CN101080121A - An organic EL part and its making method - Google Patents
An organic EL part and its making method Download PDFInfo
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- CN101080121A CN101080121A CN 200710118482 CN200710118482A CN101080121A CN 101080121 A CN101080121 A CN 101080121A CN 200710118482 CN200710118482 CN 200710118482 CN 200710118482 A CN200710118482 A CN 200710118482A CN 101080121 A CN101080121 A CN 101080121A
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Abstract
This invention relates to a package structure of an organic electroluminescent device and its manufacturing method, in which, the organic electroluminescent device includes a package structure with a flat packaged cover made of glass, polymer, metal or alloy material and its composite film material, and the flat package cover can be prepared by a roller extrusion method. The package structure is especially suitable for large size or soft OLED, since no gas space exists during the packaging process, the device can be made thinner and distortion of the cover can be avoided.
Description
Technical field
The present invention relates to encapsulating structure of a kind of organic electroluminescence device and preparation method thereof, belong to technical field of organic electroluminescence.
Background technology
Now, along with the arriving of Development of Multimedia Technology and information-intensive society, more and more higher to the flat-panel monitor performance demands.Newly occurred three kinds of Display Techniques in recent years: plasma display, Field Emission Display and display of organic electroluminescence (hereinafter to be referred as OLED) have all remedied the deficiency of cathode ray tube and LCD to a certain extent.Wherein, a series of advantages such as display of organic electroluminescence has from main light emission, low-voltage DC driven, solidifies entirely, the visual angle is wide, color is abundant, compare with LCD, display of organic electroluminescence does not need backlight, the visual angle is big, power is low, and its response speed can reach 1000 times of LCD, and its manufacturing cost but is lower than the LCD of equal resolution.Therefore, display of organic electroluminescence has broad application prospects, and is counted as the utmost point and composes one of following flat panel display of competitiveness.
The OLED product is technical from volume production, also do not reach at present the requirement of commercialization, realize the difficulty that the OLED volume production is faced, mainly contain the following aspects: the life problems of (1) OLED, (2) production technology and quality management problem, (3) correlation technique problem (particularly Driving technique), wherein, the life-span is one of greatest problem that faces at present.We can say that the life problems of OLED can not get corresponding solution, the commercialization and the practicability of the display of a new generation are not just known where to begin.At present, because organic substance in the device and negative electrode are all very responsive to steam and oxygen, the life problems of OLED depends on the quality of device package effect to a great extent in other words.A large amount of studies show that steam and oxygen are the main causes that cause OLED to lose efficacy, and are easy to and steam, oxygen reaction as the active metal of OLED negative electrode.We can do a simple estimation, and the atomic weight of Mg is 24, and density is 1.74g/cm
3If the thickness of the metallic cathode Mg layer among the OLED is 50nm, then the amount of this device containing metal Mg is 3.6 * 10
-7Mol/cm
2, only need about 6.4 * 10
-6G water is complete reaction with it just.Make that the complete destroyed time of Mg is 1 year, then encapsulated layer must make the water permeability less than 1.5 * 10
-4G/m
2/ day.As long as and in fact in the device negative electrode have 10% oxidized, the not light-emitting zone that forms is just very obviously (if the oxidation of negative electrode occurs in metal and at the interface organic, even only being 5 , ruined negative electrode also may cause component failure), it has been generally acknowledged that, ignore the destruction to organic layer of water, oxygen, the encapsulated layer water oxygen permeability that OLED requires should be less than 10
-5G/m
2/ day (Burrows PE, Graff GL, Gross ME, et al.Displays 22,65 2001).
