KR20050020800A - Method of cleaning chamber of vacuum evaporation apparatus for production of organic el element - Google Patents
Method of cleaning chamber of vacuum evaporation apparatus for production of organic el element Download PDFInfo
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- KR20050020800A KR20050020800A KR10-2004-7018211A KR20047018211A KR20050020800A KR 20050020800 A KR20050020800 A KR 20050020800A KR 20047018211 A KR20047018211 A KR 20047018211A KR 20050020800 A KR20050020800 A KR 20050020800A
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- fluorine
- compound
- chamber
- containing alcohol
- organic
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 37
- 238000004140 cleaning Methods 0.000 title claims description 19
- 238000007738 vacuum evaporation Methods 0.000 title 1
- 150000001875 compounds Chemical class 0.000 claims abstract description 37
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011737 fluorine Substances 0.000 claims abstract description 26
- JUGSKHLZINSXPQ-UHFFFAOYSA-N 2,2,3,3,4,4,5,5-octafluoropentan-1-ol Chemical compound OCC(F)(F)C(F)(F)C(F)(F)C(F)F JUGSKHLZINSXPQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007740 vapor deposition Methods 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 12
- 238000001704 evaporation Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 150000002894 organic compounds Chemical class 0.000 claims description 6
- 229960003540 oxyquinoline Drugs 0.000 claims description 6
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 125000001153 fluoro group Chemical group F* 0.000 claims description 5
- 239000007983 Tris buffer Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 150000004696 coordination complex Chemical class 0.000 claims description 4
- NBUKAOOFKZFCGD-UHFFFAOYSA-N 2,2,3,3-tetrafluoropropan-1-ol Chemical compound OCC(F)(F)C(F)F NBUKAOOFKZFCGD-UHFFFAOYSA-N 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims description 2
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 claims description 2
- 239000002994 raw material Substances 0.000 description 19
- 239000010409 thin film Substances 0.000 description 18
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- 239000010408 film Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- CXENHBSYCFFKJS-OXYODPPFSA-N (Z,E)-alpha-farnesene Chemical compound CC(C)=CCC\C(C)=C\C\C=C(\C)C=C CXENHBSYCFFKJS-OXYODPPFSA-N 0.000 description 1
- FCEUVAQYYKMPRC-UHFFFAOYSA-N 2,2,3,3,4,4-hexafluorobutan-1-ol Chemical compound OCC(F)(F)C(F)(F)C(F)F FCEUVAQYYKMPRC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- -1 benzoquinolinol aluminum Chemical compound 0.000 description 1
- UFVXQDWNSAGPHN-UHFFFAOYSA-K bis[(2-methylquinolin-8-yl)oxy]-(4-phenylphenoxy)alumane Chemical compound [Al+3].C1=CC=C([O-])C2=NC(C)=CC=C21.C1=CC=C([O-])C2=NC(C)=CC=C21.C1=CC([O-])=CC=C1C1=CC=CC=C1 UFVXQDWNSAGPHN-UHFFFAOYSA-K 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Electroluminescent Light Sources (AREA)
- Physical Vapour Deposition (AREA)
Abstract
유기 EL 소자를 제조할 때 챔버 내표면에 축적되어 폐기되었던 Alq3 등의 화합물을 회수, 재이용함으로써 제조 비용을 저감한다. Alq3 등의 화합물이 부착된 챔버 내의 표면 또는 챔버 내의 부재를, 2,2,3,3,4,4,5,5-옥타플루오로펜탄올 등의 불소함유 알코올을 사용해 세정하여 Alq3 을 회수한다.The manufacturing cost is reduced by recovering and reusing compounds such as Alq 3 that have been accumulated and discarded on the inner surface of the chamber when the organic EL device is manufactured. The surface of the chamber or a member in the chamber to which a compound such as Alq 3 is attached is washed with a fluorine-containing alcohol such as 2,2,3,3,4,4,5,5-octafluoropentanol to thereby remove Alq 3 . Recover.
Description
본 발명은, 유기 EL 소자 제조용 증착장치의 챔버 세정방법에 관한 것이다.This invention relates to the chamber cleaning method of the vapor deposition apparatus for organic electroluminescent element manufacture.
