 소제(Aspergillus sojae)로 이루어진 군에서 선택된 어느 하나를 사용할 수 있다.The yeast may be used any one selected from the group consisting of Aspergillus oryzae and Aspergillus sojae.
상기 생리활성화물질은 유기질 100중량부에 상기 효소활성보조제 1~5중량부 및 물 10~20중량부를 혼합 후 10~20일 동안 혐기 발효시킨 후, 1~3일 동안 호기 발효시킨 발효물질 100중량부에 물 500~600중량부를 넣어 2~5일 동안 폭기조에서 발효시킨 후 이를 정치 및 침전시켜 분리한 상등액을 포함한다.The physiologically activating substance is 100 parts by weight of the fermented substance after mixing 1 to 5 parts by weight of the enzyme activation aid and 10 to 20 parts by weight of water and then anaerobic fermentation for 10 to 20 days, and then aerobic fermentation for 1 to 3 days. Add 500 to 600 parts by weight of water to the part and ferment it in an aeration tank for 2 to 5 days, then settle and settle it to contain the separated supernatant.
상기 유기질은 등겨, 쌀겨 및 어분 중에서 선택된 어느 하나 이상을 사용할 수 있다. 상기 어분은 물고기를 말려서 빻은 가루를 의미한다.The organic material may be used any one or more selected from bran, rice bran, and fish meal. The fishmeal refers to a fish powder that has been dried and ground.
상기 부식산은 알칼리에 의해 토양에서 추출되거나 산에 의해 침적된 유기물로서, 황갈색~흑갈색의 중~고분자의 산성물질로서 무절형이며, 그 조성은 탄소 50~60%, 수소 3~5%, 질소 1.5~6%, 황 1% 내외, 회분 1% 내외, 산소 30~50% 이다. 부식산은 벤젠핵과 나프탈렌, 피리딘, 안트라센 등 방향족 고리를 가지고 있고 공역 2중결합을 많이 가지고 있는 특징이 있다. 부식산은 효소활성보조제의 보조인자로서 1차 효소반응이 이루어지면 아미노산, 포도당, 지방산, 글리세린 등으로 저분해되면서 미생물의 대사계에 이용되며, 이때 미생물이 서식할 수 있는 기질이 되므로 생물학적 촉매작용도 한다. 또 부식산은 미생물의 활성을 저해하는 인, 철, 등을 흡수하여 미생물의 활동저해를 방지하고 인산 및 탄소의 공급원이 되어 미생물이 군집을 형성하고 번성할 수 있게 한다.The humic acid is an organic substance extracted from the soil by alkali or deposited by acid, and is an acidic substance of medium to high molecular weights of yellow brown to dark brown, and its composition is 50 to 60% carbon, 3 to 5% hydrogen, and 1.5 nitrogen. It is ~6%, around 1% sulfur, around 1% ash, and 30~50% oxygen. Humic acid has a benzene nucleus and an aromatic ring such as naphthalene, pyridine, and anthracene, and has many conjugated double bonds. Humic acid is a cofactor in the enzyme activity aid, and when the first enzymatic reaction is performed, it is reduced to amino acids, glucose, fatty acids, glycerin, etc., and is used in the metabolic system of microorganisms. At this time, it becomes a substrate for microorganisms to inhabit, so biological catalysis is also possible. do. In addition, humic acid absorbs phosphorus, iron, and the like, which inhibit the activity of microorganisms, prevents the activity of microorganisms, and becomes a source of phosphoric acid and carbon, allowing microorganisms to form colonies and thrive.
상기 풀빅산(Fulvic Acid)은 천연 휴믹물질로부터 정제수를 이용하여 추출하는 정제수 추출법에 의해 추출된 것이다. 천연 휴믹 물질의 농도가 5~10%가 되도록 정제수를 부가한 다음 60~70℃의 온탕에서 교반하여 얻어진 상등액을 여과 및 농축하여 추출된다.The Fulvic Acid is extracted from a natural humic substance by a purified water extraction method using purified water. Purified water is added so that the concentration of the natural humic substance is 5-10%, and then the supernatant obtained by stirring in hot water at 60-70° C. is filtered and concentrated to extract.
