CN1141859C - Preparation method of organic electroluminescent device - Google Patents
Preparation method of organic electroluminescent device Download PDFInfo
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- CN1141859C CN1141859C CNB011155191A CN01115519A CN1141859C CN 1141859 C CN1141859 C CN 1141859C CN B011155191 A CNB011155191 A CN B011155191A CN 01115519 A CN01115519 A CN 01115519A CN 1141859 C CN1141859 C CN 1141859C
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Abstract
The present invention discloses a method for manufacturing an organic electroluminescent device. An invented trapezoidal insulating column (isolating column) with a large upper part and a small lower part is manufactured on a first electrode pattern of the device. Then, an organic layer and a metal layer are orderly formed by vapor deposition. A second electrode of the device is effectively divided by the shadow effect of the insulating column. The inverted trapezoidal insulating column is manufactured by the following steps: rotating and coating an insulating polymer film twice, exposing once and developing twice. The present invention has the advantages of simple technology, low cost and high finished product ratio.
Description
Technical field
The present invention relates to a kind of preparation method of organic electroluminescence device, belong to electronic semi-conductor's components and parts technical field.
Background technology
Organic electroluminescence device usually like this constitutes: first electrode (transparency electrode) of printing opacity, be deposited on the organic electroluminescent medium on first electrode and be positioned at second electrode (metal electrode) above the organic electroluminescent medium.Transparency electrode is as the anode of device, and metal electrode is as the negative electrode of device.Apply high level to transparency electrode, apply low level to metal electrode and make device luminous.One group of anode parallel to each other (negative electrode) constitutes two-dimentional X-Y addressing matrix with one group of vertical with it negative electrode parallel to each other (anode).
The pattern wiring of normally transparent electrode is realized by photoetching technique.The pattern wiring of metal electrode adopts the method for metal mask evaporation or the method for photoetching to realize.But the complex manufacturing technology of metal mask plate, cost height in the pattern wiring of metal electrode, lines are difficult for running business into particular one, and realize having difficulties on the high-resolution at device.Metal mask plate contacts with organic membrane and destroys organic layer easily simultaneously, causes the short circuit between transparency electrode and the metal electrode.If carry out metal line with the method for photoetching, can have following problem again: 1. the baking temperature of photoresist (as 120 ℃) can make organic membrane be damaged; 2. the solvent of photoresist, developer solution, corrosive liquid can damage organic membrane; 3. if adopt dry etching, the organic membrane of can breaking of particle flux wherein.More than these destructive factors all can make the device property deterioration.
Japanese patent application JP10106747 (open day: adopt the insulated column technology to carry out the pattern wiring of metal electrode on April 24th, 1998).Device architecture such as Fig. 1: deposit transparent conductive film 2 on transparency carrier 1 makes transparent conductive film 2 by lithography one group of array that is parallel to each other.On transparent conductive film 2, adopt the method for plasma chemical enhancement mode vapor deposition (PECVD) to prepare silicon nitride (SiN) 3, silicon dioxide (SiO continuously
2) 4, silicon nitride (SiN) 5.After applying photoresist on the silicon nitride 5, make by lithography one group with transparent conductive film 2 vertical element parallel to each other of quadrature mutually.Figure with silicon nitride 5 is a mask then, uses hydrofluoric acid (HF) wet etching to go out the figure of silicon dioxide 4.Last dry etching again goes out the figure of silicon nitride 3.Direct deposit organic layer and metal level on silicon nitride 3, silicon dioxide 4, silicon nitride 5 three-layer insulated films.Silicon nitride 3, silicon dioxide 4, silicon nitride 5 three-layer insulated films have the shape of similar inverted ladder type as the insulated column of device.Because shadow effect continues the evaporation organic layer on device and metal level does not form film at the side surface of insulated column, has guaranteed the electric insulation between the adjacent image point.But this scheme has following shortcoming:
(1) insulated column is made up of three layers of inoranic membrane (silicon nitride 3-silicon dioxide 4-silicon nitride 5), needs to adopt plasma enhanced chemical vapor deposition (PECVD) method deposition film.The PECVD apparatus expensive, film-forming process complexity, process conditions are wayward, cause that rate of finished products is low in large-scale production, cost is high;
(2) in the reacting furnace of PECVD equipment, need to feed silane, nitrogen and oxygen, form silicon nitride and silicon dioxide by chemical reaction.Silane is poisonous, and the reacting furnace of equipment and gas piping need perform seal operation.Gaseous emission should be noted environmental protection simultaneously.These work meetings increase production cost;
(3) the insulated column shape realizes by single exposure, wet etching silicon dioxide 4 and twice dry etching silicon nitride 3 and 5.Figure complicated process of preparation, process conditions are wayward, cause that rate of finished products is low in the large-scale production, cost is high.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of organic electroluminescence device, shortcomings such as, cost height low at the complex process, the rate of finished products that exist among the insulated column preparation technology in the past, a kind of simple effective method that twice rotation coating insulating polymer film, single exposure and twice development prepare insulated column that passes through is provided, has reached the purpose of simplifying technology, reducing cost.
