KR100761602B1 - Wet Etching Agent Composition - Google Patents
Wet Etching Agent Composition Download PDFInfo
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- KR100761602B1 KR100761602B1 KR1020027009580A KR20027009580A KR100761602B1 KR 100761602 B1 KR100761602 B1 KR 100761602B1 KR 1020027009580 A KR1020027009580 A KR 1020027009580A KR 20027009580 A KR20027009580 A KR 20027009580A KR 100761602 B1 KR100761602 B1 KR 100761602B1
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Abstract
옥살산과, 폴리옥시에틸렌 알킬에테르 황산염 및/또는 폴리옥시에틸렌 알킬페닐에테르 황산염을 함유하는 수용액인 투명도전막용 습식에칭제 조성물이다. 비정질 ITO을 옥살산 수용액을 사용한 습식에칭시에 에칭 잔류물을 전혀 발생하지 않고 또한 온화한 조건하에서 에칭을 행할 수 있는 습식에칭제를 제공할 수 있다.It is a wet etching agent composition for transparent conductive films which is an aqueous solution containing oxalic acid and polyoxyethylene alkyl ether sulfate and / or polyoxyethylene alkylphenyl ether sulfate. It is possible to provide a wet etching agent capable of etching under mild conditions without generating any etching residues when wet etching an amorphous ITO with an aqueous solution of oxalic acid.
Description
본 발명은 액정 디스플레이 등에 화소전극으로서 사용되는 ITO(산화인듐 주석) 등의 투명도전막의 습식에칭에 사용되는 에칭제 조성물에 관한 것이다.TECHNICAL FIELD The present invention relates to an etchant composition used for wet etching of a transparent conductive film such as ITO (indium tin oxide) used as a pixel electrode in a liquid crystal display or the like.
ITO 막을 비롯한 투명도전막은 대전방지막, 열반사막, 광전변환소자 혹은 각종 플랫 패널 디스플레이의 투명전극 등의 전자장치 분야에 광범위하게 사용되어 왔다. 특히 최근에는 노트북PC, 소형TV, 휴대용 정보단말기 등의 보급과 함께 액정 디스플레이(LCD)에서의 수요가 증가하고 있다. ITO 막 등의 투명도전막은 플랫 패널 디스플레이 분야에 있어서는 화소의 표시전극으로서 사용되고 포토리소그래피의 에칭에 의해 제작된다.Transparent conductive films including ITO films have been widely used in the field of electronic devices such as antistatic films, heat reflecting films, photoelectric conversion devices or transparent electrodes of various flat panel displays. In recent years, the demand for liquid crystal displays (LCDs) is increasing with the proliferation of notebook PCs, small TVs, and portable information terminals. Transparent conductive films such as ITO films are used as display electrodes for pixels in the field of flat panel displays and are produced by etching of photolithography.
그러나, 액정 디스플레이(LCD), 특히 TFT-LCD 분야에 있어서는 종래 다결정 ITO가 사용되어 왔으나 기판 크기가 대형화할수록 다결정 ITO는 균일화가 어렵게 되고 있다. 또한, 상기 표시전극은 투명도전막 상에 포토레지스트를 도포하고 노광, 현상 후 포토레지스트를 마스크로 하여 에칭제를 사용하고, 에칭후 잔존하는 포토레지스트를 박리하는 방법에 의하여 형성된다.However, in the liquid crystal display (LCD), especially TFT-LCD, conventional polycrystalline ITO has been used, but as the substrate size increases, it becomes difficult to homogenize the polycrystalline ITO. In addition, the display electrode is formed by applying a photoresist on a transparent conductive film, using an etchant using a photoresist as a mask after exposure and development, and peeling off the photoresist remaining after etching.
종래에서, 상기 다결정 ITO막 등의 투명도전막의 에칭제로서 염화제2철/염산수용액, 요오드산 수용액, 인산수용액, 염산/질산수용액 (왕수) 등이 사용되어 왔다. 상기 ITO 등의 습식에칭제는 패턴 형성시에 알루미늄(Al) 등에서의 부식이 일어나고 또한 입자경계로부터 선택적 에칭이 진행되기 때문에, 가공정도가 우수한 패턴형성도 곤란하다.Conventionally, ferric chloride / aqueous hydrochloric acid, aqueous solution of iodic acid, aqueous phosphate, aqueous hydrochloric acid / nitric acid (aqua regia), and the like have been used as an etchant for transparent conductive films such as the polycrystalline ITO film. Wet etching agents, such as ITO, cause corrosion in aluminum (Al) and the like at the time of pattern formation, and selective etching proceeds from the grain boundary, thus making it difficult to form patterns with excellent processing accuracy.
