CN106206995B - A kind of preparation method and products thereof of Organic Light Emitting Diode scattering layer - Google Patents
A kind of preparation method and products thereof of Organic Light Emitting Diode scattering layer Download PDFInfo
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- CN106206995B CN106206995B CN201610866250.2A CN201610866250A CN106206995B CN 106206995 B CN106206995 B CN 106206995B CN 201610866250 A CN201610866250 A CN 201610866250A CN 106206995 B CN106206995 B CN 106206995B
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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
- H10K50/85—Arrangements for extracting light from the devices
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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
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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Abstract
This application involves display technology fields, specifically, are related to a kind of preparation method and products thereof of Organic Light Emitting Diode scattering layer.Material vapor deposition of the application by glass transition temperature less than 120 DEG C forms film in the light-emitting surface for being provided with the luminous Organic Light Emitting Diode in top, then carries out solidification annealing.Then the application makes this layer be atomized by the material in top-illuminating OLED device light-emitting surface one layer of lower glass transition temperatures of vapor deposition by annealing, have the function that light takes out and scatters, the light extraction efficiency of top-illuminating OLED can be improved and improve visual angle.
Description
Technical field
This application involves display technology fields, specifically, are related to a kind of preparation method of Organic Light Emitting Diode scattering layer
And products thereof.
Background technology
OLED, that is, Organic Light Emitting Diode (Organic Light-Emitting Diode) is provided simultaneously with self-luminous, no
It needs that backlight, contrast are high, thickness is thin, visual angle is wide, reaction speed is fast, can be made into solid state flat panel display panel, solid-state flexibility
Panel and transparent panel, the excellent specific properties such as Applicable temperature range is wide, construction and preparation process are simple.In recent years by new material
It is continuous explore and device architecture and technique advanced optimize, organic electroluminescence device has been achieved for rapid progress,
But its advantage, the luminous efficiency of organic electroluminescence device, coloration, driving electricity are given full play in the market in FPD
Pressure, service life, device stability etc. also need to further improve.Wherein, the surface work function of anode material, resistivity, light
It learns characteristic, chemical stabilization and whether is matched with base drive circuit and organic layer compatibility, be to determine OLED device photo electric
The key factor of news can be put forward with wide product rate.
Top light emitting OLED device is that pixel-driving circuit is produced below device, this solves the drive of OLED device pixel
The problem of dynamic circuit and display light-emitting area are vied each other, to improve the aperture opening ratio of display device.Make one efficiently
Top light emitting organic electroluminescence device, it is necessary to which one of satisfying the requirements, it is steady to have sought to low resistance, high reflectance, chemical property
It is fixed, and realize good compatible and matched hearth electrode with substrate and hole injection layer material.In top illuminating device, due to existing
Microcavity effect, viewing angle problem can not avoid.
Patent application 201510494601.7, which gives, a kind of scraping the block polymer solution of polybutadienes-polystyrene
The light-emitting surface for being applied to the substrate of setting Organic Light Emitting Diode forms film, then the method for carrying out solidification annealing coating.By
In the cathode of OLED device wave relatively more living, after general vacuum evaporation has prepared cathode, it is necessary to by encapsulation, obstruct air, ability
Ensure the normal work of device.Therefore this method is only applicable to bottom luminescent device, and light-emitting surface passes through at this time in glass substrate at this time
The method of blade coating prepares scattering layer, will not destroy OLED device structure.And for top illuminating device, light-emitting surface is exactly OLED the moon
Pole can destroy OLED device structure, cause device lifetime low or even can not work normally at this time if using the method applied is hung.
In consideration of it, special propose the application.
Invention content
The primary goal of the invention of the application is to propose a kind of preparation method of Organic Light Emitting Diode scattering layer.
The second goal of the invention of the application is to propose the organic light-emitting diodes containing the Organic Light Emitting Diode scattering layer
Pipe product.
In order to complete the purpose of the application, the technical solution used for：
This application involves a kind of preparation methods of Organic Light Emitting Diode scattering layer, and glass transition temperature is less than 120
DEG C material vacuum vapor deposition form film in the shine light-emitting surface of Organic Light Emitting Diode of top, then carry out solidification annealing.
Preferably, the condition of the vacuum evaporation is：It is less than 10 in air pressure-2Under the conditions of Pa, the material is heated to 100
~500 DEG C, the material after vaporization is deposited on the luminous Organic Light Emitting Diode in the top with the rate of 0.1~2nm/s
Light-emitting surface.
