CN101989646B - 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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- CN101989646B CN101989646B CN2009101837690A CN200910183769A CN101989646B CN 101989646 B CN101989646 B CN 101989646B CN 2009101837690 A CN2009101837690 A CN 2009101837690A CN 200910183769 A CN200910183769 A CN 200910183769A CN 101989646 B CN101989646 B CN 101989646B
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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 no longer of display device be confined to complanation, and provides polynary profile, can process 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; Realize flexible the demonstration more easily, and be 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 P MOLED 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, high, the waterproof oxygen excellent performance of surface flatness, but the elasticity of glass is not enough, does not reach the degree of crook that needs, and in manufacturing process, is prone to break.(2) mostly plastic substrate is organic polymer, and pliability is enough good, is at present by the substrate material of the F-PMOLED of extensive employing.But its poor flatness, rat bring defective can for the device film layer structure, and the water oxygen permeability is high, 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; Like 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 the substrate of promptly making through electroforming process, this substrate need not can have than the better surface smoothness of stainless steel through grinding and polishing.Simultaneously, on insulating barrier, increased protective layer, 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 present invention provides a kind of flexible passive organic electroluminescent device that adopts novel substrate, and the surface smoothness of this substrate is high, need not complicated abrasive polishing process.The object of the invention can be realized through following technical scheme:
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.
Can find out from Fig. 1-4, compare that 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 with stainless steel substrates.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 redistributed; Make the light that has only 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 through resonant cavity, makes luminous energy 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 AFM picture before for the electroformed nickel plate;
Fig. 2 is coated with layer of cloth AFM picture before for stainless steel substrates;
Fig. 3 is coated with layer of cloth AFM picture afterwards for the electroformed nickel plate;
Fig. 4 is coated with layer of cloth AFM 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 sketch map of the embodiment of the invention 1;
Figure 10 is the device architecture sketch map of the embodiment of the invention 2.
Wherein, description of reference numerals is following:
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, like 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, like metal organic complex (like 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 (like rubrene), Coumarins (like DMQA, C545T) or two pyrans class (like 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, like 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 (like Alq
3, Gaq
3, Al (Saph-q), BAlq or Ga (Saph-q)), aromatic condensed ring class (like pentacene 、 perylene) or o-phenanthroline class (like Bphen, BCP) compound.
Hole transmission layer, the material of use are generally the low molecular material of the arylamine class and the branch polymer same clan, like 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, promptly on insulating barrier, has increased protective layer.
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 vapor deposition prepares anode, again vapor deposition 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 vapor deposition deposits Ag as anode 3 on insulating barrier, and thickness is 300～500nm.
(5) with the method for vapor deposition 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) with the Li of the method for vapor deposition deposition 0.5nm
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 up 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 that the washing agent of heat is ultrasonic to be cleaned with the ultrasonic method of deionized water, places in the cleaning oven baking dry then.
(2) with the method for vapor deposition 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) deposited by evaporation method
MgAg thick alloy layer and
thick Ag film as a cathode.
(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 up 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.Can find out from Fig. 5, Fig. 6, depress in same electrical that the brightness of embodiment 1 device is depressed in same electrical apparently higher than Comparative Examples 1 device, the current density of embodiment 1 device also is higher than Comparative Examples 1 device, and illustrative 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.As can beappreciated from fig. 8 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.
In addition, the anode of embodiment 1 adopts the method for vapor deposition, 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 vapor deposition, 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) SiOx for preparing 100nm with the method for chemical vapour deposition (CVD) is as insulating barrier.
(4) epoxy resin that on insulating barrier, is coated with 1 μ m is as protective layer 9, baking-curing.
(5) method with vapor deposition deposits Ag as anode on insulating barrier, and thickness is 300～500nm.
(6) with the method for vapor deposition 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) with the Li of the method for vapor deposition deposition 0.5nm
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 up 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 technological personage, do not breaking away from the spirit and scope of the present invention, when doing various changes and retouching; Therefore, protection scope of the present invention is as the criterion when the claim with application defines.
Claims (11)
1. flexible passive organic electroluminescent device; This device comprises: substrate, insulating barrier, anode, organic function layer, negative electrode; It is characterized in that; Said substrate is the tinsel that electroforming forms, and said metal is selected from nickel, iron, copper, gold, silver, nickel-ferro alloy, platinum nickel-cobalt alloy, cobalt-tungsten alloy; The Rms value of the surface roughness of wherein said substrate is less than 10nm.
2. flexible passive organic electroluminescent device according to claim 1 is characterized in that, the thickness of said substrate is 20 μ m～700 μ m.
3. according to the arbitrary described flexible passive organic electroluminescent device of claim 1-2, it is characterized in that, go back matcoveredn on the said insulating barrier.
4. flexible passive organic electroluminescent device according to claim 3 is characterized in that, the material of said insulating barrier is polymer or inorganic molecules material.
5. flexible passive organic electroluminescent device according to claim 4 is characterized in that, the material of said insulating barrier is mixture, SiOx or the SiNx of polyimides, polytetrafluoroethylene, polyimides and polytetrafluoroethylene.
6. according to claim 4 or 5 described flexible passive organic electroluminescent devices, it is characterized in that said protective layer is a resin.
7. flexible passive organic electroluminescent device according to claim 6 is characterized in that, said protective layer is epoxy resin or acryl resin.
8. according to the flexible passive organic electroluminescent device of claim 7, it is characterized in that the thickness of said protective layer is 500nm-10 μ m.
9. according to the flexible passive organic electroluminescent device of claim 3, it is characterized in that the method preparation of said protective layer used coating.
10. 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.
11. the method for preparation according to claim 10 flexible passive organic electroluminescent device as claimed in claim 1 is characterized in that, said step prepares protective layer after also comprising the formation insulating barrier.
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| 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 |
| 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 |
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| JP2004050821A (en) * | 2002-05-30 | 2004-02-19 | Sumitomo Heavy Ind Ltd | Steam permeation preventing membrane and its manufacturing method |
| US20040053431A1 (en) * | 2002-09-13 | 2004-03-18 | Industrial Technology Research Institute | Method of forming a flexible thin film transistor display device with a metal foil substrate |
| US20060125387A1 (en) * | 2004-12-09 | 2006-06-15 | Masaya Adachi | Light emitting device, lighting device, and display device having light emitting device |
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| JP2004050821A (en) * | 2002-05-30 | 2004-02-19 | Sumitomo Heavy Ind Ltd | Steam permeation preventing membrane and its manufacturing method |
| US20040053431A1 (en) * | 2002-09-13 | 2004-03-18 | Industrial Technology Research Institute | Method of forming a flexible thin film transistor display device with a metal foil substrate |
| US20060125387A1 (en) * | 2004-12-09 | 2006-06-15 | Masaya Adachi | Light emitting device, lighting device, and display device having light emitting device |
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