Existing OLED method for packing is a helmet formula encapsulating structure, promptly uses metal or glass as cap, and adhesive is bonded together relative sealed space of formation at the edge that is coated on cap with cap and display screen; In order further to absorb steam, also need cap is made a groove, and xeraphium or drying sheet are filled in the groove of cap.This kind method for packing can well solve the injury to the OLED device of water, oxygen, but because entire display screen is to be made by two blocks of thick and heavy glass or metal, makes OLED lose its frivolous advantage; In addition, owing to have a groove on the cap, the center of cap certainly exists collapse-deformation, when the large-sized display screen of preparation, thisly subsides more obviously, and the pixel of the center of cap even the display screen that can rub is destroyed display screen; Because the variation of the gas pressure intensity in the groove produces a pressure difference with atmosphere, and then causes packaging plastic the crack to occur, destroy packaging effect in the process of subsiding.Simultaneously, this method for packing also can't be used for soft display and not be suitable for soft screen, because soft screen device is when bending, and the bonding case chip destruction metal level that might rub.Nowadays, OLED is as a kind of display device (no matter being micromolecule or polymer) of full curing, its prime advantage is to prepare flexible display device, flexible organic electroluminescent device refers to the flexible material to be the organic electroluminescence device of substrate, because the characteristics of flexible substrate have given unique application prospect just for this class device, as the display device of flexibility, flexible e-newspaper, the wallpaper TV, wearable display etc.
Be directed to above situation, thin-film package technology progressively development and perfect, its representative is the compound thin-film package technology of the organic-inorganic of Vitex company.The characteristics of its technology are at first to utilize organic material to form a smooth plane in the device back side, the inorganic thin film that then forms a densification on this plane is to reach the ability that intercepts water, oxygen, because single inorganic thin film layer can't obtain good barriering effect, encapsulated layer need be prepared into the structure that multilayer replaces.But the organic polymer and the inorganic ceramic class material that prepare a plurality of cycles, technology, equipment are all very complicated, ceramic-like materials particularly, the general methods such as magnetron sputtering, plasma enhanced chemical gaseous phase deposition that adopt prepare, temperature is higher in the preparation process, destroy the organic layer or the metal electrode of OLED device easily, and when object is bent, the material (as ceramic material) of bending ability comes off easily, and follow the mechanism of " tunnelling-layering-protuberance-fracture ", influence the life-span and the mechanical performance of device.Therefore, this technology exists preparation section, equipment complexity in production application, and technology difficulty increases, and rhythm of production is slow, shortcomings such as the cost height of preparation.
Summary of the invention
Emphasis of the present invention is at the problem that exists in the above-mentioned thin-film package technology, a kind of new encapsulating structure and method for packing are proposed, be particularly useful for large-sized OLED and flexible OLED, significantly to improve the life-span of utilizing the prepared device of thin-film package technology, simplify preparation technology simultaneously, reduce production costs.
The present invention proposes a kind of organic electroluminescence device, comprises substrate, anode, negative electrode and the organic function layer between two electrodes, also comprises encapsulating structure, has the planar package lid in this encapsulating structure.
Encapsulating structure is positioned at negative electrode one side of device, and is bonding by packaging plastic and device.
The material of planar package lid of the present invention is glass, polymer, metal or alloy material and composite film material thereof.Preferable material is a kind of in polyester (PET), polycarbonate (PC), polyether sulfone (PES), the poly (arylene ether nitrile) (PEN), a kind of in aluminium foil, steel foil, TiN/ steel foil sheet, the PET/ aluminium foil.
Packaging plastic among the present invention is selected from a kind of in UV glue, heat-curable glue, the AB glue.
Can also be doped with dry hygroscopic material in this packaging plastic.Dry hygroscopic material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, have at least a in the metal alcoholate of long-chain hydrocarbon.
Also comprise layer protecting film between packaging plastic in the encapsulating structure and the device, its material is selected from least a in organic small molecule material, inorganic material or the metal material, preferably a kind of in AlQ, CuPc, SiOx, AlOx, SiNxOy, TiN.
Also comprise one deck drying layer between planar package lid in the encapsulating structure and the device, its material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, has the metal alcoholate of long-chain hydrocarbon.
Also comprise one deck water, oxygen barrier layer between planar package lid in the encapsulating structure and the device, its material is selected from a kind of and composite construction in SiOx, AlOx, SiNxOy, TiN, polymethyl methacrylate, polyethyl methacrylate, epoxy resin, acrylate, the UV curing glue.
The substrate of organic electroluminescence device of the present invention can be flexibility, and its material is selected from plastics, tinsel or ultra-thin glass.
The present invention also provides the method for encapsulating structure in a kind of organic electroluminescence device, when the planar package lid is flexible material, encapsulation process comprises: device transmits, packaging plastic deposits, the planar package lid transmits, the planar package lid covers on the device, packaging plastic solidifies, and it is characterized in that it is to cover on the device by the drum extrusion method that planar package is covered.