Preferably, the thickness that film is formed after the vapor deposition is 20~500nm.
Preferably, the condition of the solidification annealing is to be kept for 1~4 hour under conditions of 80~100 DEG C.
Preferably, the glass transition temperature of the material is less than 100 DEG C.
Preferably, it is 300~800 and in 420~680nm visible-ranges without absorption that the material, which is selected from molecular weight,
Compound.
Preferably, the compound is selected from such as at least one of Formulas I, Formula II, formula III, formula IV compound represented；
Wherein, R11、R12、R13、R14、R21、R22、R31、R32、R41、R42、R43、R44It is separate be respectively selected from substitution or
Unsubstituted C6~26Aryl, C5~22Heterocyclic base；Substituent group is selected from C1~6Alkyl.
Preferably, the arene compounds are selected from least one of following compound：
The application further relates to a kind of luminous Organic Light Emitting Diode in top, is arranged on the light-emitting surface of the Organic Light Emitting Diode
The scattering layer being prepared just like the preparation method of the application.
Preferably, light transmittance of the scattering layer in 400~700nm wave-length coverages be 75~95%, mist degree be 5~
40%.
The technical solution of the application at least has following beneficial effect：
The application is by the material in top-illuminating OLED device light-emitting surface one layer of lower glass transition temperatures (Tg) of vapor deposition, so
So that this layer is atomized by annealing afterwards, has the function that light takes out and scatters, the light extraction efficiency of top-illuminating OLED can be improved and change
Kind visual angle.
Description of the drawings
Fig. 1 is the schematic diagram of the luminous Organic Light Emitting Diode scattering layer in the application top；
Fig. 2 is the schematic diagram of the luminous Organic Light Emitting Diode scattering layer in the application top.
Wherein：
1- scattering layers；
2- top electrodes (Ag-15nm)；
3- organic function layers (HIL/HTL/EML/EIL)；
4- hearth electrodes (ITO/Ag/ITO)；
5- optically coupled layers (CPL).
Specific implementation mode
In top illuminating device, since there are microcavity effect, viewing angle problem can not avoid.It is asked currently in order to solving visual angle
Topic is had and is shone the bottom of using, however bottom shines, there are the insufficient defects of aperture opening ratio.Using transparent metal oxide (TCO) as cloudy
Pole, however TCO is needed to sputter and be prepared, and is damaged to organic film larger.Other such as prepare light using Non-planar substrates, light-emitting surface
It learns the methods of lenticule, encapsulated layer addition scattering particles and there is larger technology difficulty.The high-resolution used due to mobile phone
There is more TFT circuit, so can only generally use top illuminating device structure on the glass substrate of AMOLED.The applicant is logical
Cross sharp study, it is proposed that a kind of preparation method of Organic Light Emitting Diode scattering layer, specially：Glass transition temperature is low
Film is formed in the light-emitting surface of the luminous Organic Light Emitting Diode in top in 120 DEG C of material vapor depositions, then carries out solidification annealing, is lured
Molecular crystalline is led, the film (i.e. scattering layer 1) with micro-structure is formed, there is certain mist degree, generates dispersion effect, to
Solves viewing angle problem.The schematic diagram of dispersion effect is as illustrated in fig. 1 and 2.
As a kind of improvement of the application preparation method, the condition of vacuum evaporation is：It is less than 10 in air pressure-2Under the conditions of Pa,
The material is heated to 100~500 DEG C, the material after vaporization is deposited on the luminous organic hair in top with the rate of 0.1~2nm/s
The light-emitting surface of optical diode.
Wherein, air pressure is preferably 2 × 10-4Pa~10-2Pa, heating temperature are preferably 220~240 DEG C, and deposition rate is preferred
For 0.2~1nm/s.And material can be positioned in crucible and be heated.
As a kind of improvement of the application preparation method, the thickness that film is formed after the vapor deposition is 20~500nm, and excellent
Select 40~100nm, further preferred 50~60nm.If thickness is excessive, the defect that light transmittance can be brought to reduce, and if thickness
It is excessively thin, it is limited to the effect for improving visual angle.
As a kind of improvement of the application preparation method, the condition of the solidification annealing is the item at 80~100 DEG C
It is kept for 1~4 hour under part, and is preferably kept for 3~4 hours under conditions of 90~100 DEG C.In the range, the material of vapor deposition
It crystallizes, being formed has crystallizing layer, to have the effect of atomization.