The preparation method of the organic electroluminescence device that the present invention proposes may further comprise the steps:
(1) on transparent glass substrate or flexible base, board deposit transparent conductive film tin indium oxide (hereinafter to be referred as ITO) or zinc oxide (ZnO) etc. as first electrode of device, thickness is 70nm~230nm, the square resistance of conducting film is 10 Ω~60 Ω, on transparent conductive film, make one group of vertical element that is parallel to each other and separates then by lithography, the width (being live width) that makes first electrode is 220 μ m~600 μ m, gaps between electrodes (being the lines gaps) is 20 μ m~100 μ m, cleans through acetone ethanol;
(2) rotation simultaneously applies the ground floor insulating material on above-mentioned first electrode and gaps between electrodes, as plain edition polyimides, Photosensitive polyimides etc., the thickness of first insulating barrier is 2 μ m~4 μ m, toasts 20min~50min down at 100 ℃~240 ℃;
(3) continue rotation on above-mentioned first insulating barrier and apply second layer insulating material, as Photosensitive polyimides or negative photoresist etc., the thickness of second insulating barrier is 1.5 μ m~2.5 μ m, toasts 20min~40min down at 80 ℃~190 ℃;
(4) above-mentioned second insulating barrier is directly carried out photoetching, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, wherein developing time is 40s~120s, the width that makes second insulating barrier is 20 μ m~100 μ m, the gap is 250 μ m~600 μ m, toasts 10min~25min down at 110 ℃~180 ℃;
(5) figure with above-mentioned second insulating barrier is a mask, first insulating barrier is developed, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, developing time is 45s~120s, the edge that makes first insulating barrier is than the inside 2 μ m~15 μ m of contraction in the edge of second insulating barrier, the width of first insulating barrier upper end is 16 μ m~70 μ m, the gap is 254 μ m~630 μ m, first insulating barrier and second insulating barrier form the up big and down small trapezoidal insulated column that falls together, above-mentioned two insulating barriers are toasted, baking temperature is 95 ℃~250 ℃, and the time is 20min~40min;
(6) on above-mentioned second insulating barrier and removed evaporation organic function layer on the transparent conductive film of two-layer insulating polymer and the transparent conductive film lines gap, organic function layer can be made up of single or multiple lift, single layer structure by three (oxine) aluminium (hereinafter to be referred as Alq
3) or N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines compositions such as (hereinafter to be referred as NPB), sandwich construction is successively by ketone phthalocyanine (hereinafter to be referred as CuPc), NPB and Alq
3Or successively by CuPc, NPB, Alq
3: 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino styryl)-4H-pyrans compositions such as (hereinafter to be referred as DCM), the evaporation speed of organic function layer is 0.1nm/s~0.4nm/s, and the thickness of CuPc is 7nm~25nm, and the thickness of NPB is 35nm~40nm, Alq
3Thickness be 40nm~70nm, DCM is at Alq
3In doping be 8%;
(7) evaporated metal layer on above-mentioned organic function layer, as be followed successively by Mg-Ag alloy and Ag or be followed successively by LiF and Al etc. as second electrode of device, the thickness of Mg-Ag alloy is 100nm~150nm, the thickness of Ag is 50nm~70nm, the thickness of LiF is 0.5nm, and the thickness of Al is 150nm.