유기 EL 소자의 제조에 있어서, 유기 화합물 (이하, 원료라고도 함) 의 박막을 형성하는 방법으로서 진공 증착법이 알려져 있다. 진공 증착법은 진공조 내에서 증발원과 막형성용 기판을 적당히 조합하여 박막을 형성하는 방법으로, 스핀 코트법이나 딥 법 등의 웨트 프로세스에 비하여 균질한 박막을 얻기 쉽다는 등의 이점이 있다. 진공 증착법으로는, 비교적 전기저항이 높은 금속용기 (금속 보드) 에 원료를 부착시키고, 그 금속용기에 전류를 흘려보냄으로써 그 금속용기를 발열시키고 원료를 증발시켜 막형성용 기판 표면에 원료의 박막을 형성하는 저항 가열 증착법이나, 원료에 전자빔이나 레이저빔을 조사하고 그 빔의 에너지로 원료를 증발시켜 막형성용 기판 표면에 원료의 박막을 형성하는 전자빔ㆍ레이저빔 증착법 등이 알려져 있다. 그 중에서도 저항 가열 증착법은, 증착장치의 구성이 간편하고 싼 가격으로 양질의 박막형성을 실현할 수 있다는 점에서 널리 보급되어 있다.In the manufacture of an organic EL element, the vacuum vapor deposition method is known as a method of forming the thin film of an organic compound (henceforth a raw material). The vacuum evaporation method is a method of forming a thin film by appropriately combining an evaporation source and a film forming substrate in a vacuum chamber, and has an advantage of easily obtaining a homogeneous thin film as compared to a wet process such as a spin coat method or a dip method. In the vacuum evaporation method, a raw material is attached to a metal container (metal board) having a relatively high electrical resistance, and a current is flowed through the metal container to generate heat and evaporate the metal container to form a thin film of the raw material on the surface of the film-forming substrate. The resistive heating vapor deposition method which forms the film | membrane, the electron beam, the laser beam vapor deposition method which irradiates an electron beam or a laser beam to a raw material, and evaporates a raw material by the energy of the beam, and forms a thin film of a raw material on the film formation substrate surface is known. Among them, the resistive heating evaporation method is widely used in that the structure of the evaporation apparatus is simple and a high quality thin film can be realized at a low price.
상기 증착법에 사용되는 장치의 경우, 증발된 원료는 일부가 유기 EL 소자용 기판 표면에 퇴적하고, 나머지 원료는 증착장치의 챔버 내표면이나 그 챔버 내에 배치된 부재의 표면에 축적된다. 따라서, 유기 EL 소자용 기판 표면의 박막을 형성하는 원료는 원료 전체의 일부이며, 대부분은 챔버 내표면 등에 부착되어 이용되지 않은 상태로 폐기되는 문제가 있다. 유기 EL 소자의 원료는 비싼 화합물이 많이 때문에, 원료를 효율적으로 사용할 수 없다면 소자의 제조 비용이 높아지는 문제도 있다. 또, 그 챔버를 다른 원료의 막형성에 사용한 경우, 챔버 내표면에 축적된 원료가 불순물로서 막 중에 혼입됨으로써 막이 오염되는 문제가 있다.In the apparatus used for the vapor deposition method, part of the evaporated raw material is deposited on the surface of the substrate for the organic EL element, and the remaining raw material is accumulated on the inner surface of the chamber of the vapor deposition apparatus or on the surface of the member disposed in the chamber. Therefore, the raw material for forming the thin film on the surface of the organic EL element substrate is a part of the whole raw material, and most of the raw material adheres to the inner surface of the chamber or the like and is disposed of unused. Since the raw material of an organic electroluminescent element has many expensive compounds, when the raw material cannot be used efficiently, there also exists a problem that manufacturing cost of an element becomes high. In addition, when the chamber is used for film formation of other raw materials, there is a problem that the film is contaminated by mixing raw materials accumulated on the inner surface of the chamber as impurities in the film.
본 발명자들은 상기 문제를 해결할 목적으로, 증착장치의 챔버의 내표면이나 그 챔버 내에 배치된 부재의 표면에 부착된 유기 화합물을 유기용제를 사용해 세정하여 회수하는 방법에 관해서 예의 검토하였다.MEANS TO SOLVE THE PROBLEM In order to solve the said problem, the present inventors earnestly examined the method which wash | cleans and collect | recovers the organic compound adhering to the inner surface of the chamber of a vapor deposition apparatus, or the surface of the member arrange | positioned in the chamber using an organic solvent.