천연휴믹물질(Natural Humic substance)은 수질환경 및 양어장 환경개선에 상당한 효과를 이루면서도 항균, 항진균 효과가 우수한 천연물질이다. 이러한 천연휴믹물질은 식물의 잔재물이 퇴적되어 수천만년동안 분해과정을 거친 퇴적토양인 휴민토양이 이에 해당된다. 이러한 천연휴믹물질에서 추출한 저분자량의 산으로 구성된 풀빅산은 생물활성이 높고 분자구조 중에 미네랄과 요소와 쉽게 결합하는 능력을 가지고 있을 뿐만 아니라, 수백종의 복합 미네랄과 다수의 영양수, 그리고 다량의 용존 산소를 함유하고 있으며, 표면장력이 낮아 피부 침투력이 우수하다.Natural Humic Substances are natural substances with excellent antibacterial and antifungal effects while achieving significant effects in improving the water environment and the environment of fish farms. These natural humic substances are humiliated soils, which are sedimentary soils that have been decomposed for tens of millions of years due to the accumulation of plant residues. Fulvic acid, which is composed of low molecular weight acids extracted from these natural humic substances, has high biological activity and the ability to easily bind minerals and urea in its molecular structure, as well as hundreds of complex minerals, a large number of nutrients, and a large amount of dissolved water. It contains oxygen and has excellent skin penetration due to low surface tension.
본 발명에 따른 반도체 및 디스플레이 제조공정용 세정제 조성물은 금속 오염물을 제거할 뿐만 아니라 파티클의 재부착을 방지할 수 있는 장점이 있다. The cleaning agent composition for semiconductor and display manufacturing processes according to the present invention has the advantage of not only removing metal contaminants, but also preventing re-adhesion of particles.
본 발명의 반도체 및 디스플레이 제조공정용 세정제 조성물은 기판의 부식을 방지할 수 있는 장점이 있다.The cleaning agent composition for a semiconductor and display manufacturing process of the present invention has an advantage of preventing corrosion of a substrate.
이하, 실시 예를 통하여 본 발명의 구성 및 효과를 더욱 상세히 설명하고자 한다. 이들 실시 예는 오로지 본 발명을 예시하기 위한 것일 뿐 본 발명의 범위가 이들 실시 예에 의해 제한되는 것은 아니다. Hereinafter, the configuration and effects of the present invention will be described in more detail through examples. These examples are for illustrative purposes only, and the scope of the present invention is not limited by these examples.
에틸렌디아민테트라아세트산(ethylenediaminetetraacetic acid) 2중량%, 락트산 알킬 에스테르(lactic acid alkyl ester) 0.5중량%, 디이소프로판올아민 2중량%, 과산화수소 0.5중량%, 폴리스티렌술폰산 0.5중량%, 테트라에틸암모늄 하이드록사이드(tetraethylammonium hydroxide) 0.5중량%, 폴리옥시에틸렌노닐페닐에테르 2중량%, 폴리옥시부틸렌 실록산 1중량% 및 초순수 91중량%를 혼합한 후 23℃에서 500rpm의 속도로 교반하여 반도체 및 디스플레이 제조공정용 세정제 조성물을 제조하였다. Ethylenediaminetetraacetic acid 2% by weight, lactic acid alkyl ester 0.5% by weight, diisopropanolamine 2% by weight, hydrogen peroxide 0.5% by weight, polystyrenesulfonic acid 0.5% by weight, tetraethylammonium hydroxide ( tetraethylammonium hydroxide) 0.5% by weight, 2% by weight of polyoxyethylene nonylphenyl ether, 1% by weight of polyoxybutylene siloxane, and 91% by weight of ultrapure water are mixed and stirred at 23°C at a speed of 500 rpm to be a cleaner for semiconductor and display manufacturing processes. The composition was prepared.
실시예 1에서 제조한 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 세정력향상제 1중량부를 추가적으로 혼합하였다.1 part by weight of a cleaning power improving agent was additionally mixed with 100 parts by weight of the cleaning agent composition for semiconductor and display manufacturing processes prepared in Example 1.
상기 세정력향상제는 불화테트라메틸암모늄 40중량%, 디에틸렌글리콜모노메틸에테르 25중량%, 디메틸아세트아미드 15중량%, 석신산(succinic acid) 15중량% 및 트리플루오로아세트산(trifluoroacetic acid) 5중량%를 혼합하여 제조하였다. The cleaning power improving agent is tetramethylammonium fluoride 40% by weight, diethylene glycol monomethyl ether 25% by weight, dimethylacetamide 15% by weight, succinic acid 15% by weight, and trifluoroacetic acid 5% by weight Was prepared by mixing.
[비교예 1][Comparative Example 1]
수산화칼륨 4중량%, 아세트산 칼슘 0.5중량%, 시클로헥산-1,2-디아민 테트라아세트산 0.8중량%, 비이온성계면활성제(softanol 90) 0.1중량% 및 초순수 94.6중량%를 혼합한 후 23℃에서 500rpm의 속도로 교반하여 세정제 조성물을 제조하였다. After mixing 4% by weight of potassium hydroxide, 0.5% by weight of calcium acetate, 0.8% by weight of cyclohexane-1,2-diamine tetraacetic acid, 0.1% by weight of nonionic surfactant (softanol 90) and 94.6% by weight of ultrapure water, 500 rpm at 23°C Stirring at a speed of to prepare a detergent composition.
