CN109244268A - Oled device and its manufacturing method - Google Patents
Oled device and its manufacturing method Download PDFInfo
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- CN109244268A CN109244268A CN201811094207.4A CN201811094207A CN109244268A CN 109244268 A CN109244268 A CN 109244268A CN 201811094207 A CN201811094207 A CN 201811094207A CN 109244268 A CN109244268 A CN 109244268A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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Abstract
The present invention provides a kind of oled device, the oled device includes organic light-emitting diode element layer and the encapsulated layer that is packaged to the organic light-emitting diode element layer, wherein, the material that the encapsulated layer is made includes metal-organic framework material.The present invention also provides a kind of manufacturing methods of oled device.The encapsulated layer of the oled device can preferably completely cut off water oxygen, and the oled device is made to have lesser thickness, be more applicable for oled device flexible.
Description
Technical field
The present invention relates to Organic Light Emitting Diode fields, and in particular, to a kind of oled device and should
The manufacturing method of oled device.
Background technique
Oled device have actively shine, thickness it is small, it is at low cost, low in energy consumption, layer flexibility device can be made
The advantages that part, is widely used in the numerous areas such as illumination and display.
But since Organic Light Emitting Diode is especially sensitive to oxygen and water vapour, to Organic Light Emitting Diode
The encapsulation of device requires especially high.It is traditional using glass as substrate, using glass or metal as the rigid organic light emission of cover board
In diode apparatus, epoxy resin is usually used to bond substrate and cover board as binder in vacuum environment.It is residual in order to remove
Stay in the water vapour and oxygen in device, it will usually the dry agent film such as calcium oxide, barium monoxide be deposited on the cover board, and also need
It will be in desiccant layers such as the raw attaching barium monoxide of cover board, calcium oxide.
After multilayer desiccant layer is arranged, oled device structure becomes complicated.However, it is very difficult to be applied to flexibility
Oled device in.Which results in the industrialization of oled device flexible well below people
Expection.
Therefore, how effectively this field technology urgently to be resolved is encapsulated into oled device progress to ask
Topic.
Summary of the invention
The purpose of the present invention is to provide a kind of oled device and a kind of oled devices
Manufacturing method has good packaging effect using oled device made from the manufacturing method.
To achieve the goals above, as one aspect of the present invention, a kind of oled device is provided, it is described
Oled device includes organic light-emitting diode element layer and seals to the organic light-emitting diode element layer
The encapsulated layer of dress, wherein the material that the encapsulated layer is made includes metal-organic framework material.
Preferably, the bore hole size of the metal-organic framework material is no more than 0.34nm.
Preferably, the metal-organic framework material includes that organic ligand and metal ion pass through the coordination being self-assembly of
Compound has unsatuated metal site in the complex.
Preferably, the metal ion in transition metal ions and lanthanide metal ion any one or it is any several
Person, the organic ligand include aromatic dicarboxylic acids and polycarboxylic aromatic acids.
Preferably, the oled device further includes cover sheet, bonding piece and underlay substrate, described organic
Light-emitting diode layer is formed on the underlay substrate, and the encapsulated layer includes organic body membrane and is formed in described organic
The separating layer of ontology film surface, the material of the separating layer include the metal-organic framework material, and the bonding piece is used for will
The underlay substrate for being formed with organic light-emitting diode element layer and encapsulated layer is bonded together with the cover sheet.
Preferably, the oled device further includes underlay substrate flexible, the Organic Light Emitting Diode
Element layer is arranged on the underlay substrate flexible.
As the second aspect of the invention, a kind of manufacturing method of oled device is provided, wherein described
Manufacturing method includes:
The underlay substrate for having organic light-emitting diode element layer is provided；
The organic light-emitting diode element layer is packaged using the encapsulated layer that encapsulating material is formed, wherein described
Encapsulating material includes metal-organic framework material.
Preferably, the step of being packaged using encapsulating material to the organic light-emitting diode element layer include:
With target made of metal-organic framework material to be formed with the underlay substrate of organic light-emitting diode element layer into
Row sputtering, to form the encapsulated layer for encapsulating the organic light-emitting diode element layer.
Preferably, the step of being packaged using encapsulating material to the organic light-emitting diode element layer include:
Surface is carried out to organic bulk film using the metal-organic framework material casting solution for including metal organic frame particle
Hydridization, to obtain encapsulated layer；
The organic light-emitting diode element layer is packaged using the encapsulated layer；
The underlay substrate and protection cap of organic light-emitting diode element layer and the encapsulated layer will be formed with using bonding piece
The fixed bonding of plate.