상기 방법을 실시하기 위해서는, 상기 유기 화합물에 대하여 어느 정도의 용해성을 갖는 유기용제를 사용하여 세정할 필요가 있다고 생각되지만, 일반적으로 유기 EL 소자의 제조 원료로서 사용되는 화합물을 용해할 수 있는 유기용제는 한정된다.In order to perform the said method, it is thought that it is necessary to wash | clean using the organic solvent which has a some solubility with respect to the said organic compound, but the organic solvent which can melt | dissolve the compound generally used as a raw material of manufacture of an organic EL element. Is limited.
예를 들어, 상기 유기 화합물로서 트리스(8-히드록시퀴놀리나토)알루미늄 (이하, Alq3 이라 함) 이 있는데, Alq3 을 용해할 수 있는 유기용제로는 클로로포름이 알려져 있으나 클로로포름과 같은 하이드로클로로카본은 오존 파괴 계수가 높다는 등의 문제가 있다.For example, tris (8-hydroxyquinolinato) aluminum (hereinafter referred to as Alq 3 ) is an organic compound, and an organic solvent capable of dissolving Alq 3 is known as chloroform, but hydrochloro such as chloroform. Carbon has a problem such as high ozone destruction coefficient.
본 발명은, 유기 EL 소자 제조용 증착장치의 챔버 세정방법으로서, 유기 EL 소자를 제조할 때 챔버 내표면에 축적되어 폐기되었던 원료를 재이용함으로써 제조 비용을 절감하고, 또한 챔버 내표면에 축적된 원료가 불순물로서 제품인 박막 중에 혼입되는 것을 방지하며, 또한 오존 파괴 등의 환경 문제를 갖지 않기 위한 방법의 제공을 과제로 한다.The present invention provides a chamber cleaning method for a deposition apparatus for manufacturing an organic EL element, which reduces manufacturing costs by reusing raw materials accumulated and disposed on the inner surface of the chamber when the organic EL element is manufactured. It is an object of the present invention to provide a method for preventing mixing into a thin film as a product and preventing environmental problems such as ozone destruction.
본 발명은, 증착장치의 챔버 내에서, 기판 표면에 8-히드록시퀴놀린 또는 그 유도체의 금속착물로 이루어지는 화합물을 증착하는 유기 EL 소자 제조용 증착장치의 챔버 세정방법으로서, 기재 표면에 상기 화합물이 증착되는 동시에, 상기 화합물이 부착된 챔버의 내표면 또는 챔버 내에 배치된 부재의 표면을 불소함유 알코올로 세정하여 부착된 상기 화합물을 제거하는 공정 및 상기 화합물을 함유하는 불소함유 알코올을 회수하는 공정을 구비하는 것을 특징으로 하는 유기 EL 소자 제조용 증착장치의 챔버 세정방법을 제공한다.The present invention provides a chamber cleaning method for a deposition apparatus for manufacturing an organic EL device, in which a compound consisting of a metal complex of 8-hydroxyquinoline or a derivative thereof is deposited on a substrate surface in a chamber of a deposition apparatus, wherein the compound is deposited on a substrate surface. And at the same time, cleaning the inner surface of the chamber to which the compound is attached or the surface of the member disposed in the chamber with a fluorine-containing alcohol to remove the attached compound and recovering the fluorine-containing alcohol containing the compound. The chamber cleaning method of the vapor deposition apparatus for organic electroluminescent element manufacture characterized by the above-mentioned.
(발명을 실시하기 위한 최선의 형태)(The best mode for carrying out the invention)
본 발명에 있어서는, 기재 표면에 8-히드록시퀴놀린 또는 그 유도체의 금속착물로 이루어지는 화합물이 증착되는 동시에, 해당 화합물이 부착된 챔버의 내표면 또는 챔버 내에 배치된 부재의 표면을 세정한다.In the present invention, a compound consisting of a metal complex of 8-hydroxyquinoline or a derivative thereof is deposited on the surface of the substrate, and at the same time, the inner surface of the chamber to which the compound is attached or the surface of the member disposed in the chamber is cleaned.