The preparation method of organic electroluminescence device provided by the invention has the following advantages:
(1) insulated column is made up of two-layer dielectric film, and by rotation painting method preparation, film-forming process is simple, and rate of finished products height, cost are low in large-scale production;
(2) the insulated column shape realizes that by single exposure, twice development figure preparation technology is simple, easy control of process conditions, and rate of finished products height, cost are low in large-scale production, are particularly useful for the preparation of high-resolution dot matrix screen.
The metal level of device prepared by this method can be separated effectively by insulated column, and device is luminous evenly, and it is low to open bright voltage.
Description of drawings
Fig. 1 is the section of structure of organic electroluminescence device in the prior art.
Fig. 2 is the section of structure of organic electroluminescence device among the present invention.
Fig. 3 is the vertical view of organic electroluminescence device among the present invention.
Fig. 4 a-Fig. 4 d is the preparation flow figure (part sectioned view of AA direction among Fig. 3) of isolating column of organic electroluminescent device among the present invention.
Among above-mentioned Fig. 1~Fig. 4, the 1st, transparency carrier, 2 is first electrodes, the 3rd, silicon nitride, the 4th, silicon dioxide, the 5th, silicon nitride, the 6th, organic function layer, 7 is second electrodes, and 8 is first insulating barriers, and 9 is second insulating barriers.
Embodiment
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 200nm, and square resistance is 15 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is 220 μ m, the lines gap is 20 μ m.Rotation applies the first insulating barrier plain edition polyimides after acetone ethanol is cleaned, and thickness is 3 μ m, rotates behind the baking 20min to apply the second insulating barrier Photosensitive polyimides in 240 ℃ convection oven again, and thickness is 1.5 μ m.In 190 ℃ convection oven, toast 20min.The Photosensitive polyimides is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 40s, and live width is 20 μ m, and the lines gap is 250 μ m.In 180 ℃ convection oven, toast 10min once more.Figure with the Photosensitive polyimides is that mask develops to ground floor plain edition polyimide film, prolonging developing time makes the edge of ground floor plain edition polyimides than the inside 2 μ m of contraction in the edge of second layer Photosensitive polyimides, developing time is 45s, live width is 16 μ m, the lines gap is 254 μ m, so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 250 ℃, time 20min.After the preparation of insulated column figure is finished, continue evaporation organic function layer and metal level.Organic function layer is successively by CuPc, NPB and Alq
3Form, thickness is respectively 7nm, 35nm and 40nm.Metal level is made up of Mg-Ag alloy and Ag successively, and thickness is respectively 150nm and 50nm.The evaporation speed of organic function layer is 0.1nm/s, and the evaporation speed of Mg-Ag alloy and Ag is 0.6nm/s.It is 3V that device opens bright voltage, luminous even.
Embodiment 2
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 70nm, and square resistance is 60 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is 600 μ m, the lines gap is 100 μ m.Rotation applies the first insulating barrier plain edition polyimides after acetone ethanol is cleaned, and thickness is 4 μ m, rotates behind the baking 30min to apply the second insulating barrier negative photoresist in 220 ℃ convection oven again, and thickness is 2.5 μ m.In 150 ℃ convection oven, toast 30min.Negative photoresist is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 90s, and live width is 100 μ m, and the lines gap is 600 μ m.In 160 ℃ convection oven, toast 20min once more.Figure with negative photoresist is that mask develops to ground floor plain edition polyimide film, prolonging developing time makes the edge of ground floor plain edition polyimides than the inside 15 μ m of contraction in the edge of second layer negative photoresist, developing time is 120s, live width is 70 μ m, lines gap 630 μ m are so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 140 ℃, and the time is 40min.After the preparation of insulated column figure is finished, continue evaporation organic function layer and metal level.Organic function layer is successively by CuPc, NPB and Alq
3Form, thickness is respectively 25nm, 40nm and 70nm.Metal level is made up of LiF and Al successively, and thickness is respectively 0.5nm and 150nm.The evaporation speed of organic function layer is 0.3nm/s, the evaporation speed 0.2nm/s of LiF, and the evaporation speed of Al is 1.2nm/s.It is 3.5V that device opens bright voltage, luminous even.