[실험예 1][Experimental Example 1]
실시예 1, 2 및 비교예 1의 세정제 조성물을 이용하여, 알루미늄 잔사, 스테인레스 잔사, 철 잔사, 그리스에 대한 세정력을 평가하여 표 1에 나태내었다. Using the detergent compositions of Examples 1 and 2 and Comparative Example 1, the cleaning power of aluminum residue, stainless steel residue, iron residue, and grease was evaluated and shown in Table 1.
구체적으로, 오염시편 제작은 각 오염물을 IPA(이소프로필 알코올)에 500ppm의 농도로 분산시킨 후 비정질실리콘 단막 기판(3㎝×3㎝)에 도포 하였다. 도포후, 상기 기판을 50bar로 프레스를 가하면서 200℃로 베이크하여 오염물을 고착화시켜 제작하였다.Specifically, in the preparation of contaminated specimens, each contaminant was dispersed in IPA (isopropyl alcohol) at a concentration of 500 ppm and then coated on an amorphous silicon single film substrate (3 cm×3 cm). After coating, the substrate was baked at 200° C. while pressing at 50 bar to fix contaminants.
평가 전, 제작된 오염시편에 대한 오염물, 즉 금속 잔사의 갯수를 확인하였다. 또한, 그리스의 경우 제작된 오염시편 표면에 존재하는 입자형태의 오염물의 개수로 확인하였다. 제작된 오염시편을 각 실시예 1, 2 및 비교예 1의 세정제 조성물에 1분간 40℃에서 침지시켰다. 이후, 평가 전·후 금속 잔사 및 입자형태의 오염물의 갯수를 비교하고, 이의 차이를 백분율로 환산하여 세정력의 정도를 평가하였다(하기 식1 참조). 이때, 백분율이 100%에 가까울수록 세정력이 높음을 의미한다.Before evaluation, the number of contaminants, that is, metal residues, was confirmed for the produced contaminated specimen. Also, in the case of grease, the number of contaminants in the form of particles present on the surface of the produced contaminated specimen was confirmed. The prepared contaminated specimens were immersed in the detergent compositions of Examples 1 and 2 and Comparative Example 1 at 40° C. for 1 minute. Thereafter, before and after the evaluation, the number of metal residues and contaminants in the form of particles were compared, and the difference was converted into a percentage to evaluate the degree of cleaning power (see Equation 1 below). In this case, the closer the percentage is to 100%, the higher the cleaning power.
[식1][Equation 1]
세정력(%) = [1 - {(세정 후, 오염물의 갯수) / (세정 전, 오염물의 갯수)}]Х100Cleaning power (%) = [1-{(After washing, the number of contaminants) / (Before washing, the number of contaminants)}]Х100
세정력Aluminum residue
Cleaning power
세정력Stainless residue
Cleaning power
세정력Iron residue
Cleaning power
세정력Greece
Cleaning power
표 2에 나타낸 바와 같이, 실시예 1, 2에서 제조한 세정제 조성물은 비교예 1에서 제조한 세정제 조성물에 비하여 알루미늄 잔사, 스테인레스 잔사, 철 잔사 등으로 대표될 수 있는 금속 잔사의 제거에 탁월한 효과를 발휘함을 확인할 수 있다. 동시에 입자형태의 오염물을 포함하는 그리스에 대한 세정능 또한 우수함을 확인할 수 있다.As shown in Table 2, the detergent composition prepared in Examples 1 and 2 has an excellent effect on removing metal residues, which may be represented by aluminum residues, stainless residues, iron residues, etc., compared to the detergent composition prepared in Comparative Example 1. It can be confirmed that it is exerted. At the same time, it can be confirmed that the cleaning ability for grease containing particulate contaminants is also excellent.
실시예 1에서 제조한 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 부식방지제 1중량부를 추가적으로 혼합하였다. 1 part by weight of a corrosion inhibitor was additionally mixed with 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes prepared in Example 1.
상기 부식방지제는 벤조트리아졸(1,2,3-benzotriazol) 50중량%, 피로갈롤(Pyrogallol) 25중량%, 티오글리세롤 14중량%, 폴리아미노설폰 10중량% 및 5-아미노 테트라졸(5-amino-1H-Tetrazole) 1중량%를 혼합하여 제조하였다.The corrosion inhibitor is benzotriazole (1,2,3-benzotriazol) 50% by weight, pyrogallol (Pyrogallol) 25% by weight, thioglycerol 14% by weight, polyaminosulfone 10% by weight and 5-amino tetrazole (5- Amino-1H-Tetrazole) was prepared by mixing 1% by weight.