상기 화합물로는, 구체적으로는 Alq3 (트리스(8-히드록시퀴놀리나토)알루미늄), Almq3 (Alq3 에 전자 공여성 메틸기를 도입한 유도체), Alph3 (벤조퀴놀리놀알루미늄 착물), Znq2 (8-히드록시퀴놀린의 Zn 과의 4배위 착물), BAlq1 등을 들 수 있다.Specific examples of the compound include Alq 3 (tris (8-hydroxyquinolinato) aluminum), Almq 3 (a derivative in which an electron donating methyl group is introduced into Alq 3 ), and Alph 3 (benzoquinolinol aluminum complex) , Znq 2 (quadrate complex with Zn of 8-hydroxyquinoline), BAlq 1 and the like.
본 발명에서는, 세정제로서 불소함유 알코올을 사용한다. 불소함유 알코올은 Alq3 의 용해성이 우수하고, 불연성 또는 난연성이어서 취급이 용이하고, 수지나 금속 등으로 이루어지는 유기 EL 소자 제조용 증착장치를 구성하는 부재에 대한 영향이 거의 없는 등의 이점을 갖는다.In the present invention, a fluorine-containing alcohol is used as the cleaning agent. The fluorine-containing alcohol has advantages such as excellent solubility of Alq 3 , nonflammability or flame retardancy, and easy handling, and little effect on members constituting the vapor deposition apparatus for producing an organic EL device made of resin, metal, or the like.
본 발명에서 사용되는 불소함유 알코올로는, 예를 들어 하기 화학식 1 로 표시되는 화합물을 들 수 있다.As a fluorine-containing alcohol used by this invention, the compound represented by following formula (1) is mentioned, for example.
[화학식 1][Formula 1]
RfCHX-OHR f CHX-OH
상기 화학식 1 에 있어서 X 는 수소원자, 불소원자 또는 트리플루오로메틸기, Rf 는 불소원자 또는 탄소수 1∼4 의 폴리플루오로알킬기이다. 폴리플루오로알킬기란 알킬기의 수소원자 2개 이상이 불소원자로 치환된 기를 말한다. 폴리플루오로알킬기는 직쇄 구조일 수도 있고 분기 구조일 수도 있다.In Formula 1, X is a hydrogen atom, a fluorine atom or a trifluoromethyl group, and R f is a fluorine atom or a polyfluoroalkyl group having 1 to 4 carbon atoms. The polyfluoroalkyl group refers to a group in which two or more hydrogen atoms of an alkyl group are substituted with fluorine atoms. The polyfluoroalkyl group may be linear or branched.
식 1 로 나타내는 화합물의 구체예로는, 예를 들어 이하의 화합물을 들 수 있다.As a specific example of a compound represented by Formula 1, the following compounds are mentioned, for example.
H(CF2)2CH2OH(2,2,3,3-테트라플루오로프로판올),H (CF 2 ) 2 CH 2 OH (2,2,3,3-tetrafluoropropanol),
H(CF2)3CH2OH(2,2,3,3,4,4-헥사플루오로부탄올)H (CF 2 ) 3 CH 2 OH (2,2,3,3,4,4-hexafluorobutanol)
H(CF2)4CH2OH(2,2,3,3,4,4,5,5-옥타플루오로펜탄올),H (CF 2 ) 4 CH 2 OH (2,2,3,3,4,4,5,5-octafluoropentanol),
(CF3)2CHOH(1,1,1,3,3,3-헥사플루오로이소프로판올).(CF 3 ) 2 CHOH (1,1,1,3,3,3-hexafluoroisopropanol).
이들 화합물은 특히 Alq3 의 용해성이 우수한 점에서 바람직하다.These compounds are particularly preferred from the viewpoint of excellent solubility of Alq 3.
또, 본 발명에서의 불소함유 알코올로는, 용해도 파라미터 (δ값) 가 8 이상 20 이하인 것이 바람직하고, 특히 9 이상 15 이하, 나아가서는 10 이상 12 이하인 것이 바람직하다. 예를 들어, 상기 서술한 식 1 로 나타내는 화합물의 용해도 파라미터 (δ값) 는 이하와 같다.Moreover, as a fluorine-containing alcohol in this invention, it is preferable that solubility parameter (delta value) is 8 or more and 20 or less, It is especially preferable that it is 9 or more and 15 or less, Furthermore, it is 10 or more and 12 or less. For example, the solubility parameter (delta value) of the compound represented by Formula 1 mentioned above is as follows.
