CN101989646A - Flexible passive organic electroluminescent device and production method thereof - Google Patents
Flexible passive organic electroluminescent device and production method thereof Download PDFInfo
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- CN101989646A CN101989646A CN2009101837690A CN200910183769A CN101989646A CN 101989646 A CN101989646 A CN 101989646A CN 2009101837690 A CN2009101837690 A CN 2009101837690A CN 200910183769 A CN200910183769 A CN 200910183769A CN 101989646 A CN101989646 A CN 101989646A
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Abstract
The invention discloses a flexible passive organic electroluminescent device and a production method thereof, relating to a flexible organic electroluminescent device and particularly to a substrate of a flexible passive organic electroluminescent device. In the invention, the substrate used has the advantages of good flexibility, high smoothness and excellent water-oxygen isolation property, and can ensure that the flexible organic electroluminescent device has favorable property and longer service life.
Description
Technical field
The present invention relates to a kind of flexible organic electroluminescent device (Flexible Organic Light EmittingDiode, hereinafter to be referred as FOLED) structure, relate in particular to the substrate of a kind of flexible passive organic electroluminescent device (Flexible Passive Matrix Organic Light Emitting Diode is hereinafter to be referred as F-PMOLED).
Background technology
Flexible display technologies makes the design of display device no longer be confined to complanation, and provides polynary profile, can make e-newspaper that people dream of, wall TV, wearable display etc.The soft deformability of these flexible display devices, and not fragile.Another key factor of exploitation flexible display device is, the manufacturing process of display device can convert Roll-to-Roll Manufacturing (scroll bar formula processing procedure) to by Sheet-fed Batch Processing (load formula processing procedure in batches), so, the manufacturing cost of display can significantly reduce.Therefore, flexible display technologies becomes the international research focus that shows industry day by day.
Organic electroluminescence device (Organic Light Emitting Diode, hereinafter to be referred as OLED) as the full display device that solidifies, do not contain the material of any liquid state, compare with liquid crystal device, easier realization is flexible to be shown, and is that active illuminating, visual angle are wide, response is fast.Difference according to its type of drive can be divided into passive drive (Passive Matrix Organic Light Emitting Diode, hereinafter to be referred as PMOLED) and active driving (ActiveMatrix Organic Light Emitting Diode is hereinafter to be referred as AMOLED).Traditional PMOLED cooks substrate with glass, if replace existing substrate with flexible substrate, then becomes F-PMOLED, realizes flexible the demonstration.
The device architecture of F-PMOLED is generally substrate/anode/organic function layer/negative electrode, and organic function layer comprises luminescent layer, can also comprise electron transfer layer, hole transmission layer etc.Substrate is because have very big relevance and playing the part of very important role with device cost, display quality, reliability, process etc.At present, the material of F-PMOLED substrate mainly contains three kinds of ultra-thin glass, plastics, sheet metal, when adopting metal substrate, will increase insulating barrier between substrate and the anode.When glass or plastics were cooked substrate, light appeared from substrate one side, was the end luminous (bottom emission); When metal was cooked substrate, because of the opaqueness of metal, light appeared from negative electrode one side, was top luminous (top emission).But no matter adopt which kind of substrate, also there are a lot of problems in F-PMOLED in aspect of performance and preparation process:
(1) glass substrate has good light transmittance, surface flatness height, waterproof oxygen excellent performance, but the elasticity of glass is not enough, does not reach the degree of crook that needs, and easily breaks in manufacturing process.(2) mostly plastic substrate is organic polymer, and pliability is enough good, is the substrate material of the F-PMOLED that is widely adopted at present.But its poor flatness, rat bring defective can for the device film layer structure, water oxygen permeability height, cause device aging rapidly.(3) metal substrate has excellent waterproof oxygen characteristic, and does not have splintering problem.For fear of getting rusty, adopt the material of stainless steel usually as metal substrate.But stainless surface roughness is big, unevenness, and through complicated grinding and electrochemical polish technology, surface smoothness is still good inadequately.
Insulating barrier adopts polymer or inorganic molecules material usually, and these materials can be destroyed by chemical substance in the subsequent technique process of device preparation, as the alkaline-based developer used in netted insulating base of etching or the insulated column process, the organic solvent etc. of luminescent material in the organic function layer, thereby influence life-span of entire device.