As a kind of improvement of the application preparation method, the glass transition temperature of material is less than 100 DEG C.The glass of the material
Glass conversion temperature is high, may influence photoelectric properties and the service life of device.The application is by selecting glass transition temperature to be less than
100 DEG C of material does not interfere with the performance of device.
As a kind of improvement of the application preparation method, it is 300~800 and in 420~680nm that material, which is selected from molecular weight,
Compound of the visible-range without absorption.
And the arene compounds that further preferred structure is relatively more symmetrical, planes of molecules is relatively good.
As a kind of improvement of the application preparation method, compound is selected to be changed as shown in Formulas I, Formula II, formula III, formula IV
Close at least one of object；
Wherein, R11、R12、R13、R14、R21、R22、R31、R32、R41、R42、R43、R44It is separate be respectively selected from substitution or
Unsubstituted C6~26Aryl, C5~22Heterocyclic base；Substituent group is selected from C1~6Alkyl.
Carbon atom number be 6~26 aryl, such as phenyl, benzene alkyl, at least contain there are one phenyl aryl such as xenyl,
Condensed-nuclei aromatics base such as naphthalene, anthracene, phenanthrene, xenyl and condensed-nuclei aromatics base can also be replaced by alkyl or alkenyl.Preferably, it selects
Select carbon atom number be 6~16 aryl, it is further preferred that select carbon atom number for 6~14 aryl, still more preferably
Ground, select carbon atom number for 6~9 aryl.As the example of aryl, can specifically enumerate：Phenyl, benzyl, xenyl, to first
Phenyl, o-tolyl, tolyl.
The heterocyclic base that carbon atom number is 5~26, can be selected from：Furyl, thienyl, pyrrole radicals, thiazolyl, imidazole radicals, pyrrole
Piperidinyl, pyrazinyl, pyrimidine radicals, pyridazinyl, indyl, quinolyl.
Preferably, R11、R12、R13、R14、R21、R22It is separate be respectively selected from substituted or unsubstituted phenyl, naphthalene,
Pyridyl group；Substituent group is selected from C1~6Alkyl.
As a kind of improvement of the application preparation method, arene compounds are selected from least one of following compound；
The application further relates to a kind of Organic Light Emitting Diode, is provided with top on the light-emitting surface of the Organic Light Emitting Diode
The scattering layer 1 that method is prepared.
As a kind of improvement of the application OLED, light transmittance of the scattering layer 1 in 400~700nm wave-length coverages be 75~
95%, mist degree is 5~40%；
Preferably, light transmittance of the scattering layer 1 in 400~700nm wave-length coverages be 80~92%, mist degree be 10~
20%.
Embodiment
Material shown in table 1 is used for vacuum evaporation, vapor deposition forms thin in the light-emitting surface of the luminous Organic Light Emitting Diode in top
Then film carries out solidification annealing；The thickness of the scattering layer 1 of formation is 250nm；The condition of vacuum evaporation and curing process is such as
Shown in table 2；
Table 1：
Table 2：
Wherein, comparative example 3 and embodiment 6 are that the CPL5 of 200nm thickness is prepared using compound shown in formula 5, are then being used
1 compound of formula prepares the scattering layer 1 of 50nm thickness.
Detection method：
Current efficiency：By OLED top illuminating device light-emitting surface face spectral investigators, apply to the OLED device that area is S
2~6V voltages, stepping 0.1V test electric current (I) and the light emission luminance B under each voltage (V), current efficiency E=SB/I；
Luminous efficiency=π SB/ (I × V)；
60 ° of brightness：OLED device is rotated, makes the normal of OLED device light-emitting surface and the axis angle of spectrum test instrument be
60 °, the brightness B2 divided by B of acquisition, as 60 ° of brightness are tested at this time.
Experimental result is as shown in table 3：
Table 3：
The material of lower glass transition temperatures is respectively adopted as scattering layer in Examples 1 to 6, and carries out thermal annealing, produces
Raw obvious atomizing effect.The current efficiency, luminous efficiency, 60 degree of brightness for generating each embodiment of atomizing effect are different
The raising of degree illustrates that the scattering layer after atomization plays the role of light and takes out and scatter really, and finally improves top and shine
The light extraction efficiency of OLED simultaneously improves visual angle.
Although comparative example 1 is using the material of lower glass transition temperatures, without by annealing, not generating atomization effect
Fruit.
Comparative example 2 and 3 uses high glass transition temperature materials, and (100 under the tolerable maximum conditions of OLED device
DEG C annealing 4 hours) annealing, also without generate atomizing effect.