Preferably, the manufacturing method further includes the steps that preparing metal-organic framework material, this, which prepares metal, machine frame
The step of frame material includes:
Organic ligand is mixed with metal salt solution；
The metal-organic framework material is obtained using solvent heat seal.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is a kind of schematic diagram of embodiment of oled device provided by the present invention；
Fig. 2 is the schematic illustration of encapsulated layer barrier water, oxygen；
Fig. 3 is the schematic diagram of the another embodiment of oled device provided by the present invention；
Fig. 4 is-[{ Co2(bpbp)}2bdc](PF6)4Molecular formula schematic diagram；
Fig. 5 a to Fig. 5 j is the coordination mode schematic diagram of oxygen-containing polybasic carboxylic acid；
Fig. 6 is the schematic diagram of solvent-thermal process method preparation metal-organic framework material；
Fig. 7 is the flow chart of manufacturing method provided by the present invention；
Fig. 8 is a kind of flow chart of embodiment of step S120.
Description of symbols
110: organic light-emitting diode element layer 120: encapsulated layer
130: underlay substrate 140: cover sheet
150: bonding piece
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
As one aspect of the present invention, a kind of oled device is provided, as shown in Figure 1, organic hair
Optical diode device includes organic light-emitting diode element layer 110 and is packaged to the organic light-emitting diode element layer 110
Encapsulated layer 120, wherein the material that encapsulated layer 120 is made includes metal-organic framework material.
Metal-organic framework material has the lesser duct of size, can obstruct extraneous water vapour and oxygen and pass through,
So as to be protected well to organic light-emitting diode element layer 110.Also, in the present invention, only by including gold
Effective encapsulation to organic light-emitting diode element layer 110 can be realized in the encapsulated layer 120 for belonging to organic framework materials, is conducive to drop
The integral thickness of low oled device.
As mentioned above it is possible, using including the encapsulated layer 120 of metal-organic framework material to organic light-emitting diode element
Layer 110 is packaged the integral thickness that can reduce oled device, and therefore, scheme provided by the present invention is especially
Suitable for oled device flexible.
In the present invention, special requirement is not done to the bore hole size of the metal-organic framework material in encapsulated layer 120.It is logical
Often, the kinetic diameter of hydrone is 0.4nm, and the kinetic diameter of oxygen molecule is 0.346nm.Therefore, as long as metal is organic
The bore hole size of frame material is no more than 0.34nm, and preferable water oxygen barriers function can be realized.
Due to having hole in the metal-organic framework material, and be formed as three-dimensional porous framework material, therefore, institute
Metal-organic framework material also specific surface area with higher is stated, therefore, the surface of the metal-organic framework material can be higher,
Therefore, remain in steam and oxygen in organic LED display device after encapsulation can be adsorbed, thus further
It prevents organic light-emitting diode element layer 110 from being corroded by water oxygen, extends the service life of oled device.In addition to because
Outside capable of being adsorbed to hydrone and oxygen molecule for higher surface, the metal position of sum is not protected in metal-organic framework material
Point, film cavity surface extension can roll into a ball between different interaction absorption to hydrone and oxygen molecule also may be implemented.
As shown in Fig. 2, the encapsulated layer in oled device provided by the present invention can not only completely cut off the external world
Water vapour and oxygen (in Fig. 2 shown in hollow arrow), can also be to water vapour and oxygen remaining in oled device
Gas is adsorbed (in Fig. 2 shown in solid arrow).
In the present invention, special regulation is not done to the specific material type of metal-organic framework material, it is preferable that described
Metal-organic framework material includes that organic ligand and metal ion pass through the complex being self-assembly of, the ligand compound
There is unsatuated metal site in object.Unsatuated metal ion ambient electron cloud density is higher, can provide for oxygen molecule properly
Electron amount form irreversible suction-operated so that interacting between unsatuated metal ion and oxygen molecule.
In the present invention, special requirement is not done to the metal ion in metal-organic framework material, as a kind of preferred
Embodiment, any one of the metal ion in transition metal ions and lanthanide metal ion.It is further preferred that
The metal ion can be selected from the transition metal ions of lower valency, for example, manganese ion, cobalt ions, nickel ion, cadmium ion, zinc
Any one in ion and copper ion or any several persons.
In the present invention, there is no special requirement, the coordination structure of oxygen-containing class polybasic carboxylic acid aromatic ligand to organic ligand
Type is abundant, the thermal stability and structural rigidity of coordination polymer frame structure can be significantly increased, therefore, as a kind of preferred reality
Mode is applied, organic ligand can be oxygen-containing class polybasic carboxylic acid aromatic ligand.