[실험예 2][Experimental Example 2]
실시예 1, 3 및 비교예 1의 세정제 조성물을 이용하여, 플렉서블 유기발광다이오드 기판 제조에 사용될수 있는 유·무기막 단막질에 대한 식각속도를 측정하여, 부식방지성을 평가하였다. 상기 식각속도는 엘립소미터(J.A.WOOLLAM社 M-2000)로 평가전·후 기판의 두께변화를 측정하여 계산하였다.Using the cleaning agent compositions of Examples 1 and 3 and Comparative Example 1, the etching rate of the organic/inorganic single film material that can be used for manufacturing the flexible organic light emitting diode substrate was measured to evaluate the corrosion resistance. The etch rate was calculated by measuring the thickness change of the substrate before and after evaluation with an ellipsometer (J.A. WOOLLAM M-2000).
구체적으로, 평가에 사용된 단막질은 비정질실리콘(a-Si), SiO2, SiNx 또는 글라스 단막 기판(3㎝×3㎝)을 사용하였다. 상기 단막 기판을 각 실시예 1, 3 및 비교예 1의 세정제 조성물에 1분간 40℃에서 침지시켰다. 이후, 평가 전·후 각 단막 기판의 두께변화를 측정하여, 식각속도로 평가하였다.Specifically, as the single film material used in the evaluation, amorphous silicon (a-Si), SiO 2 , SiNx, or a glass single film substrate (3 cm×3 cm) was used. The single-film substrate was immersed in the detergent compositions of Examples 1 and 3 and Comparative Example 1 at 40°C for 1 minute. Thereafter, the change in thickness of each single-film substrate before and after the evaluation was measured and evaluated by the etch rate.
대한 식각속도
(Å/min)on α-Si substrate
About etch rate
(Å/min)
대한 식각속도
(Å/min)SiO 2 on the substrate
About etch rate
(Å/min)
대한 식각속도
(Å/min)On SiNx substrate
About etch rate
(Å/min)
기판에 대한
식각속도
(Å/min)Flexible glass
For the substrate
Etching speed
(Å/min)
표 2에 나타낸 바와 같이, 실시예 1, 3에서 제조한 세정제 조성물은 실리콘 함유 하부막이 형성된 기판에 부식이나 손상을 야기하지 않고, 플렉시블 유리 기판에 대한 손상도 야기하지 않았다.As shown in Table 2, the cleaning agent compositions prepared in Examples 1 and 3 did not cause corrosion or damage to the substrate on which the silicon-containing lower film was formed, and did not cause damage to the flexible glass substrate.
반면, 비교예 1의 세정제 조성물은 실리콘 함유 하부막이 형성된 기판은 물론 플렉시블 유리 기판에 대한 손상도 야기하였다.On the other hand, the cleaning agent composition of Comparative Example 1 caused damage to the flexible glass substrate as well as the substrate on which the silicon-containing lower film was formed.
실시예 1에서 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 하부막보호제 1중량부를 추가적으로 포함하였다. In Example 1, 1 part by weight of the lower film protector was additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes.
상기 하부막보호제는 벤조트리졸(benzotrizole) 50중량%, 메틸 글리콜(methyl glycol) 30중량%, 메틸트리부틸암모늄 하이드록사이드 15중량% 및 히드로퀴논 5중량%를 혼합하여 제조하였다.The lower film protective agent was prepared by mixing 50% by weight of benzotrizole, 30% by weight of methyl glycol, 15% by weight of methyltributylammonium hydroxide, and 5% by weight of hydroquinone.
[실험예 3][Experimental Example 3]
실시예 1, 4 및 비교예 1의 세정제 조성물을 사용하여 세정한 후에 알루미늄의 부식 정도를 측정하기 위한 실험을 실시하였다. 기판 위에 640nm 두께의 알루미늄 박막을 형성한 후에 실시예 1, 4 및 비교예 1의 세정제 조성물을 0.4중량% 포함하는 세정제를 각각 사용하여 세정 한 후에 알루미늄 층의 두께를 다시 측정하였으며, 그 결과를 표 3에 나타내었다. 이때 세정제의 종류를 제외하고 다른 실험 조건은 모두 동일하였다. After washing using the detergent compositions of Examples 1 and 4 and Comparative Example 1, an experiment was conducted to measure the degree of corrosion of aluminum. After forming an aluminum thin film with a thickness of 640 nm on the substrate, the thickness of the aluminum layer was measured again after cleaning using a cleaning agent containing 0.4% by weight of the cleaning agent composition of Examples 1 and 4 and Comparative Example 1, respectively, and the results are shown in the table. It is shown in 3. At this time, all other experimental conditions were the same except for the type of detergent.