Embodiment 3
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 230nm, and square resistance is 10 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is 400 μ m, the lines gap is 40 μ m.Rotation applies the first insulating barrier Photosensitive polyimides after acetone ethanol is cleaned, and thickness is 2 μ m, rotates behind the baking 50min to apply the second insulating barrier negative photoresist in 100 ℃ convection oven again, and thickness is 2 μ m.In 80 ℃ convection oven, toast 40min.Negative photoresist is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 120s, and live width is 40 μ m, and the lines gap is 400 μ m.In 110 ℃ convection oven, toast 25min once more.Figure with negative photoresist is that mask develops to ground floor Photosensitive polyimide film, prolonging developing time makes the edge of ground floor Photosensitive polyimides than the inside 5 μ m of contraction in the edge of second layer negative photoresist, developing time is 60s, live width is 30 μ m, the lines gap is 410 μ m, so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 95 ℃, and the time is 30min.After the preparation of insulated column figure is finished, continue evaporation organic function layer and metal level.Organic function layer is successively by CuPc, NPB and Alq
3: DCM forms, and thickness is respectively 15nm, 40nm and 60nm.DCM is at Alq
3In doping be 8%.Metal level is made up of Mg-Ag alloy and Ag successively, and thickness is respectively 100nm and 70nm.The evaporation speed of organic function layer is 0.4nm/s, and the evaporation speed of Mg-Ag alloy and Ag is 1nm/s.It is 4V that device opens bright voltage, luminous even.
Claims (7)
1, a kind of preparation method of organic electroluminescence device is characterized in that this method may further comprise the steps:
(1) on transparency carrier the deposit transparent conductive film as first electrode of device, thickness is 70nm~230nm, the square resistance of conductive film is 10 Ω~60 Ω, on transparent conductive film, make one group of vertical element that is parallel to each other and separates then by lithography, the width that makes first electrode is 220 μ m~600 μ m, and gaps between electrodes is 20 μ m~100 μ m;
(2) rotation simultaneously applies the ground floor insulating material on above-mentioned first electrode and gaps between electrodes, and the thickness of first insulating barrier is 2 μ m~4 μ m, toasts 20min~50min down at 100 ℃~240 ℃;
(3) continue rotation on above-mentioned first insulating barrier and apply second layer insulating material, the thickness of second insulating barrier is 1.5 μ m~2.5 μ m, toasts 20min~40min down at 80 ℃~190 ℃;
(4) above-mentioned second insulating barrier is carried out photoetching, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, wherein developing time is 40s~120s, the width that makes second insulating barrier is 20 μ m~100 μ m, the gap is 250 μ m~600 μ m, toasts 10min~25min down at 110 ℃~180 ℃;
(5) figure with above-mentioned second insulating barrier is a mask, first insulating barrier is developed, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, developing time is 45s~120s, the edge that makes first insulating barrier is than the inside 2 μ m~15 μ m of contraction in the edge of second insulating barrier, the width of first insulating barrier upper end is 16 μ m~70 μ m, the gap is 254 μ m~630 μ m, first insulating barrier and second insulating barrier form the up big and down small trapezoidal insulated column that falls together, above-mentioned two insulating barriers are toasted, baking temperature is 95 ℃~250 ℃, and the time is 20min~40min;
(6) on above-mentioned second insulating barrier and removed evaporation organic function layer on the transparent conductive film of two-layer insulating polymer and the transparent conductive film lines gap, the evaporation speed of organic function layer is 0.1nm/s~0.4nm/s:
(7) evaporated metal layer is as second electrode of device on above-mentioned organic function layer, and the evaporation speed of metal level is 0.2nm/s~1.2nm/s, is organic electroluminescence device.