It is the common coordination mode of polybasic carboxylic acid shown in Fig. 5 a to Fig. 5 j.It is huge legendary turtle that Fig. 5 a, which is monodentate ligand, Fig. 5 b,
Conjunction coordination, Fig. 5 c are bidentate Z, and Z-type coordination, Fig. 5 d are bidentate Z, and the coordination of E type, Fig. 5 e are bidentate E, and E type is coordinated, Fig. 5 f is three teeth
(a) type is coordinated, and Fig. 5 g is that three tooth (b) types are coordinated, Fig. 5 h is that three tooth (c) types are coordinated, Fig. 5 i is the coordination of four tooth (a) types, and Fig. 5 j is
The coordination of four tooth (b) types.Wherein, alphabetical M indicates metal ion.
For example, the polycarboxylic aromatic acids can be the binary aromatic carboxylic acid containing pyridine ring, being also possible to other can be real
The polycarboxylic aromatic acids of existing identical function.
Nitrogen-atoms on pyridine ring for coordination can provide the coordination of the adsorption of oxygen in addition to ligand unsatuated metal point
Point.Be shown in Fig. 6 with the binary aromatic carboxylic acid containing pyridine ring and metal ion (can for manganese ion, cobalt ions, nickel from
Son, cadmium ion, zinc ion, in copper ion any one or it is any several) by solvent-thermal process method acquisition metal have machine frame
The schematic diagram of frame material, obtain product in still have be not coordinated nitrogen-atoms (uncoordinated nitrogen atom).
In the metal-organic framework material prepared using the binary aromatic carboxylic acid containing pyridine ring and metal ion
Bore hole size is less than the kinetic diameter of oxygen molecule and hydrone.
Certainly, the present invention is not limited thereto.The organic ligand can also be phosphoric acid class, sulphonic acids, imidazoles amine, pyrrole
Pyridine class and phenols etc., as long as guaranteeing that ligand can be coordinated with metal ion.
It is metal-organic framework material-[{ Co shown in Fig. 42(bpbp)}2bdc](PF6)4Schematic arrangement,
Under room temperature (25 DEG C), this metal-organic framework material reaches 2.8wt% to the chemical adsorption amount of oxygen molecule, that is to say, that
The metal-organic framework material of every 100 mass parts can adsorb the oxygen molecule of 2.8 mass parts.In the material shown in Fig. 4, cobalt
Atom is pentacoordinate, respectively by from ligand three nitrogen-atoms and two oxygen atoms surround, there is unsaturated adsorption site,
Possibility is provided for the selective chemical absorption of oxygen molecule, when oxygen molecule reaches adsorption site, central metal cobalt atom reaches
To the saturation state of hexa-coordinate.
Certainly, in the present invention, metal-organic framework material is not limited to above-mentioned-[{ Co2(bpbp)}2bdc](PF6)4,
It can also be molecular formula material as shown in following formula (1):
Mn5(btac)4(μ3-OH)2(EtOH)·2DMF·3EtOH·3H2O(1)
In molecular formula in the material as shown in formula (1), unsaturated manganese atom has oxygen molecule under the air pressure told somebody what one's real intentions are
Suction-operated.This is because unsaturated manganese atom ambient electron cloud density is high, electricity can be provided for oxygen molecule, so that manganese
Atom is attracted each other with oxygen molecule, and then realizes irreversible absorption.
In the present invention, special limitation is not done to the specific structure of encapsulated layer and concrete component, as long as in encapsulated layer
With metal-organic framework material.
As an implementation, as shown in Figure 1, encapsulated layer 120 is made using metal-organic framework material.It can use
Sputtering or plasma reinforced chemical vapour deposition mode obtain encapsulated layer 120 made of metal-organic framework material.
It is another embodiment shown in Fig. 3, in this embodiment, the oled device
Including underlay substrate 130, cover sheet 140 and bonding piece 150, organic light-emitting diode element layer 110 is formed in underlay substrate
On 130.Correspondingly, encapsulated layer 120 includes organic body membrane and is formed in the separating layer of the organic bulk film surface, and described point
The material of absciss layer includes the metal-organic framework material.Bonding piece 150 will be for that will be formed with organic light-emitting diode element layer
110 and the underlay substrate 130 of encapsulated layer 120 be bonded together with cover sheet 140.
In embodiment shown in fig. 3, cover sheet 140 can be to encapsulated layer 120 and Organic Light Emitting Diode
Element layer 110 is protected.The encapsulated layer can be obtained by carrying out hydridization technique to organic bulk film.