표 3에 나타낸 바와 같이, 실시예 1, 4에서 제조한 세정제 조성물을 사용하여 세정하는 경우 알루미늄의 손상은 거의 없는데 비하여, 비교예 1에서 제조한 세정제 조성물을 사용하여 세정하는 경우에는 알루미늄의 손상이 매우 심하다는 것을 알 수 있다.As shown in Table 3, when cleaning using the cleaning agent composition prepared in Examples 1 and 4, there is little damage to aluminum, whereas when cleaning using the cleaning agent composition prepared in Comparative Example 1, damage to aluminum You can see that it is very severe.
실시예 1에서 제조한 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 거품제거제 1중량부를 추가적으로 포함하였다. 1 part by weight of a foam remover was additionally included in 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes prepared in Example 1.
상기 거품제거제는 헥산올 55중량%, 폴리에틸렌글리콜 25중량%, 트리이소부틸포스페이트 15중량% 및 과불소화노난올(CF3(CF2)8OH) 5중량%를 혼합하여 제조하였다. The foam remover was prepared by mixing 55% by weight of hexanol, 25% by weight of polyethylene glycol, 15% by weight of triisobutyl phosphate, and 5% by weight of perfluorinated nonanol (CF 3 (CF 2 ) 8 OH).
[실험예 4][Experimental Example 4]
반도체 기판을 각 실시예 1, 5 및 비교예 1의 세정제 조성물에 5분간 침지시켰다. 그 후, 기판을 꺼내어 거품 발생 정도를 평가하여 얻어진 결과를 표 4에 나타내었다.The semiconductor substrate was immersed in the cleaning agent compositions of Examples 1 and 5 and Comparative Example 1 for 5 minutes. Thereafter, the substrate was taken out and the degree of foam generation was evaluated, and the results obtained are shown in Table 4.
○ : 약간 거품이 발생한다
△ : 다소 거품 발생이 심하다
× : 실용상 사용이 우려되는 레벨의 심한 거품 발생이 관측된다◎: There is no problem of foaming
○: A little bubble is generated
△: Somewhat severe foaming
×: occurrence of severe foaming at a level of concern for practical use is observed
표 4에 나타낸 바와 같이, 실시예 1, 5의 세정제 조성물은 비교예 1의 세정제 조성물에 비하여 거품 제거 효과가 우수한 것을 확인할 수 있다.As shown in Table 4, it can be seen that the detergent compositions of Examples 1 and 5 have superior foam removal effects compared to the detergent compositions of Comparative Example 1.
실시예 1에서 제조한 반도체 및 디스플레이 제조공정용 세정제 조성물 100중량부에 재흡착방지제 1중량부를 추가적으로 혼합하였다. 1 part by weight of an anti-resorbent was additionally mixed with 100 parts by weight of the cleaning composition for semiconductor and display manufacturing processes prepared in Example 1.
상기 재흡착방지제는 수산화세슘(Cesium hydroxide) 55중량%, 폴리옥시에틸렌도데실페닐에테르 25중량%, 테트라부틸암모늄 하이드록사이드(TBAH) 15중량%, 수산화칼륨(KOH) 4중량% 및 풀빅산 발효물 1중량%를 혼합하여 제조하였다.The re-adsorption inhibitor is cesium hydroxide (Cesium hydroxide) 55% by weight, polyoxyethylene dodecylphenyl ether 25% by weight, tetrabutylammonium hydroxide (TBAH) 15% by weight, potassium hydroxide (KOH) 4% by weight and fulvic acid It was prepared by mixing 1% by weight of the fermented product.