이상의 이유에 의해, 기판 크기의 대형화, TFT 패널의 대형화, 고정밀화, 알루미늄제 배선 등에 수반하여, 화소 표시전극으로서 가공정도가 양호하고 에칭가능한 에칭제에 대한 요구가 높아지고 있다. 이러한 문제를 해결하기 위하여, 최근 비정질 ITO를 사용하고, 약산, 특히 옥살산수용액으로 비정질 ITO를 습식에칭하는 방법이 제안되고 있다.For the above reasons, along with the increase in the size of the substrate, the increase in the size of the TFT panel, the high precision, the wiring made of aluminum, and the like, there is a demand for an etching agent having a high degree of processing as an pixel display electrode and capable of etching. In order to solve this problem, a method of wet etching an amorphous ITO with a weak acid, in particular an oxalic acid solution, has recently been proposed.
그러나, 옥살산 수용액을 사용하여 비정질 ITO를 습식에칭했을 때에, 에칭 잔류물이 발생하는 문제가 있어서 이러한 에칭잔류물을 발생하지 않는 에칭제가 요망된다.However, when wet etching amorphous ITO using an aqueous oxalic acid solution, there is a problem in that etching residues are generated, and therefore, an etching agent that does not generate such etching residues is desired.
본 발명의 목적은 종래 기술에 있어서의 상기와 같은, 비정질 ITO를 옥살산 수용액을 이용한 습식에칭시에 에칭잔류물이 전혀 발생하지 않고 또한 온화한 조건하에 에칭을 행할 수 있는 습식에칭제를 제공하는 것이다.An object of the present invention is to provide a wet etching agent capable of etching under mild conditions without generating any etching residues in wet etching of amorphous ITO in the prior art using an aqueous solution of oxalic acid.
본 발명자 등은 상기의 문제를 해결하기 위해 예의 검토한 결과, 옥살산과 계면활성제인 폴리옥시에틸렌 알킬에테르 황산염 및/또는 폴리옥시에틸렌 알킬페닐에테르 황산염을 함유하는 수용액이 비정질 ITO 에칭시 온화한 조건하에서 에칭할 수 있고, 또한 잔류물이 전혀 발생하지 않는 사실을 발견하고, 이러한 발견에 의거하여 본 발명을 완성하기에 이른 것이다. MEANS TO SOLVE THE PROBLEM As a result of earnestly examining in order to solve the said problem, the aqueous solution containing oxalic acid and polyoxyethylene alkyl ether sulfate which are surfactant, and / or polyoxyethylene alkylphenyl ether sulfate is etched under mild conditions at the time of amorphous ITO etching. It is possible to discover the fact that no residue is generated, and to complete the present invention based on this finding.
즉, 본 발명은 옥살산과 폴리옥시에틸렌 알킬에테르 황산염 및/또는 폴리옥시에틸렌 알킬페닐에테르 황산염을 함유한 수용액을 포함하는 것을 특징으로 하는 투명도전막용 습식에칭제 조성물에 관한 것이다.That is, the present invention relates to a wet etching agent composition for a transparent conductive film comprising an aqueous solution containing oxalic acid, polyoxyethylene alkyl ether sulfate and / or polyoxyethylene alkylphenyl ether sulfate.
본 발명에서 사용되는 옥살산의 농도는 0.01-10중량% 이며 0.01중량% 이하에서는 에칭속도가 늦고 또한 10중량% 이상에서는 에칭속도가 향상되지 않으므로 좋지 않다.The concentration of oxalic acid used in the present invention is 0.01-10% by weight and is not good because the etching rate is slow at 0.01% by weight or less and the etching rate is not improved at 10% by weight or more.