본 발명에 있어서, 불소함유 알코올은 1종을 단독으로 사용할 수도 있고, 2종 이상의 혼합물로서 사용해도 된다.In the present invention, the fluorine-containing alcohol may be used alone, or may be used as a mixture of two or more thereof.
본 발명의 세정방법을 적용할 수 있는 유기 EL 소자를 제조하기 위해 사용되는 증착장치로는, 저항 가열 증착장치, 전자빔 증착장치, 레이저빔 증착장치 등의 진공 증착장치를 들 수 있다. 그 중에서도, 본 발명의 세정방법은 저항 가열 증착장치의 세정에 사용한 경우에 효과적이라고 생각된다. 증착장치의 챔버 내에는 유기 화합물의 증발원, 막두께 센서, 기판유지 기구, 메탈 섀도우 마스크 등의 부재가 배치되는데, 이들 부재가 세정되는 대상이 된다.As a vapor deposition apparatus used to manufacture the organic electroluminescent element which can apply the washing | cleaning method of this invention, a vacuum vapor deposition apparatus, such as a resistance heating vapor deposition apparatus, an electron beam vapor deposition apparatus, and a laser beam vapor deposition apparatus, is mentioned. Especially, it is thought that the washing | cleaning method of this invention is effective when used for the washing | cleaning of a resistive heating vapor deposition apparatus. In the chamber of the vapor deposition apparatus, members such as an evaporation source of an organic compound, a film thickness sensor, a substrate holding mechanism, a metal shadow mask, and the like are disposed, and these members are subjected to cleaning.
다음에, 본 발명의 세정방법을 실시하기 위한 순서를 구체적으로 설명한다. 8-히드록시퀴놀린 또는 그 유도체의 금속착물로 이루어지는 화합물의 박막 형성공정에서, 증착장치의 챔버 내에 있는 증발원에서 상기 화합물을 증발시킨다. 증발한 상기 화합물은 유기 EL 소자를 제조하기 위한 기판 상에 부착되는 동시에 상기 챔버의 내표면이나 챔버 내에 배치된 부재의 표면에도 부착된다.Next, the procedure for implementing the cleaning method of the present invention will be described in detail. In a thin film formation process of a compound consisting of a metal complex of 8-hydroxyquinoline or a derivative thereof, the compound is evaporated from an evaporation source in the chamber of the deposition apparatus. The evaporated compound is attached to the substrate for producing the organic EL device and also to the inner surface of the chamber or the surface of the member disposed in the chamber.
상기 화합물이 부착된 챔버의 내표면이나 부재의 표면에 불소함유 알코올을 접촉시켜 상기 화합물을 제거한다. 제거방법으로는, 스프레이 노즐 등으로부터 불소함유 알코올을 분사하여 챔버의 내표면 및 부재의 표면에 내뿜어 제거하는 방법을 들 수 있다.The compound is removed by bringing a fluorine-containing alcohol into contact with the inner surface of the chamber to which the compound is attached or the surface of the member. As a removal method, the method of spraying a fluorine-containing alcohol from a spray nozzle etc. and spraying it on the inner surface of a chamber and the surface of a member is mentioned.
이어서, 얻어진 상기 화합물을 함유하는 불소함유 알코올을 회수한다.Subsequently, the fluorine-containing alcohol containing the obtained compound is recovered.
회수된 상기 화합물을 함유하는 불소함유 알코올을, 상기 화합물과 불소함유 알코올로 분리한다. 분리방법으로는 상압 또는 감압 하에서 유기용제를 증발시키는 방법을 들 수 있다.The fluorine-containing alcohol containing the recovered compound is separated into the compound and the fluorine-containing alcohol. As a separation method, the method of evaporating an organic solvent under normal pressure or a reduced pressure is mentioned.