It is that cylinder transmits that planar package lid described in the method for packing of the organic electroluminescence device among the present invention transmits.
Device transfer approach described in the method for packing of organic electroluminescence device of the present invention be selected from that conveyer belt transmits and cylinder-cylinder transmission in a kind of.
Packaging plastic deposition described in the method for packing of organic electroluminescence device of the present invention is that deposition process is carried out in the device transport process by the printing process deposition.
Technical scheme advantage of the present invention: cap is a planar package lid, does not have the gas compartment in the encapsulation process, avoids therefore and the cap that produces distortion, and then causes leaking gas and destroy the defective of negative electrode, can be so that device is prepared into thinner; Encapsulation process can be taked continuous productive process, rhythm of production continuously, fast, stable, be particularly suitable for that large scale screen system is equipped with, large-scale production.
Description of drawings
Fig. 1 is the method for packing schematic diagram of device in the embodiments of the invention 4.
Embodiment
(1) preparation method of organic luminescent device OLED:
On substrate, prepare anode, organic function layer and negative electrode successively:
The substrate transparent substrate can be glass or flexible substrate, and flexible substrate adopts a kind of material in polyesters, polyimides compounds, tinsel or the ultra-thin glass;
Anode layer can adopt inorganic material or organic conductive polymer, 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 optimized ITO that is chosen as, organic conductive polymer are preferably a kind of material in polythiophene/polyvinylbenzenesulfonic acid sodium (hereinafter to be referred as PEDOT:PSS), the polyaniline (hereinafter to be referred as PANI);
Cathode layer generally adopts the alloy of the lower metal of work functions such as lithium, magnesium, calcium, strontium, aluminium, indium or they and copper, gold, silver, or the electrode layer that alternately forms of metal and metal fluoride, the present invention is preferably Mg:Ag alloy-layer, Ag layer and LiF layer successively, Al layer successively;
Organic function layer comprises luminescent layer, can also comprise functional layers such as electron transfer layer, hole transmission layer.
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, 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, wherein carbazole derivates such as CBP, polyvinylcarbazole (PVK) are material of main part, but Doping Phosphorus photoinitiator dye in this material of main part is 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.
Concrete preparation method at first cleans the substrate that is carved with anode in advance, evaporation hole transport layer material, luminescent layer material and electric transmission layer material successively thereon then, and the method by evaporation prepares cathode layer at last.
(2) preparation method of the organic light-emitting device encapsulating structure of the present invention's proposition:
The material of planar package lid can be glass, polymer, metal or alloy material and composite film material thereof, be preferably a kind of in polyester (PET), polycarbonate (PC), polyether sulfone (PES), the poly (arylene ether nitrile) (PEN), a kind of in aluminium foil, steel foil, TiN/ steel foil sheet, the PET/ aluminium foil.
Packaging plastic is selected from UV glue, heat-curable glue or AB glue.The thickness of packaging plastic is about 10 μ m～500 μ m.
Can also be doped with dry hygroscopic material in the packaging plastic.Dry hygroscopic material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, have at least a in the metal alcoholate of long-chain hydrocarbon.Drier shared volume percent content in packaging plastic is 10%～60%.
Can also comprise layer protecting film between packaging plastic and the device, its material is selected from least a in organic small molecule material, inorganic material or the metal material, preferably a kind of in AlQ, CuPc, SiOx, AlOx, SiNxOy, TiN.
Can also comprise one deck drying layer between planar package lid and the device, its material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, has the metal alcoholate of long-chain hydrocarbon.
Can also comprise one deck water, oxygen barrier layer between planar package lid and the device, its material is selected from a kind of and composite construction in SiOx, AlOx, SiNxOy, TiN, polymethyl methacrylate, polyethyl methacrylate, epoxy resin, acrylate, the UV curing glue.
When preparing encapsulating structure of the present invention, can adopt following two kinds of methods:
(2-1) at first packaging plastic is deposited on the cathode layer at the OLED device back side with wet method film-forming methods such as spin coating, printings, the planar package lid is pasted on the packaging plastic closely.