2, preparation method as claimed in claim 1 is characterized in that wherein said first electrode is tin indium oxide or zinc oxide.
3, preparation method as claimed in claim 1 is characterized in that wherein said ground floor insulating material is plain edition polyimides or Photosensitive polyimides.
4, preparation method as claimed in claim 1 is characterized in that wherein said second layer insulating material is Photosensitive polyimides or negative photoresist.
5, preparation method as claimed in claim 1 is characterized in that wherein said organic function layer is a single layer structure, and material is three (oxine) aluminium or N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines.
6, preparation method as claimed in claim 1, it is characterized in that wherein said organic function layer is a sandwich construction, material is followed successively by the ketone phthalocyanine, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines and three (oxine) aluminium or be followed successively by the ketone phthalocyanine, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4, the 4-diamines, three (oxine) aluminium: 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino styryl)-4H-pyrans, the thickness of ketone peptide cyanines is 7nm~25nm, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4, the thickness of 4-diamines are 35nm~40nm, the thickness of three (oxine) aluminium is 40nm~70nm, and 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino the styryl)-doping of 4H-pyrans in three (oxine) aluminium is 8%.
7, preparation method as claimed in claim 1, it is characterized in that wherein said metal level is followed successively by Mg-Ag alloy and Ag or is followed successively by LiF and Al, the thickness of Mg-Ag alloy is 100nm~150nm, and the thickness of Ag is 50nm~70nm, the thickness of LiF is 0.5nm, and the thickness of Al is 150nm.
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Families Citing this family (13)
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JP3837344B2 (en) * | 2002-03-11 | 2006-10-25 | 三洋電機株式会社 | Optical element and manufacturing method thereof |
US6878208B2 (en) * | 2002-04-26 | 2005-04-12 | Tohoku Pioneer Corporation | Mask for vacuum deposition and organic EL display manufactured by using the same |
KR100465883B1 (en) * | 2002-05-03 | 2005-01-13 | 엘지.필립스 엘시디 주식회사 | The organic electro-luminescence device and method for fabricating of the same |
JP4173722B2 (en) | 2002-11-29 | 2008-10-29 | 三星エスディアイ株式会社 | Vapor deposition mask, organic EL element manufacturing method using the same, and organic EL element |
US20040163592A1 (en) * | 2003-02-20 | 2004-08-26 | Tohoku Poineer Corporation | Mask for vacuum deposition and organic EL display panel manufactured by using the same |
CN100372443C (en) * | 2004-07-06 | 2008-02-27 | 胜华科技股份有限公司 | Method for making display |
CN100496175C (en) * | 2005-11-24 | 2009-06-03 | 中国科学院微电子研究所 | A silicon-based organic luminescence micro-display metal anode and cathode insulation pole preparation method |
EP2073247B1 (en) | 2007-12-20 | 2011-08-31 | Canon Kabushiki Kaisha | Light-emitting substrate and display apparatus using the same |
CN102668706B (en) | 2009-11-17 | 2015-03-25 | 联合创新技术有限公司 | Organic el display |
CN102222684B (en) * | 2011-06-30 | 2013-08-07 | 信利半导体有限公司 | Organic electroluminescent display and manufacture method thereof |
CN103022375A (en) * | 2012-12-05 | 2013-04-03 | 昆山维信诺显示技术有限公司 | Organic light-emitting diode (OLED) device and preparation method thereof |
CN110456578A (en) * | 2019-08-13 | 2019-11-15 | 深圳市恒开源电子有限公司 | Liquid crystal writing film and liquid crystal writing film processing method based on evaporation process |
CN111180465B (en) * | 2020-01-03 | 2022-09-23 | 京东方科技集团股份有限公司 | Display panel, preparation method and display device |
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