The inventor has adopted a kind of new type of metal substrate through concentrating on studies, and promptly by the substrate of electroforming process manufacturing, this substrate need not can have than the better surface smoothness of stainless steel through grinding and polishing.Simultaneously, increased protective layer on insulating barrier, the protection insulating layer material is not destroyed by alkali, organic solvent etc. in subsequent preparation process, and has further improved surface smoothness, has improved the performance of the organic function layer on it.
Summary of the invention
The invention provides a kind of flexible passive organic electroluminescent device that adopts novel substrate, the surface smoothness height of this substrate, need not complicated abrasive polishing process.Purpose of the present invention can be achieved through the following technical solutions:
Flexible passive organic electroluminescent device comprises substrate, insulating barrier, anode, organic function layer, negative electrode, and substrate is the tinsel that electroforming forms.
The material of substrate is selected from nickel, iron, copper, gold, silver, nickel-ferro alloy, platinum nickel-cobalt alloy, cobalt-tungsten alloy, and thickness is 20 μ m to 700 μ m, and the Rms of surface roughness (rout mean square) is worth less than 10nm.Go back matcoveredn on the insulating barrier.The material of insulating barrier is polymer or inorganic molecules material, is preferably mixture, SiOx or the SiNx of polyimides, polytetrafluoroethylene, polyimides and polytetrafluoroethylene.The material of protective layer is a resin, is preferably epoxy resin or acryl resin.The thickness of protective layer is 500nm to 10um, with the method preparation of coating.
Another object of the present invention is to provide a kind of method for preparing flexible passive organic electroluminescent device, step comprises:
(1) electroforming forms tinsel;
(2) form insulating barrier;
(3) form anode, organic function layer, negative electrode successively;
(4) form encapsulated layer.
After above-mentioned steps can also be included in and form insulating barrier, the preparation protective layer.
From Fig. 1-4 as can be seen, compare with stainless steel substrates, the electroformed nickel plate is better at the surface smoothness that is coated with the insulating layer coating front and back, can not cause defective to the film layer structure of organic function layer.The metal that electroforming process is used usually such as copper, iron etc. equally also have good evenness.And the electroforming metal paillon foil is better than the water oxygen barrier performance of plastic substrate.Therefore, the electroforming metal paillon foil is done performance and the life-span that the substrate of F-PMOLED can improve device.
The electroformed nickel plate is when doing the substrate of F-PMOLED, because its opaqueness adopts the top ray structure during fabricate devices.In OLED,, resonant cavity effect is in various degree arranged all no matter be the luminous or end luminescent device in top.The microresonator effect is meant that mainly the photon density of different energy states is reallocated, make and have only the light of specific wavelength after meeting cavity modes, be able to penetrate, so the halfwidth of light wave (FWHM) also can narrow down in specific angle, also can be different at the intensity and the optical wavelength of different angles.In end illuminating OLED, negative electrode is translucent metal electrode, so light increases in the reflection of this electrode, and causes the multi-photon beam interferometer, so the microresonator effect is also just more obvious.The luminous zone is positioned at the resonant cavity of total reflection film and half reflection film formation, and light emits by resonant cavity, makes luminous energy be strengthened, and spectrum is narrowed, thereby obtains good color saturation.Use the F-PMOLED of electroformed nickel plate than the F-PMOLED that uses plastic substrate higher brightness to be arranged, higher efficient and purer colourity.
Simultaneously, protective layer prevents that effectively insulating layer material from being destroyed by alkali, organic solvent etc. in subsequent preparation process, and has further improved surface smoothness, has improved the performance of the organic function layer on it.
Description of drawings
Fig. 1 is coated with layer of cloth atomic force microscope picture before for the electroformed nickel plate;
Fig. 2 is coated with layer of cloth atomic force microscope picture before for stainless steel substrates;
Fig. 3 is coated with layer of cloth atomic force microscope picture afterwards for the electroformed nickel plate;
Fig. 4 is coated with layer of cloth atomic force microscope picture afterwards for stainless steel substrates;
Fig. 5 is the brightness-voltage relationship figure of the embodiment of the invention 1 and Comparative Examples 1 device;
Fig. 6 is the current density-voltage relationship figure of the embodiment of the invention 1 and Comparative Examples 1 device;
Fig. 7 is the current efficiency-current density graph of a relation of the embodiment of the invention 1 and Comparative Examples 1 device;
Fig. 8 is the spectrogram of the embodiment of the invention 1 and Comparative Examples 1 device;
Fig. 9 is the device architecture schematic diagram of the embodiment of the invention 1;
Figure 10 is the device architecture schematic diagram of the embodiment of the invention 2.