분리, 회수된 상기 화합물은 유기 EL 소자의 박막 형성재료로서 다시 사용할 수 있는 순도까지 정제하는 것이 바람직하다. 정제방법으로는, 재결정 정제, 액체 크로마토그래프 정제, 승화 정제 등의 정제방법을 들 수 있다. 정제는 클린 룸 또는 냉암소에서 실시하는 것이 바람직하다. 상기 화합물에 대해서는, 정제한 후, 추가로 메타노스 환류 하에서 불순물을 추출, 제거하는 조작을 실시할 수도 있다.It is preferable to refine | purify the said separated and collect | recovered compound to the purity which can be used again as a thin film formation material of organic electroluminescent element. As a purification method, purification methods, such as recrystallization refinement | purification, a liquid chromatograph refinement, and a sublimation refinement | purification, are mentioned. Purification is preferably carried out in a clean room or cool dark place. About the said compound, after refine | purifying, the operation which further extracts and removes an impurity under metanose reflux may be performed.
이하에 본 발명의 세정방법을 구체적으로 설명하는데, 본 발명은 이들에 의해 한정되지 않는다.Although the washing | cleaning method of this invention is demonstrated concretely below, this invention is not limited by these.
공정 1 : 유기 EL 소자를 제조하기 위해 사용된 증착장치의 챔버 내에 설치된 스프레이 노즐로부터 불소함유 알코올을 분사하여, Alq3 이 부착된 챔버 내표면 및 챔버 내의 부재 표면을 세정한다.Step 1: A fluorine-containing alcohol is sprayed from a spray nozzle installed in a chamber of a vapor deposition apparatus used for producing an organic EL element, and the surface of the chamber in which Alq 3 is attached and the member surface in the chamber are cleaned.
공정 2 : Alq3 을 함유하는 불소함유 알코올을 챔버의 바닥에서 빼내어 회수조에 회수한다.Step 2: The fluorine-containing alcohol containing Alq 3 is removed from the bottom of the chamber and recovered in a recovery tank.
공정 3 : 회수한 Alq3 을 함유하는 불소함유 알코올을 감압으로 하고, 불소함유 알코올을 증발시키고 Alq3 을 농축하여 석출시킨다.Step 3: The fluorine-containing alcohol containing recovered Alq 3 is reduced under reduced pressure, the fluorine-containing alcohol is evaporated, and Alq 3 is concentrated to precipitate.
공정 4 : 석출된 Alq3 을 Alq3 에 대하여 적절한 용해능을 갖는 용제, 예를 들어 염화메틸렌에 용해시켜 Alq3 용액을 얻는다.Step 4: The precipitated Alq 3 is dissolved in a solvent having an appropriate solubility for Alq 3 , for example methylene chloride, to obtain an Alq 3 solution.
공정 5 : Alq3 용액을 냉각시켜 용해된 Alq3 을 석출시킨다. 냉각 온도는 바람직하게는 -30℃∼20℃, 보다 바람직하게는 -15℃∼18℃ 이다. 냉각 시간은 바람직하게는 30분∼2시간, 보다 바람직하게는 45분∼1시간 30분이다.Step 5: The Alq 3 solution is cooled to precipitate dissolved Alq 3 . Cooling temperature becomes like this. Preferably it is -30 degreeC-20 degreeC, More preferably, it is -15 degreeC-18 degreeC. Cooling time becomes like this. Preferably it is 30 minutes-2 hours, More preferably, it is 45 minutes-1 hour 30 minutes.
공정 6 : 석출된 Alq3 을 여과하여 건조시킴으로써 Alq3 을 회수한다. 건조 온도는 40∼60℃ 가 바람직하고, 45∼55℃ 가 보다 바람직하다. 건조 시간은 10∼40시간이 바람직하고 12∼35 시간이 보다 바람직하다.Step 6: Alq 3 is recovered by filtering and drying the precipitated Alq 3 . 40-60 degreeC is preferable and, as for a drying temperature, 45-55 degreeC is more preferable. 10-40 hours are preferable and, as for drying time, 12-35 hours are more preferable.
[예 1][Example 1]
불소함유 알코올에 대한 Alq3 의 용해성에 대하여 이하의 방법으로 확인하였다.The solubility of Alq 3 in the fluorine-containing alcohol was confirmed by the following method.
25℃ 에서, Alq3 1㎎ 과 H(CF2)4CH2OH 3㎖ 를 혼합하여 이루어지는 혼합액을 조제하였다. 혼합상태를 육안으로 확인한 결과, Alq3 은 완전히 용해되어 있는 것이 확인되었다.At 25 ° C, a mixed solution obtained by mixing 1 mg of Alq 3 and 3 ml of H (CF 2 ) 4 CH 2 OH was prepared. As a result of visual inspection of the mixed state, it was confirmed that Alq 3 was completely dissolved.