If (2-2) the planar package lid is flexible material, packaging technology schematic diagram such as Fig. 1, the transmission of substrate is to transmit by the conveyer belt mode, if being flexible substrate, substrate can adopt the method for cylinder-cylinder to transmit, with printing process deposition packaging plastic film, cover substrate band package-side surface in the substrate transport process, cap transmits and transmits by cylinder-cylinder mode, with the drum extrusion method cap is covered on the substrate, pass through UV rayed cure package glue at last.Utilize the cylinder technology effectively the bubble in the packaging plastic to be extruded, and be particularly suitable for large-scale production.
Embodiment 1
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of ito glass substrate in advance: utilize the ultrasonic and ultrasonic method of deionized water of the washing agent of heat that the transparent conduction base sheet ito glass is cleaned, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ito glass, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) above-mentioned device is imported in the glove box, prepare one deck polyethyl methacrylate with printing process at device surface, thickness is 100 μ m;
(2-2) glass is pressed on the above-mentioned device, the UV rayed is solidified makes substrate and case chip form an integral body.
Embodiment 2
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of ito glass substrate in advance: utilize the ultrasonic and ultrasonic method of deionized water of the washing agent of heat that the transparent conduction base sheet ito glass is cleaned, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ito glass, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) splash-proofing sputtering metal Al in vacuum cavity feeds highly purified oxygen simultaneously, and the air pressure in the cavity is 10
-2Pa, depositing Al on the device described in (1)
2O
3, deposition rate is 0.5nm/s, thickness is 80nm;
(2-2) above-mentioned device is imported in the glove box, prepare the A glue and the B glue of AB glue with printing process respectively at device surface and plane package board TiN/ steel foil, thickness is 100 μ m;
(2-3) the TiN/ steel foil is pressed on the above-mentioned device, places after 1 minute, substrate and case chip form an integral body.
Embodiment 3
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of ito glass substrate in advance: utilize the ultrasonic and ultrasonic method of deionized water of the washing agent of heat that the transparent conduction base sheet ito glass is cleaned, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ito glass, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) keep the pressure of vacuum cavity constant, the electrodeless material SiOxNy of sputter on the device described in (1), deposition rate is 0.5nm/s, thickness is 120nm;
(2-2) keep the pressure of vacuum chamber constant, evaporation one deck epoxide-resin glue on SiOxNy, thickness are 20 μ m;
(2-3) the PET substrate is pressed on the above-mentioned device, the PET substrate surface has the laminated film that is formed by SiO2 and Al2O3, advances the UV rayed, makes substrate and case chip form an integral body.
Embodiment 4
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of ito glass substrate in advance: utilize the ultrasonic and ultrasonic method of deionized water of the washing agent of heat that the transparent conduction base sheet ito glass is cleaned, substrate is of a size of 370cm * 470cm, place it in the vacuum drying oven after the cleaning and dry, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ito glass, be evacuated to 1 * 10
-4Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) keep the pressure of vacuum cavity constant, evaporation organic material CuPc on the device described in (1), deposition rate is 0.5nm/s, thickness is 300nm;
(2-2) above-mentioned device is imported in the glove box, be placed on the transport tape, substrate prepares one deck epoxide-resin glue with printing process at device surface with the speed transmission of 10cm/min, and thickness is 300 μ m;
(2-3) the Al paper tinsel is enclosed within on the cylinder, cylinder rolls with the linear velocity of 10cm/min, and the Al paper tinsel is pressed on the substrate.Placed 1 hour under 80 ℃ condition, package board and substrate form an integral body.
Embodiment 5
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of the pet substrate of ITO in advance: utilize the method that washing agent is ultrasonic and deionized water is ultrasonic of heat that the PET substrate that transparent conduction base sheet covers water oxygen barrier layer and ITO is cleaned, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ITO substrate, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) keep the pressure of vacuum cavity constant, sputtering method prepares one deck Al on the device described in (1)
2O
3Film, deposition rate are 0.5nm/s, and thickness is 120nm;
(2-2) above-mentioned device is imported in the glove box, prepare one deck epoxide-resin glue with printing process at device surface, be mixed with the CaO particle of diameter 200nm in the epoxide-resin glue, thickness is 200 μ m;
(2-3) the PC substrate is pressed on the above-mentioned device, the PC substrate surface has the laminated film that is formed by SiO2 and Al2O3, advances the UV rayed, makes substrate and case chip form an integral body.