상기 풀빅산 발효물은 바이오세라믹 스톤 정제수 50중량%, 복합효소액 30중량% 및 풀빅산 분말 20중량%를 혼합한 혼합물을 25℃에서 72시간 동안 호기발효하여 제조하였다. 상기 바이오세라믹 스톤 정제수는 물 100중량부에 바이오세라믹 스톤 5중량부를 넣고 14시간 동안 방치하여 수득하였다. 상기 바이오세라믹 스톤은 진주석 50중량%, 견운모 30중량% 및 황토 20중량%를 포함하는 혼합물을 물에 넣고 혼련한 후 숙성시킨 다음, 1,400℃의 온도에서 2시간 동안 소성시켜 제조하였다. 상기 복합효소액은 효소활성보조제 100중량부에 미생물혼합균주 10중량부, 생리활성화물질 20중량부 및 부식산 5중량부를 혼합하여 제조하였다. 상기 효소활성보조제는 육류 세척수 100중량부에 바실러스 낫토균 1중량부를 가하고 7일 동안 혐기 발효하고, 40일 동안 폭기하여 호기 발효하여 제조하였다. 상기 미생물혼합균주는 홍국균 50중량%, 고초균 25중량%, 효모 15중량% 및 누룩균 10중량%를 혼합하여 제조하였다. 상기 생리활성화물질은 유기질 100중량부에 상기 효소활성보조제 5중량부 및 물 15중량부를 혼합 후 10일 동안 혐기 발효시킨 후, 3일 동안 호기 발효시킨 발효물질 100중량부에 물 500중량부를 넣어 3일 동안 폭기조에서 발효시킨 후 이를 정치 및 침전시켜 분리한 상등액을 사용하였다. 상기 유기질은 어분을 사용하였다. The fermented fulvic acid was prepared by aerobic fermentation at 25° C. for 72 hours in a mixture of 50% by weight of purified bioceramic stone, 30% by weight of complex enzyme solution, and 20% by weight of fulvic acid powder. The bioceramic stone purified water was obtained by adding 5 parts by weight of bioceramic stone to 100 parts by weight of water and allowing it to stand for 14 hours. The bioceramic stone was prepared by adding a mixture containing 50% by weight of pearlite, 30% by weight of silky mica, and 20% by weight of loess in water, followed by kneading and then aging, and then calcined at a temperature of 1,400°C for 2 hours. The complex enzyme solution was prepared by mixing 10 parts by weight of a microorganism mixed strain, 20 parts by weight of a physiologically active substance, and 5 parts by weight of humic acid to 100 parts by weight of an enzyme activity aid. The enzyme activity aid was prepared by adding 1 part by weight of Bacillus natto bacteria to 100 parts by weight of meat washing water, anaerobic fermentation for 7 days, aeration for 40 days, and aerobic fermentation. The microorganism-mixed strain was prepared by mixing 50% by weight of honggukgyun, 25% by weight of Bacillus bacillus, 15% by weight of yeast, and 10% by weight of yeast. The physiologically activating material was mixed with 5 parts by weight of the enzyme activation aid and 15 parts by weight of water to 100 parts by weight of organic matter, and then anaerobic fermentation was performed for 10 days, and then 500 parts by weight of water was added to 100 parts by weight of the fermented material that was aerobic fermented for 3 days After fermentation in an aeration tank for 1 day, it was allowed to stand and precipitate, and the separated supernatant was used. Fish meal was used as the organic material.
[실험예 5][Experimental Example 5]
APM 및 HFM(염산과 과산화수소와 물과의 혼합물)으로 세정한 8인치(20.32㎝)베어(Bare)-Si웨이퍼를 금속이온(K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn)을 14ppb 첨가한 약액에 25℃, 1분간 침지시킨 후 DIW린스하고, 처리 전후의 금속 이온량(atoms/㎠:1㎠당 금속 이온의 개수)을 전반사형광X선 분석장치(TXRF(Rigaku))로 측정하였으며, 그 결과를 표 5에 나타내었다. The 8-inch (20.32cm) Bare-Si wafer washed with APM and HFM (a mixture of hydrochloric acid, hydrogen peroxide, and water) was transferred to metal ions (K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn). ) Is immersed in 14ppb-added chemical solution at 25°C for 1 minute, then rinsed with DIW, and the amount of metal ions before and after treatment (the number of metal ions per atom/cm2:1cm2) is measured by a total reflection fluorescence X-ray analyzer (TXRF (Rigaku)). It was measured as, and the results are shown in Table 5.
×1010
(atoms/
㎠)1.36
×10 10
(atoms/
㎠)
×1012
(atoms/
㎠)2.32
×10 12
(atoms/
㎠)
(atoms/
㎠)6.51×10 11
(atoms/
㎠)
×1013
(atoms/
㎠)4.98
×10 13
(atoms/
㎠)
표 5에 나타낸 바와 같이, 실시예 6의 세정제 조성물은 재부착한 금속이온이 없는 것을 확인할 수 있다.As shown in Table 5, it can be seen that the detergent composition of Example 6 does not have reattached metal ions.
또한, 실시예 1의 세정제 조성물은 비교예 1의 세정제 조성물에 비하여 재부착 방지 효과가 우수한 것을 확인할 수 있다.In addition, it can be seen that the detergent composition of Example 1 is superior to the detergent composition of Comparative Example 1 to prevent reattachment.