또, 본 발명에 사용되는 폴리옥시에틸렌 알킬에테르 황산염은 다음의 일반식[I] 으로 표시되고,Moreover, the polyoxyethylene alkyl ether sulfate used for this invention is represented by the following general formula [I],
화학식 [I]Formula [I]
(단, R은 탄소수 6-22의 알킬기, n은 1-500의 정수, M은 암모니아, 유기아민, 제4급 암모늄 염 또는 알칼리금속을 나타낸다)(Where R is an alkyl group having 6-22 carbon atoms, n is an integer of 1-500, M represents ammonia, an organic amine, a quaternary ammonium salt or an alkali metal)
구체적으로는 상품명으로서 에멀 20C (카오사제), 하이테놀325D (제일공업제약사제), 알스코프 AP-30, 알스코프 LE-240(동방화학사제), 선놀 605N (라이온사제) 등이 바람직하게 사용된다.Specifically, Emulsion 20C (manufactured by Cao Corporation), Hytenol 325D (manufactured by Cheil Industries Co., Ltd.), Alscope AP-30, Alscope LE-240 (manufactured by Toyo Chemical Co., Ltd.), and Sunol 605N (manufactured by Lion Corporation) are preferably used as trade names. do.
또한, 본 발명에 사용되는 폴리옥시에틸렌 알킬페닐에테르 황산염은 다음의 일반식[II] 으로 표시되고,In addition, the polyoxyethylene alkylphenyl ether sulfate used for this invention is represented by the following general formula [II],
화학식 [II]Formula [II]
(단, R은 탄소수 4-20의 알킬기, n은 1-500의 정수, M은 암모니아, 유기아민, 제4급 암모늄 염 또는 알칼리금속을 나타낸다)(Where R is an alkyl group having 4-20 carbon atoms, n is an integer of 1-500, M represents ammonia, an organic amine, a quaternary ammonium salt or an alkali metal)
구체적으로는 상품명으로서 하이테놀 N-08, 하이테놀 N-12 (제일공업제약사제), 에멀 NC-35 (카오사제) 등이 바람직하게 사용된다. Specifically, hytenol N-08, hytenol N-12 (manufactured by Cheil Industries, Ltd.), emulsion NC-35 (manufactured by Cao Corporation) and the like are preferably used as trade names.
상기 폴리옥시에틸렌 알킬에테르 황산염, 폴리옥시에틸렌 알킬페닐에테르 황산염은 단독으로도 혹은 2종 이상의 조합물로서 사용해도 좋으며 바람직한 농도는 0.0001-5중량% 이다.The polyoxyethylene alkyl ether sulfate and polyoxyethylene alkylphenyl ether sulfate may be used alone or as a combination of two or more thereof, and a preferable concentration is 0.0001-5% by weight.
상기 폴리옥시에틸렌 알킬에테르 황산염, 폴리옥시에틸렌 알킬페닐에테르 황산염의 농도가 0.0001중량% 이하이면 에칭시 잔류물이 발생하고 5중량% 이상이면 ITO 등의 투명도전막의 에칭속도가 저하되어 바람직하지 않다.If the concentration of the polyoxyethylene alkyl ether sulfate and polyoxyethylene alkylphenyl ether sulfate is 0.0001% by weight or less, residues occur during etching, and when 5% by weight or more, the etching rate of the transparent conductive film such as ITO decreases, which is not preferable.
본 발명에 따른 습식에칭제 조성물의 사용농도는 상온에서 90℃ 까지이고 사용시간은 1-30분 정도이다. 또한, 본 발명은 비정질 ITO 이외에 IZO (인듐-아연산화물) 등의 습식에칭에도 바람직하게 사용된다.The concentration of the wet etchant composition according to the present invention is up to 90 ° C. and the use time is about 1-30 minutes at room temperature. The present invention is also preferably used for wet etching of IZO (indium zinc oxide) in addition to amorphous ITO.
다음에, 본 발명을 실시예에 의거하여 구체적으로 설명하나, 이러한 실시예에 의해 하등 제한되는 것은 아니다.Next, although an Example demonstrates this invention concretely, it is not restrict | limited at all by this Example.