Embodiment 6
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of the pet substrate of ITO in advance: utilize the method that washing agent is ultrasonic and deionized water is ultrasonic of heat that the PET substrate that transparent conduction base sheet covers water oxygen barrier layer and ITO is cleaned, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ITO substrate, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50mn;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) keep the pressure of vacuum cavity constant, sputtering method prepares one deck TiN film on the device described in (1), and deposition rate is 0.5nm/s, and thickness is 80nm;
(2-2) above-mentioned device is imported in the glove box, be placed on the cylinder, roll, prepare one deck epoxide-resin glue at device surface, be mixed with the CaCl of diameter 200nm in the epoxide-resin glue with printing process with the linear velocity of 10cm/min
2Particle, thickness are 200 μ m;
(2-3) with the PEN/Al case chip, be placed on the cylinder, roll with the linear velocity of 10cm/min, the PEN/Al case chip is pressed on the device, under 80 ℃ of conditions, place 1 hour curing epoxy resin adhesive, make substrate and case chip form an integral body.
Embodiment 7
(1) on substrate, prepare anode, organic function layer and negative electrode:
(1-1) be carved with the cleaning of ito glass substrate in advance: the method that washing agent is ultrasonic and deionized water is ultrasonic of utilizing heat is cleaned transparent conduction base sheet ito glass or the PET substrate that covers the water oxygen barrier layer, place it in oven dry under the infrared lamp after the cleaning, ito substrate to oven dry carries out the preliminary treatment that UV ozone is cleaned and the low energy oxygen ion beam bombards then, wherein the ITO film above the conductive substrate is as the anode layer of device, the square resistance of ITO film is 50 Ω, and thickness is 150nm;
(1-2) preparation of organic luminous layer: place in the vacuum chamber with above-mentioned cleaning, drying and through pretreated ito glass, be evacuated to 1 * 10
-3Pa, evaporation one deck hole mobile material NPB on above-mentioned ITO film then, the evaporation speed of material film is 0.5nm/s, thickness is 50nm; Evaporation one deck luminous organic material on hole mobile material, oxine aluminium Alq, the evaporation speed of material film is 0.5nm/s, thickness is 50nm;
(1-3) preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, evaporation Mg successively on above-mentioned electron transfer layer, the Ag alloy-layer is as the cathode layer of device, and thickness is 8nm.The Ag layer of evaporation 15nm again on the MgAg alloy-layer.Wherein alloy-layer adopts the method for double source evaporation to mix;
(2) encapsulating structure of fabricate devices:
(2-1) keep the interior pressure of vacuum chamber constant, evaporating Al q on the device of method preparation described in (1), deposition rate is 0.5nm/s, thickness is 500nm;
(2-2) above-mentioned device is imported in the glove box, prepare one deck polyethyl methacrylate with printing process at device surface, thickness is 100 μ m;
(2-3) on the packaged glass surface with the molecular sieve desiccant of the method coating liquid of rotary coating, the speed of rotation is 1000 commentaries on classics/min, places 2 hours under 220 ℃ condition, the solvent evaporates in the molecular sieve desiccant becomes solid fully.
(2-4) glass that will be coated with drier is pressed on the device, and the UV rayed is solidified, integral body of substrate and case chip formation.
Because gas permeation rate checkout equipment commonly used can only detect 10
-2G/m
2The above transmitance of/day, encapsulation back transmitance are all at this below scope, so come the influence of number of detection cycles to encapsulation performance with the oxidation of active metal Ca:
Above-mentioned three embodiment see the following form with the Ca oxidation test result of not carrying out packaging:
Encapsulating structure is: glass substrate (perhaps PET substrate)/Ca/ encapsulated layer
50 ℃ of temperature, with the naked eye the time of Ca complete oxidation is observed under the environment of humidity 95%:
| Encapsulating structure | Ca complete oxidation time/h |
| Feng Zhuan glass substrate not | 10.2 |
| Embodiment 1 | 603.1 |
| Embodiment 2 | 517.5 |
| Embodiment 3 | 452.8 |
| Embodiment 4 | 592.0 |
| Embodiment 7 | 713.3 |
| Feng Zhuan PET substrate not | 8.0 |
| Embodiment 5 | 226.9 |
| Embodiment 6 | 135.6 |
Contrast is the structure of encapsulation not, and encapsulating structure of the present invention has improved the transmitance of water, oxygen significantly, therefore can protection device not be subjected to extraneous water, oxygen attack.