Claims (6)
상기 거품제거제는 헥산올 50~60중량%, 폴리에틸렌글리콜 20~30중량%, 트리이소부틸포스페이트 10~20중량% 및 과불소화노난올(CF3(CF2)8OH) 1~5중량%를 포함하는,
반도체 및 디스플레이 제조공정용 세정제 조성물.
Ethylenediaminetetraacetic acid 1 to 5% by weight, lactic acid alkyl ester 0.1 to 1% by weight, diisopropanolamine 1 to 5% by weight, hydrogen peroxide 0.1 to 1% by weight, polystyrene sulfonic acid 0.1 to 1 Including wt%, tetraethylammonium hydroxide 0.1 to 1 wt%, polyoxyethylene nonylphenyl ether 1 to 5 wt%, polyoxybutylene siloxane 1 to 3 wt%, and ultrapure water 80 to 85 wt% An additional 0.1 to 1 part by weight of a defoaming agent is included in 100 parts by weight of the mixture,
The defoaming agent contains 50 to 60% by weight of hexanol, 20 to 30% by weight of polyethylene glycol, 10 to 20% by weight of triisobutyl phosphate, and 1 to 5% by weight of perfluorinated nonanol (CF 3 (CF 2 ) 8 OH) Included,
Cleaning agent composition for semiconductor and display manufacturing processes.
상기 혼합물 100중량부에 세정력향상제 0.1~1중량부를 추가적으로 포함하되,
상기 세정력향상제는 불화테트라메틸암모늄 40~50중량%, 디에틸렌글리콜모노메틸에테르 20~30중량%, 디메틸아세트아미드 10~20중량%, 석신산(succinic acid) 10~20중량% 및 트리플루오로아세트산(trifluoroacetic acid) 1~5중량%를 포함하는,
반도체 및 디스플레이 제조공정용 세정제 조성물.
The method of claim 1,
An additional 0.1 to 1 part by weight of a cleaning power improving agent is included in 100 parts by weight of the mixture,
The cleaning power improving agent is tetramethylammonium fluoride 40-50% by weight, diethylene glycol monomethyl ether 20-30% by weight, dimethylacetamide 10-20% by weight, succinic acid 10-20% by weight, and trifluoro Containing 1 to 5% by weight of acetic acid (trifluoroacetic acid),
Cleaning agent composition for semiconductor and display manufacturing processes.
상기 혼합물 100중량부에 부식방지제 0.1~1중량부를 추가적으로 포함하되,
상기 부식방지제는 벤조트리아졸(1,2,3-benzotriazol) 40~50중량%, 피로갈롤(Pyrogallol) 20~30중량%, 티오글리세롤 10~20중량%, 폴리아미노설폰 5~15중량% 및 5-아미노 테트라졸(5-amino-1H-Tetrazole) 0.1~1중량%를 포함하는,
반도체 및 디스플레이 제조공정용 세정제 조성물.
The method of claim 1,
An additional 0.1 to 1 part by weight of a corrosion inhibitor is included in 100 parts by weight of the mixture,
The corrosion inhibitor is benzotriazole (1,2,3-benzotriazol) 40 to 50% by weight, pyrogallol (Pyrogallol) 20 to 30% by weight, thioglycerol 10 to 20% by weight, polyaminosulfone 5 to 15% by weight and 5-amino tetrazole (5-amino-1H-Tetrazole) containing 0.1 to 1% by weight,
Cleaning agent composition for semiconductor and display manufacturing processes.
상기 혼합물 100중량부에 하부막보호제 0.1~1중량부를 추가적으로 포함하되,
상기 하부막보호제는 벤조트리졸(benzotrizole) 50~60중량%, 메틸 글리콜(methyl glycol) 20~30중량%, 메틸트리부틸암모늄 하이드록사이드 10~20중량% 및 히드로퀴논 1~5중량%를 포함하는,
반도체 및 디스플레이 제조공정용 세정제 조성물.
The method of claim 1,
An additional 0.1 to 1 part by weight of a lower film protector is included in 100 parts by weight of the mixture,
The lower film protective agent includes 50 to 60% by weight of benzotrizole, 20 to 30% by weight of methyl glycol, 10 to 20% by weight of methyltributylammonium hydroxide, and 1 to 5% by weight of hydroquinone doing,
Cleaning agent composition for semiconductor and display manufacturing processes.