Wherein, description of reference numerals is as follows:
The 1-substrate, 2-insulating barrier, 3-anode, 4-hole injection layer, 5-hole transmission layer, 6-luminescent layer, 7-electron transfer layer, 8-negative electrode, 9-protective layer.
Embodiment
Insulating barrier can be polymer or inorganic molecules material, as mixture, SiOx or the SiNx of polyimides, polytetrafluoroethylene, polyimides and polytetrafluoroethylene.
Anode can adopt inorganic material or organic conductive polymer, and inorganic material is generally the higher metals of work function such as metal oxides such as ITO, zinc oxide, zinc tin oxide or gold, copper, silver; The organic conductive polymer is preferably polythiophene/polyvinylbenzenesulfonic acid sodium (being called for short PEDOT:PSS) or polyaniline (being called for short PANI).
Organic function layer comprises luminescent layer, can also comprise electron transfer layer, hole transmission layer etc.
Luminescent layer can adopt small molecule material, also can adopt polymeric material.The luminescent layer material can be fluorescent material, as metal organic complex (as Alq
3, Gaq
3, Al (Saph-q) or Ga (Saph-q)) compounds, can be doped with dyestuff in this small molecule material, doping content is the 0.01wt%～20wt% of small molecule material, and dyestuff is generally a kind of material in aromatic condensed ring class (as rubrene), Coumarins (as DMQA, C545T) or two pyrans class (as DCJTB, the DCM) compound.The luminescent layer material also can adopt phosphor material, and wherein carbazole derivates such as CBP, polyvinylcarbazole (PVK) they are material of main part, but Doping Phosphorus photoinitiator dye in this material of main part, as three (2-phenylpyridine) iridium (Ir (ppy)
3), two (2-phenylpyridine) (acetylacetone,2,4-pentanedione) iridium (Ir (ppy)
2(acac)), octaethylporphyrin platinum (PtOEP) etc.
Electron transfer layer, materials used are generally the micromolecule electron transport material, can be metal organic complex (as Alq
3, Gaq
3, Al (Saph-q), BAlq or Ga (Saph-q)), aromatic condensed ring class (as pentacene, perylene) or o-phenanthroline class (as Bphen, BCP) compound.
Hole transmission layer, the material that uses is generally the low molecular material of the arylamine class and the branch polymer same clan, as N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines (NPB), N, N '-diphenyl-N, N '-two (aminomethyl phenyl)-1,1 '-xenyl-4,4 '-diamines (TPD) etc.
Negative electrode generally adopts the composite construction of the less metal of work function, alloy or metal halide and metal, as: Al, Ag, Li, Mg, Ca, Ba, MgAg alloy or LiF/Al.Simultaneously, the light transmittance of at least one layer material in anode and the negative electrode will be got well.
The device architecture of F-PMOLED of the present invention can also be substrate/insulating barrier/protective layer/anode/organic function layer/negative electrode, has promptly increased protective layer on insulating barrier.
Concrete preparation method at first cleans substrate; spin coating or spray coating insulating layer material, protective layer material successively on substrate then; method with sputter or evaporation prepares anode, again evaporation hole transport layer material, luminescent layer material, electric transmission layer material and cathode material successively.
Present embodiment provides a kind of technical process that has adopted the copper coin of electroforming formation as the F-PMOLED of substrate, and device architecture is: electroforming copper coin/polyimides/Ag/HAT/NPB/Alq
3/ Li
3N/Ag.
(1) anode in the electrotyping bath is placed metallic copper, and negative electrode is placed the silicon chip that needs electroforming, contains NiSO in the electroplate liquid
4, NiCl
2, H
3BO
3, the electroforming temperature is 45～65 degrees centigrade.With potassium hydroxide silicon is eroded, the copper coin that obtains thickness and be 100 μ m is as substrate 1 again.
The washing agent of (2) utilization heat is ultrasonic to be cleaned the nickel plate with the ultrasonic method of deionized water, places baking drying in the cleaning oven then.
(3) process with spin coating prepares polyimide film as insulating barrier 2 on substrate, and thickness is 0.2～2 μ m, baking-curing.
(4) method with evaporation deposits Ag as anode 3 on insulating barrier, and thickness is 300～500nm.