In the present invention, special requirement is not done to the specific ingredient of organic bulk film, for example, the organic bulk film can
To be made of polysulfones, can also be made of vinyl alcohol polymer.It hereinafter will be to how to organic bulk film progress hydridization
It obtains the separating layer to describe in detail, not repeat first here.
As mentioned above it is possible, oled device provided by the present invention is particularly suitable for organic light emission flexible
Diode apparatus, correspondingly, the oled device further include underlay substrate 130 flexible, organic light-emitting diodes
Tube elements layer 110 is arranged on underlay substrate 130 flexible.
In the present invention, special restriction is not done to the specific structure of oled device and particular use.
For example, the oled device can be lighting device, it is also possible to display device.When the organic light-emitting diodes
When pipe device is display device, the organic light-emitting diode element layer includes multiple pixel units, in each pixel unit
It is provided with Organic Light Emitting Diode.
As the second aspect of the invention, a kind of manufacturing method of organic light emission thermal diode device is provided, wherein such as
Shown in Fig. 7, the manufacturing method includes:
In step s 110, the substrate with organic light-emitting diode element layer is provided；
In the step s 120, the organic light-emitting diode element layer is sealed using the encapsulated layer that encapsulating material is formed
Dress, wherein the encapsulating material includes metal-organic framework material.
Manufacturing method provided by the present invention can be used for manufacturing above-mentioned Organic Light Emitting Diode dress provided by the present invention
It sets.
Since encapsulating material includes metal-organic framework material, the encapsulated layer can stop the water in air to steam
Vapour, oxygen enter inside oled device, can also prevent water oxygen from corroding organic light-emitting diode element layer.And
And the metal-organic framework material in the encapsulated layer can also adsorb water vapour remaining in oled device and
Oxygen.
In order to manufacture organic LED display device shown in Fig. 1 (that is, being made using metal-organic framework material
Encapsulated layer 120), step S120 may include:
The substrate for being formed with organic light-emitting diode element layer is splashed with target made of metal-organic framework material
It penetrates, to form the encapsulated layer for encapsulating the organic light-emitting diode element layer.
In order to obtain organic LED display device shown in Fig. 3, as shown in figure 8, step S120 may include:
In step S121, surface hydridization is carried out to organic bulk film using metal-organic framework material casting solution, in institute
The surface for stating organic bulk film forms separating layer, to obtain encapsulated layer；
In step S122, the organic light-emitting diode element layer is packaged using the encapsulated layer；
In step S123, the substrate of organic light-emitting diode element layer and the encapsulated layer will be formed with using bonding piece
Substrate and the fixed bonding of cover sheet.
After step S121, the surface of organic bulk film is formed with point formed by metal-organic framework material casting solution
Absciss layer, so that encapsulated layer has the function of obstructing water oxygen.
Metal-organic framework material will can be dissolved in organic solvent, to obtain metal-organic framework material casting solution.
In the present invention, special requirement is not done to the specific ingredient of organic solvent, as long as can dissolve metal has machine frame
Frame material.For example, the solvent of above-mentioned formation metal-organic framework material casting solution may include alcohols or acetone, with molten
Solve the metal-organic framework material.
It can be with other than metal-organic framework material and organic solvent, in the metal-organic framework material casting solution
Including crosslinking agent and catalyst.Crosslinking agent can select ethyl orthosilicate as a preferred implementation manner, and catalyst can select
Use dibutyl tin dilaurate.The quality of metal-organic framework material, crosslinking agent and catalyst as a preferred implementation manner,
Than for 1:(0.1~0.2): (0.03~0.05), as a preferred implementation manner, metal-organic framework material, crosslinking agent and
The mass ratio of catalyst can be 1:0.1:0.05.
In the present invention, to the specific material of organic basis material also not special limitation, for example, can use polysulfones
Or vinyl alcohol polymer is as the organic bulk film.
In the present invention, to how the surface by metal-organic framework material casting solution coated in organic bulk film is without spy
Different limitation.For example, organic bulk film can be immersed in metal-organic framework material casting solution under ultrasound environments.It impregnates pre-
The organic bulk film that metal-organic framework material casting solution is coated with after fixing time is toasted under heat lamp, vacuum dried
So that the metal-organic framework material casting solution on the surface of organic bulk film is fully crosslinked and forms fine and close separating layer, the separation
Layer includes metal-organic framework material.