상기 혼합물 100중량부에 재흡착방지제 0.1~1중량부를 추가적으로 포함하되,
상기 재흡착방지제는 수산화세슘(Cesium hydroxide) 50~60중량%, 폴리옥시에틸렌도데실페닐에테르 20~30중량%, 테트라부틸암모늄 하이드록사이드(TBAH) 10~20중량%, 수산화칼륨(KOH) 1~5중량% 및 풀빅산 발효물 0.1~1중량%를 포함하며,
상기 풀빅산 발효물은 바이오세라믹 스톤 정제수 50~70중량%, 복합효소액 10~30중량% 및 풀빅산 분말 15~25중량%를 혼합한 혼합물을 20~25℃에서 72~74시간 동안 호기발효한 발효물을 사용하며,
상기 바이오세라믹 스톤 정제수는 물 100중량부에 바이오세라믹 스톤 1~5중량부를 넣고 10~14시간 동안 방치하여 수득하며,
상기 바이오세라믹 스톤은 진주석 40~50중량%, 견운모 25~35중량% 및 황토 20~30중량%를 포함하는 혼합물을 물에 넣고 혼련한 후 숙성시킨 다음, 1,300~1,400℃의 온도에서 1~2시간 동안 소성시키며,
상기 복합효소액은 효소활성보조제 100중량부에 미생물혼합균주 1~10중량부, 생리활성화물질 20~30중량부 및 부식산 1~5중량부를 포함하며,
상기 효소활성보조제는 육류 세척수 100중량부에 바실러스 낫토균 0.1~1중량부를 가하고 5~7일 동안 혐기 발효하고, 40~42일 동안 폭기하여 호기 발효하며,
상기 미생물혼합균주는 홍국균 40~50중량%, 고초균 20~30중량%, 효모 10~20중량% 및 누룩균 5~15중량%를 포함하며,
상기 생리활성화물질은 유기질 100중량부에 상기 효소활성보조제 1~5중량부 및 물 10~20중량부를 혼합 후 10~20일 동안 혐기 발효시킨 후, 1~3일 동안 호기 발효시킨 발효물질 100중량부에 물 500~600중량부를 넣어 2~5일 동안 폭기조에서 발효시킨 후 이를 정치 및 침전시켜 분리한 상등액을 사용하는,
반도체 및 디스플레이 제조공정용 세정제 조성물.The method of claim 1,
An additional 0.1 to 1 part by weight of a re-adsorption inhibitor is included in 100 parts by weight of the mixture,
The re-adsorption inhibitor is cesium hydroxide (Cesium hydroxide) 50-60% by weight, polyoxyethylene dodecylphenyl ether 20-30% by weight, tetrabutylammonium hydroxide (TBAH) 10-20% by weight, potassium hydroxide (KOH) Including 1 to 5% by weight and 0.1 to 1% by weight of fulvic acid fermentation,
The fulvic acid fermented product is a mixture of 50 to 70% by weight of purified bioceramic stone, 10 to 30% by weight of complex enzyme solution, and 15 to 25% by weight of fulvic acid powder by aerobic fermentation at 20 to 25°C for 72 to 74 hours. Fermented products are used,
The bioceramic stone purified water is obtained by adding 1 to 5 parts by weight of bioceramic stone to 100 parts by weight of water and leaving it for 10 to 14 hours,
The bioceramic stone is a mixture containing 40 to 50% by weight of pearlite, 25 to 35% by weight of silky mica, and 20 to 30% by weight of loess, mixed with water, and then aged, then 1 to 1 at a temperature of 1,300 to 1,400°C. Firing for 2 hours,
The complex enzyme solution contains 1 to 10 parts by weight of a microorganism mixed strain, 20 to 30 parts by weight of a physiologically active substance, and 1 to 5 parts by weight of humic acid, to 100 parts by weight of an enzyme activity adjuvant,
The enzyme activity aid is aerobic fermentation by adding 0.1 to 1 parts by weight of Bacillus natto bacteria to 100 parts by weight of meat washing water, anaerobic fermentation for 5 to 7 days, aeration for 40 to 42 days,
The microorganism-mixed strain contains 40 to 50% by weight of honggukgyun, 20 to 30% by weight of Bacillus bacillus, 10 to 20% by weight of yeast, and 5 to 15% by weight of yeast,
The physiologically activating substance is 100 parts by weight of the fermented substance after mixing 1 to 5 parts by weight of the enzyme activation aid and 10 to 20 parts by weight of water and then anaerobic fermentation for 10 to 20 days, and then aerobic fermentation for 1 to 3 days. Put 500 to 600 parts by weight of water in the part and ferment it in an aeration tank for 2 to 5 days, then settle and settle it to use the separated supernatant.
Cleaning agent composition for semiconductor and display manufacturing processes.
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| KR102397607B1 (en) * | 2021-11-22 | 2022-05-13 | 주식회사 사이조은 | Ice Maker having improved Hygiene Property |
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| KR102397607B1 (en) * | 2021-11-22 | 2022-05-13 | 주식회사 사이조은 | Ice Maker having improved Hygiene Property |
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