(5) use the method for evaporation 3 * 10
-3The HAT that deposits 20nm in the vacuum chamber of Pa successively is as the NPB of hole injection layer 4, the 50nm Alq as hole transmission layer 5,50nm
3As green light emitting layer 6 and electron transfer layer 7.
(6) Li of the method deposition 0.5nm of usefulness evaporation
3The Ag of N and 30nm is as negative electrode 8.
(7) after the negative electrode preparation finishes, encapsulate with the plastic sheet (not shown), this plastic sheet contains the water oxygen barrier layer that is made of the compound insulating material of organic-inorganic.
The substrate of F-PMOLIED is light tight like this, and negative electrode is transparent, promptly from negative electrode one side bright dipping, is top illuminating device.
Comparative Examples 1
Comparative Examples one is that device architecture is with the technical process of plastics as the F-PMOLED of substrate: PET film/ITO/HAT/NPB/Alq
3/ Li
3N/Ag.
(1) thickness is the ITO that sputter has 250nm on the PET film of 120 μ m, utilizes the method that washing agent is ultrasonic and deionized water is ultrasonic of heat to clean, and places in the cleaning oven baking dry then.
(2) use the method for evaporation 3 * 10
-3The HAT that deposits 20nm in the vacuum chamber of Pa successively is as the NPB of hole injection layer, the 50nm Alq as hole transmission layer, 50nm
3As green light emitting layer and electron transfer layer.
(3) method with evaporation deposits
Thick MgAg alloy-layer and
Thick Ag film is as negative electrode.
(4) after the negative electrode preparation finishes, encapsulate with the plastic sheet (not shown), this plastic sheet contains the water oxygen barrier layer that is made of the compound insulating material of organic-inorganic.
The plastic substrate of F-PMOLIED and anode ITO are transparent like this, and negative electrode is opaque, promptly from anode one side bright dipping, is end luminescent device.
The performance comparison of the foregoing description 1 and Comparative Examples 1 is shown in accompanying drawing 5-8.From Fig. 5, Fig. 6 as can be seen, depress in same electrical, the brightness of embodiment 1 device is depressed in same electrical apparently higher than Comparative Examples 1 device, and the current density of embodiment 1 device also is higher than Comparative Examples 1 device, illustrates that embodiment 1 device more helps the injection of electronics.As can be seen from Figure 7 the light extraction efficiency of embodiment 1 device is more than 2 times of Comparative Examples 1 device light extraction efficiency obviously greater than Comparative Examples 1 device under identical electric current.The half-peak breadth of the emission wavelength of Comparative Examples 1 device is obviously greater than the half-peak breadth of the emission wavelength of embodiment 1 device, so the luminescent chromaticity of embodiment 1 device is purer than the luminescent chromaticity of Comparative Examples 1 device as can be seen from Figure 8.
In addition, the anode of embodiment 1 adopts the method for evaporation, and is consistent with the process of organic function layers such as follow-up hole transmission layer, luminescent layer.And the transparent anode ITO of Comparative Examples 1 can't use the method for evaporation, can only sputter.Therefore, the technology of embodiment 1 is simpler, reduces chamber and switches link, has improved throughput rate.
Present embodiment provides a kind of manufacture process that has adopted the nickel of electroforming growth as the F-PMOLED of substrate equally:
(1) anode in the electrotyping bath is placed metallic nickel, and negative electrode is placed the silicon chip that needs electroforming, contains NiSO in the electroplate liquid
4, NiCl
2, H
3BO
3, the electroforming temperature is 45～65 degrees centigrade.With potassium hydroxide silicon is eroded, obtaining thickness is the nickel plate of 20 μ m again.
The washing agent of (2) utilization heat is ultrasonic to be cleaned the nickel plate with the ultrasonic method of deionized water, places baking drying in the cleaning oven then.
(3) method with chemical vapour deposition (CVD) prepares the SiOx of 100nm as insulating barrier.
(4) on insulating barrier, be coated with the epoxy resin of 1 μ m as protective layer 9, baking-curing.
(5) method with evaporation deposits Ag as anode on insulating barrier, and thickness is 300～500nm.
(6) use the method for evaporation 3 * 10
-3The HAT that deposits 20nm in the vacuum chamber of Pa successively is as the NPB of hole injection layer, the 50nm Alq as hole transmission layer, 50nm
3As green light emitting layer and electron transfer layer.
(7) Li of the method deposition 0.5nm of usefulness evaporation
3The Ag of N and 30nm is as negative electrode.