도 1은 유리기판 상에, 절연막인 SiN을 형성하고, 비정질 ITO를 더 형성하고, 비정질 ITO 위에 레지스트를 도포하고 현상한 후의 기판의 단면도; 및1 is a cross-sectional view of a substrate after forming SiN as an insulating film on the glass substrate, further forming amorphous ITO, and applying and developing a resist on the amorphous ITO; And
도 2은 도 1의 기판을 비교예 1에 기재된 에칭제로 에칭한 후, 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후의 상태도이다.FIG. 2 is a state diagram after the substrate of FIG. 1 is etched with the etchant described in Comparative Example 1, followed by further peeling the resist with a basic resist stripping solution.
실시예 1Example 1
도 1은 유리기판(1) 위에 절연막인 SiN(2)을 성막하고, 비정질 ITO(3)을 더 성막하고, 비정질 ITO 위에 레지스트를 도포하고, 현상을 행한 후의 기판의 단면도이다. 도 1에 도시된 기판을 사용하고, 3.4중량%의 옥살산과 0.01중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염(상품명: 하이테놀 N-08, 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하고, 40℃ 에서 2분간 에칭을 행하여 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트(4)를 박리한 후 수세하고, 건조하였다. SEM (전자현미경)으로 표면을 관찰한 결과 비정질 ITO는 양호하게 에칭되고 잔류물은 전혀 관찰되지 않았다.FIG. 1 is a cross-sectional view of a substrate after film formation of SiN (2), which is an insulating film, on the
비교예 1Comparative Example 1
실시예 1에서 사용한 기판을 3.4중량%의 옥살산을 함유하는 수용액인 에칭제를 사용하고, 40℃ 에서 2분간 에칭을 행하여 수세한 후, 건조하였다. 또한 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하였다. SEM 관찰 결과, 비정질 ITO는 에칭되었으나 도 2에서 보는 바와 같이 다수의 잔류물(5)이 관찰되었다.The substrate used in Example 1 was etched at 40 ° C. for 2 minutes using an etchant which is an aqueous solution containing 3.4% by weight of oxalic acid, and then dried. Furthermore, the resist was peeled off with a basic resist stripping solution and washed with water. As a result of SEM observation, amorphous ITO was etched but a large number of residues 5 were observed as shown in FIG.
비교예 2Comparative Example 2
1중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염 (상품명: 하이테놀 N-08, 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃ 에서 2분간 에칭을 행하고, 수세한 후 추가적으로 염기성 박리액으로 레지스트를 박리한 후 수세하고 건조하였다. SEM 관찰결과, 비정질 ITO는 거의 에칭되지 않았다.The substrate used in Example 1 was etched at 40 ° C. for 2 minutes using an etchant which is an aqueous solution containing 1% by weight of polyoxyethylene alkylphenyl ether sulfate (trade name: Hytenol N-08, manufactured by Cheil Industries). After washing with water, the resist was further peeled off with a basic stripping solution, followed by washing with water and drying. As a result of SEM observation, amorphous ITO was hardly etched.
실시예 2Example 2
옥살산 3.4중량%, 0.1중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염 (상품명: 하이테놀 N-12: 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃에서 2분간 에칭을 행하고 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하고 건조했다. SEM 관찰결과, 비정질 ITO는 양호하게 에칭되었고 잔류물도 전혀 관찰되지 않았다.The board | substrate used in Example 1 was used at 40 degreeC using the etching agent which is the aqueous solution containing 3.4 weight% of oxalic acid and 0.1 weight% of polyoxyethylene alkylphenyl ether sulfate (brand name: Hytenol N-12: the company make). After etching and washing with water for 2 minutes, the resist was further peeled off with a basic resist stripping solution, followed by washing with water and drying. As a result of SEM observation, amorphous ITO was well etched and no residue was observed.
실시예 3Example 3
옥살산 3.4중량%와, 0.1중량%의 폴리옥시에틸렌 알킬에테르 황산염 (상품명: 하이테놀 325D: 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃에서 2분간 에칭을 행하고 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하고 건조했다. SEM 관찰결과, 비정질 ITO는 양호하게 에칭되었고 잔류물도 전혀 관찰되지 않았다. The board | substrate used in Example 1 was used for 2 minutes at 40 degreeC using the etching agent which is an aqueous solution containing 3.4 weight% of oxalic acid and 0.1 weight% of polyoxyethylene alkyl ether sulfate (brand name: Hythenol 325D: the Cheil Industries). After etching and washing with water, the resist was further peeled off with a basic resist stripping solution, followed by washing with water and drying. As a result of SEM observation, amorphous ITO was well etched and no residue was observed.