Although describe the present invention in conjunction with the preferred embodiments, the present invention is not limited to the foregoing description, and encapsulated layer especially of the present invention can prepare in device cathodes one side, also can prepare the surface in entire device.Should be appreciated that those skilled in the art can carry out various modifications and improvement under the guiding of the present invention's design, claims have been summarized scope of the present invention.
Claims (17)
1. an organic electroluminescence device comprises substrate, anode, negative electrode and the organic function layer between two electrodes, also comprises encapsulating structure, it is characterized in that, has the planar package lid in the described encapsulating structure.
2. organic electroluminescence device according to claim 1 is characterized in that, described encapsulating structure is positioned at negative electrode one side of device.
3. organic electroluminescence device according to claim 1 is characterized in that, the material of described planar package lid is glass, polymer, metal or alloy material and composite film material thereof.
4. organic electroluminescence device according to claim 3 is characterized in that, the material of described planar package lid is preferably a kind of in polyester (PET), polycarbonate (PC), polyether sulfone (PES), the poly (arylene ether nitrile) (PEN).A kind of in aluminium foil, steel foil, TiN/ steel foil sheet, the PET/ aluminium foil.
5. organic electroluminescence device according to claim 1 is characterized in that, described planar package lid is bonding by packaging plastic and device.
6. organic electroluminescence device according to claim 5 is characterized in that, described packaging plastic is selected from a kind of in UV glue, heat-curable glue, the AB glue.
7. organic electroluminescence device according to claim 5 is characterized in that, is doped with dry hygroscopic material in the described packaging plastic.
8. organic electroluminescence device according to claim 7, it is characterized in that described dry hygroscopic material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, have at least a in the metal alcoholate of long-chain hydrocarbon.
9. organic electroluminescence device according to claim 5 is characterized in that, comprises also that between described packaging plastic and device layer protecting film, its material are selected from least a in organic small molecule material, inorganic material or the metal material.
10. organic electroluminescence device according to claim 9 is characterized in that, the material of described diaphragm is a kind of in AlQ, CuPc, SiOx, AlOx, SiNxOy, TiN preferably.
11. organic electroluminescence device according to claim 1, it is characterized in that, also comprise one deck drying layer between described planar package lid and the device, its material is selected from alkali metal, alkaline-earth metal, metal oxide, halide, sulfate, perchlorate, zeolite, has the metal alcoholate of long-chain hydrocarbon.
12. organic electroluminescence device according to claim 1, it is characterized in that, also comprise one deck water, oxygen barrier layer between described planar package lid and the device, its material is selected from a kind of and composite construction in SiOx, AlOx, SiNxOy, TiN, polymethyl methacrylate, polyethyl methacrylate, epoxy resin, acrylate, the UV curing glue.
13. organic electroluminescence device according to claim 1, the substrate that it is characterized in that described device is for flexible, and its material is selected from plastics, tinsel or ultra-thin glass.
14. method for preparing encapsulating structure in the described organic electroluminescence device of claim 1, when the planar package lid is flexible material, encapsulation process comprises: device transmits, packaging plastic deposits, the planar package lid transmits, the planar package lid covers on the device, packaging plastic solidifies, and it is characterized in that it is to cover on the device by the drum extrusion method that planar package is covered.
15. the method for packing of organic electroluminescence device according to claim 14 is characterized in that, it is that cylinder transmits that described planar package lid transmits.
16. the method for packing of organic electroluminescence device according to claim 14 is characterized in that, described device transfer approach be selected from that conveyer belt transmits and cylinder-cylinder transmission in a kind of.
17. the method for packing of organic electroluminescence device according to claim 15 is characterized in that, described packaging plastic deposition is that deposition process is carried out in the device transport process by the printing process deposition.
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| CN101685843B (en) * | 2008-09-26 | 2011-03-23 | 财团法人工业技术研究院 | Method for packaging light emitting diode |
| CN102842683A (en) * | 2011-06-21 | 2012-12-26 | 海洋王照明科技股份有限公司 | Organic electroluminescence device and manufacturing method thereof |
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