(8) after the negative electrode preparation finishes, encapsulate with the plastic sheet (not shown), this plastic sheet contains the water oxygen barrier layer that is made of the compound insulating material of organic-inorganic.
Though the present invention discloses as above with preferred embodiment; yet it is not in order to limit the present invention; anyly be familiar with this technology personage; without departing from the spirit and scope of the present invention; when being used for a variety of modifications and variations; therefore, protection scope of the present invention is as the criterion when the claim with application defines.
Claims (13)
1. flexible passive organic electroluminescent device, this device comprises: substrate, insulating barrier, anode, organic function layer, negative electrode is characterized in that described substrate is the tinsel that electroforming forms.
2. flexible passive organic electroluminescent device according to claim 1 is characterized in that, described metal is selected from nickel, iron, copper, gold, silver, nickel-ferro alloy, platinum nickel-cobalt alloy, cobalt-tungsten alloy.
3. flexible passive organic electroluminescent device according to claim 2 is characterized in that, the thickness of described substrate is 20 μ m～700 μ m.
4. flexible passive organic electroluminescent device according to claim 2 is characterized in that, the Rms value of the surface roughness of described substrate is less than 10nm.
5. according to the arbitrary described flexible passive organic electroluminescent device of claim 1-4, it is characterized in that, go back matcoveredn on the described insulating barrier.
6. flexible passive organic electroluminescent device according to claim 5 is characterized in that, the material of described insulating barrier is polymer or inorganic molecules material.
7. flexible passive organic electroluminescent device according to claim 6 is characterized in that, the material of described insulating barrier is mixture, SiOx or the SiNx of polyimides, polytetrafluoroethylene, polyimides and polytetrafluoroethylene.
8. according to claim 6 or 7 described flexible passive organic electroluminescent devices, it is characterized in that described protective layer is a resin.
9. flexible passive organic electroluminescent device according to claim 8 is characterized in that, described protective layer is epoxy resin or acryl resin.
10. according to the flexible passive organic electroluminescent device of claim 9, it is characterized in that the thickness of described protective layer is 500nm-10 μ m.
11. the flexible passive organic electroluminescent device according to claim 5 is characterized in that, the method preparation of described protective layer used coating.
12. a method for preparing flexible passive organic electroluminescent device as claimed in claim 1, step comprises:
(1) electroforming forms tinsel;
(2) form insulating barrier;
(3) form anode, organic function layer, negative electrode successively;
(4) form encapsulated layer.
13. the method for preparation according to claim 12 flexible passive organic electroluminescent device as claimed in claim 1 is characterized in that, described step prepares protective layer after also comprising the formation insulating barrier.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102709492A (en) * | 2012-06-13 | 2012-10-03 | 信利半导体有限公司 | Flexible organic electroluminescence display (OELD) and manufacture method thereof |
| CN103904250A (en) * | 2012-12-25 | 2014-07-02 | 海洋王照明科技股份有限公司 | Organic electroluminescent device and preparing method thereof |
| CN109659349A (en) * | 2019-01-11 | 2019-04-19 | 京东方科技集团股份有限公司 | A kind of array substrate and preparation method thereof, display device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004050821A (en) * | 2002-05-30 | 2004-02-19 | Sumitomo Heavy Ind Ltd | Steam permeation preventing membrane and its manufacturing method |
| TW548853B (en) * | 2002-09-13 | 2003-08-21 | Ind Tech Res Inst | Method of manufacturing flexible TFT display |
| JP2006164808A (en) * | 2004-12-09 | 2006-06-22 | Hitachi Ltd | Light emitting element, lighting system and display device having it |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102709492A (en) * | 2012-06-13 | 2012-10-03 | 信利半导体有限公司 | Flexible organic electroluminescence display (OELD) and manufacture method thereof |
| CN103904250A (en) * | 2012-12-25 | 2014-07-02 | 海洋王照明科技股份有限公司 | Organic electroluminescent device and preparing method thereof |
| CN109659349A (en) * | 2019-01-11 | 2019-04-19 | 京东方科技集团股份有限公司 | A kind of array substrate and preparation method thereof, display device |
| CN109659349B (en) * | 2019-01-11 | 2021-02-19 | 京东方科技集团股份有限公司 | Array substrate, preparation method thereof and display device |
| US11508939B2 (en) | 2019-01-11 | 2022-11-22 | Beijing Boe Technology Development Co., Ltd. | Array substrate having resonant cavity formed by reflective layer and cathode, manufacturing method thereof and display device |
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