실시예 4Example 4
옥살산 1.0중량%, 0.1중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염 (상품명: 하이테놀 N-12: 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃에서 2분간 에칭을 행하고 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하고 건조했다. SEM 관찰결과, 비정질 ITO는 양호하게 에칭되었고 잔류물도 전혀 관찰되지 않았다.The board | substrate used in Example 1 was used at 40 degreeC using the etching agent which is the aqueous solution containing 1.0 weight% of oxalic acid and 0.1 weight% of polyoxyethylene alkylphenyl ether sulfate (brand name: Hytenol N-12: the company make). After etching and washing with water for 2 minutes, the resist was further peeled off with a basic resist stripping solution, followed by washing with water and drying. As a result of SEM observation, amorphous ITO was well etched and no residue was observed.
실시예 5Example 5
옥살산 5.5중량%, 0.1중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염 (상품명: 하이테놀 N-12: 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃에서 2분간 에칭을 행하고 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하고 건조했다. SEM 관찰결과, 비정질 ITO는 양호하게 에칭되었고 잔류물도 전혀 관찰되지 않았다.The substrate used in Example 1 was used at 40 ° C. using an etchant which was an aqueous solution containing 5.5% by weight of oxalic acid and 0.1% by weight of polyoxyethylene alkylphenylether sulfate (trade name: Hytenol N-12: manufactured by Cheil Industries). After etching and washing with water for 2 minutes, the resist was further peeled off with a basic resist stripping solution, followed by washing with water and drying. As a result of SEM observation, amorphous ITO was well etched and no residue was observed.
비교예 3Comparative Example 3
아세트산 5.5중량%, 0.1중량%의 폴리옥시에틸렌 알킬페닐에테르 황산염 (상품명: 하이테놀 N-12: 제일공업제약사제)를 함유하는 수용액인 에칭제를 사용하여 실시예 1에서 사용한 기판을 40℃에서 2분간 에칭을 행하고 수세한 후 추가적으로 염기성 레지스트 박리액으로 레지스트를 박리한 후 수세하고 건조했다. SEM 관찰결과, 비정질 ITO는 거의 에칭되어 있지 않았다.The substrate used in Example 1 was used at 40 ° C. using an etchant which was an aqueous solution containing 5.5% by weight of acetic acid and 0.1% by weight of polyoxyethylene alkylphenylether sulfate (trade name: Hytenol N-12: manufactured by Cheil Industries). After etching and washing with water for 2 minutes, the resist was further peeled off with a basic resist stripping solution, followed by washing with water and drying. As a result of SEM observation, almost no amorphous ITO was etched.
본 발명에 따른 에칭제 조성물을 사용하면 비정질 ITO 에칭시 온화한 조건하에서 에칭을 할 수 있고 또한 잔류물이 전혀 발생하지 않는다.Using the etchant composition according to the invention allows etching under mild conditions in amorphous ITO etching and no residue is generated.
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| CN101792907A (en) * | 2010-04-01 | 2010-08-04 | 江阴市江化微电子材料有限公司 | Aluminium-molybdenum etching liquid |
| CN102241985A (en) * | 2011-04-29 | 2011-11-16 | 西安东旺精细化学有限公司 | Wet etching solution composition for transparent conductive film |
| CN103472968A (en) * | 2013-09-26 | 2013-12-25 | 无锡宇宁光电科技有限公司 | Capacitive screen technology capable of realizing multi-point touch control by single layer of film |
| JP6485357B2 (en) * | 2013-10-30 | 2019-03-20 | 三菱瓦斯化学株式会社 | Etching solution and etching method of oxide substantially consisting of zinc, tin and oxygen |
| WO2015104962A1 (en) * | 2014-01-07 | 2015-07-16 | 三菱瓦斯化学株式会社 | Etching liquid for oxide containing zinc and tin, and etching method |
| CN104388090B (en) * | 2014-10-21 | 2017-05-17 | 深圳新宙邦科技股份有限公司 | Oxalic acid-series ITO (Indium Tin Oxide) etching liquid, as well as preparation method and application thereof |
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| JP2000008184A (en) * | 1998-06-24 | 2000-01-11 | Toppan Printing Co Ltd | Multilayer conductive film etching method |
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