[예 2][Example 2]
유기박막 형성장치 챔버의 내표면 및 마스크 등의 지그 표면에 부착된 유기 EL 소자용 재료인 트리스(8-히드록시퀴놀리나토)알루미늄(Alq3) 이 부착된 유기박막 형성장치 챔버 내표면 및 마스크 등의 부재 표면에, 그 증착장치 내의 스프레이노즐로부터 H(CF2)4CH2OH(2,2,3,3,4,4,5,5-옥타플루오로펜타놀, 이하 OFPO 라 함) 을 500㎖/min 으로 5분간 분사하여 그 유기박막 형성장치 챔버 내를 세정한다. 세정에 사용한 OFPO, 즉 Alq3 을 함유하는 OFPO (이하, OFPO 용액이라 함) 를 유기박막 형성장치의 바닥에서 유기박막 형성장치의 하부에 설치한 회수조로 빼내어 회수한다. 회수한 OFPO 용액을 130hPa, 80℃ 의 조건 하에서 OFPO 를 증발시킨다. OFPO 를 증발시킨 잔류물을 10㎖ 의 염화메틸렌에 30℃ 에서 용해시켜 염화메틸렌 용액을 조제한다. 염화메틸렌 용액을 -10℃ 로 냉각하여 1시간 방치한다. 석출된 화합물을 여과하여 건조시킴으로써 Alq3 이 얻어진다. 회수한 Alq3 은 유기 EL 소자의 박막층의 형성재료로서 사용할 수 있는 순도를 갖는다.Inner surface and mask of organic thin film forming apparatus with tris (8-hydroxyquinolinato) aluminum (Alq 3 ) attached to the inner surface of the organic thin film forming chamber and jig surfaces such as masks. H (CF 2 ) 4 CH 2 OH (2,2,3,3,4,4,5,5-octafluoropentanol, hereinafter referred to as OFPO) from the spray nozzle in the vapor deposition apparatus thereof Is sprayed at 500 ml / min for 5 minutes to clean the inside of the organic thin film forming apparatus chamber. OFPO used for washing, that is, OFPO containing Alq 3 (hereinafter referred to as OFPO solution), is taken out of the bottom of the organic thin film forming apparatus and collected by a recovery tank provided in the lower part of the organic thin film forming apparatus. OFPO solution is evaporated under conditions of 130 hPa and 80 ° C of the recovered OFPO solution. The residue from which OFPO was evaporated is dissolved in 10 ml of methylene chloride at 30 ° C. to prepare a methylene chloride solution. The methylene chloride solution is cooled to -10 占 폚 and left for 1 hour. Alq 3 is obtained by filtering and drying the precipitated compound. The recovered Alq 3 has a purity that can be used as a material for forming a thin film layer of an organic EL device.
[예 3]Example 3
OFPO 대신에 H(CF2)2CH2OH(2,2,3,3-테트라플루오로프로판올) 을 사용한 것 이외에는 예 2 와 동일하게 하여 Alq3 이 부착된 유기박막 형성장치 챔버 내표면 및 마스크 등의 부재 표면을 세정한다. 이로써 상기 Alq3 을 회수하여 재이용할 수 있다.Inner surface and mask of the organic thin film forming apparatus with Alq 3 in the same manner as in Example 2 except that H (CF 2 ) 2 CH 2 OH (2,2,3,3-tetrafluoropropanol) was used instead of OFPO. The surface of the member such as the back is cleaned. As a result, the Alq 3 can be recovered and reused.
유기 EL 소자를 제조할 때 챔버 내표면에 축적되어 폐기되었던 원료를 재이용함으로써 제조 비용을 저감하고, 또한 챔버 내표면에 축적된 원료가 불순물로서 제품인 박막 중에 혼입되는 것을 방지할 수 있다. 또한, 본 발명의 세정방법은 오존 파괴 등의 환경 문제를 갖지 않는다.The manufacturing cost can be reduced by reusing raw materials accumulated on the inner surface of the chamber and discarded when manufacturing the organic EL element, and it is possible to prevent the raw materials accumulated on the inner surface of the chamber from being mixed in the thin film as a product as impurities. In addition, the cleaning method of the present invention does not have environmental problems such as ozone destruction.
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