In the present invention, there is no special limitation to how preparing metal-organic framework material, as a kind of preferred implementation
Mode, prepare metal-organic framework material the step of include:
Organic ligand is mixed with metal salt solution；
The metal-organic framework material is obtained using solvent-thermal process method.
In the present invention, the not special requirement of the proportion to organic ligand and metal salt solution, for example, organic ligand and
The ratio between molal quantity of metal salt solution can be 1:1.It stirs evenly and (preferably, stirs 10 minutes) after the two is mixed, then
Mixture is transferred in the reaction kettle with polytetrafluoroethylsubstrate substrate, the solvent-thermal process method is carried out in the reaction kettle.
Specifically, the solvent-thermal process method includes:
By the mixture confined reaction 72 hours at 80 DEG C to 160 DEG C；
It is down to room temperature with the rate of temperature fall of 5 DEG C/h, filters, obtains the metal-organic framework material.
In the present invention, there is no special requirement to organic ligand.The coordination structure of oxygen-containing class polybasic carboxylic acid aromatic ligand
Type is abundant, the thermal stability and structural rigidity of coordination polymer frame structure can be significantly increased, therefore, as a kind of preferred reality
Mode is applied, organic ligand can be oxygen-containing class polybasic carboxylic acid aromatic ligand.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of oled device, the oled device include organic light-emitting diode element layer and
The encapsulated layer that the organic light-emitting diode element layer is packaged, which is characterized in that the material packet of the encapsulated layer is made
Include metal-organic framework material.
2. oled device according to claim 1, which is characterized in that the metal-organic framework material
Bore hole size is no more than 0.34nm.
3. oled device according to claim 1, which is characterized in that the metal-organic framework material packet
It includes organic ligand and metal ion passes through the complex being self-assembly of, there is unsatuated metal in the complex
Site.
4. oled device according to claim 3, which is characterized in that the metal ion is selected from transition gold
Belong to any one in ion and lanthanide metal ion or any several persons, the organic ligand includes oxygen-containing class polybasic carboxylic acid fragrance
Race's ligand.
5. oled device as claimed in any of claims 1 to 4, which is characterized in that described organic
Light-emitting diode assembly further includes cover sheet, bonding piece and underlay substrate, and the organic light-emitting diode element layer is formed in
On the underlay substrate, the encapsulated layer includes organic body membrane and the separating layer for being formed in the organic bulk film surface, institute
The material for stating separating layer includes the metal-organic framework material, and the bonding piece will be for that will be formed with Organic Light Emitting Diode member
The underlay substrate of part layer and encapsulated layer is bonded together with the cover sheet.
6. oled device as claimed in any of claims 1 to 4, which is characterized in that described organic
Light-emitting diode assembly further includes underlay substrate flexible, and the organic light-emitting diode element layer is arranged in the lining flexible
On substrate.
7. a kind of manufacturing method of oled device, which is characterized in that the manufacturing method includes:
The underlay substrate for having organic light-emitting diode element layer is provided；
The organic light-emitting diode element layer is packaged using the encapsulated layer that encapsulating material is formed, wherein the encapsulation
Material includes metal-organic framework material.
8. manufacturing method according to claim 7, which is characterized in that using encapsulating material to the Organic Light Emitting Diode
The step of element layer is packaged include:
The underlay substrate for being formed with organic light-emitting diode element layer is splashed with target made of metal-organic framework material
It penetrates, to form the encapsulated layer for encapsulating the organic light-emitting diode element layer.
9. manufacturing method according to claim 7, which is characterized in that using encapsulating material to the Organic Light Emitting Diode
The step of element layer is packaged include:
Surface hydridization is carried out to organic bulk film using metal-organic framework material casting solution, on the surface of the organic bulk film
Separating layer is formed, to obtain encapsulated layer；
The organic light-emitting diode element layer is packaged using the encapsulated layer；
The underlay substrate for being formed with organic light-emitting diode element layer and the encapsulated layer is consolidated with cover sheet using bonding piece
Fixed bonding.
10. the manufacturing method according to any one of claim 7 to 9, which is characterized in that the manufacturing method further includes
The step of preparing metal-organic framework material, the step of preparation metal-organic framework material include:
Organic ligand is mixed with metal salt solution；
The metal-organic framework material is obtained using solvent-thermal process method.
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| US10868275B2 (en) | 2019-02-02 | 2020-12-15 | Beijing Boe Display Technology Co., Ltd. | Display panel and preparation method thereof |
| CN114068828A (en) * | 2020-08-04 | 2022-02-18 | Tcl科技集团股份有限公司 | Composite film layer, preparation method thereof and light-emitting diode |
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