It is not for limiting claim, any this field skill although the application is disclosed as above with preferred embodiment
Art personnel can make several possible variations and modification under the premise of not departing from the application design, therefore the application
Protection domain should be subject to the range that the application claim is defined.
Claims (8)
1. a kind of preparation method of Organic Light Emitting Diode scattering layer, which is characterized in that by glass transition temperature be 62~100
DEG C material vacuum vapor deposition form film in the shine light-emitting surface of Organic Light Emitting Diode of top, then carry out solidification annealing, lure
Lead molecular crystalline；
The condition of the solidification annealing is to be kept for 1~4 hour under conditions of 80~100 DEG C.
2. preparation method according to claim 1, which is characterized in that the condition of the vacuum evaporation is：It is less than in air pressure
10-2Under the conditions of Pa, the material is heated to 100~500 DEG C, the material after vaporization is sunk with the rate of 0.1~2nm/s
Product is in the light-emitting surface of the luminous Organic Light Emitting Diode in the top.
3. preparation method according to claim 1, which is characterized in that after the vapor deposition formed film thickness be 20~
500nm。
4. preparation method according to claim 1, which is characterized in that the material be selected from molecular weight be 300~800 and
In compound of 420~680nm visible-ranges without absorption.
5. preparation method according to claim 4, which is characterized in that the compound is selected to be changed as shown in Formulas I, Formula II
Close at least one of object；
Wherein, R11、R12、R13、R14、R21、R22It is separate to be respectively selected from substituted or unsubstituted C6~26Aryl, C5~22Virtue is miscellaneous
Base；Substituent group is selected from C1~6Alkyl.
6. preparation method according to claim 5, which is characterized in that the compound is in following arene compounds
At least one：
The Organic Light Emitting Diode 7. a kind of top shines, which is characterized in that be provided on the light-emitting surface of the Organic Light Emitting Diode
The scattering layer that the preparation method as described in claim 1~6 is prepared.
The Organic Light Emitting Diode 8. top according to claim 7 shines, which is characterized in that the scattering layer 400~
Light transmittance in 700nm wave-length coverages is 75~95%, and mist degree is 5~40%.
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| US10270033B2 (en) | 2015-10-26 | 2019-04-23 | Oti Lumionics Inc. | Method for patterning a coating on a surface and device including a patterned coating |
| CN118215323A (en) | 2016-12-02 | 2024-06-18 | Oti照明公司 | Device comprising a conductive coating disposed over an emission region and method thereof |
| CN110785867B (en) | 2017-04-26 | 2023-05-02 | Oti照明公司 | Method for patterning a surface coating and apparatus comprising a patterned coating |
| WO2018211460A1 (en) | 2017-05-17 | 2018-11-22 | Oti Lumionics Inc. | Method for selectively depositing a conductive coating over a patterning coating and device including a conductive coating |
| US11751415B2 (en) | 2018-02-02 | 2023-09-05 | Oti Lumionics Inc. | Materials for forming a nucleation-inhibiting coating and devices incorporating same |
| JP7320851B2 (en) | 2018-05-07 | 2023-08-04 | オーティーアイ ルミオニクス インコーポレーテッド | Methods for providing auxiliary electrodes and devices containing auxiliary electrodes |
| CN116456753A (en) | 2019-03-07 | 2023-07-18 | Oti照明公司 | Optoelectronic device |
| CN110098345B (en) * | 2019-04-17 | 2020-11-06 | 深圳市华星光电半导体显示技术有限公司 | Organic light emitting diode display and method of manufacturing the same |
| KR20220009961A (en) | 2019-04-18 | 2022-01-25 | 오티아이 루미오닉스 인크. | Material for forming nucleation inhibiting coating and device comprising same |
| KR20220017918A (en) | 2019-05-08 | 2022-02-14 | 오티아이 루미오닉스 인크. | Material for forming nucleation inhibiting coating and device comprising same |
| US11832473B2 (en) | 2019-06-26 | 2023-11-28 | Oti Lumionics Inc. | Optoelectronic device including light transmissive regions, with light diffraction characteristics |
| JP7386556B2 (en) | 2019-06-26 | 2023-11-27 | オーティーアイ ルミオニクス インコーポレーテッド | Optoelectronic devices containing optically transparent regions with applications related to optical diffraction properties |
| KR20220045202A (en) | 2019-08-09 | 2022-04-12 | 오티아이 루미오닉스 인크. | Optoelectronic Device Including Auxiliary Electrodes and Partitions |
| US12113279B2 (en) | 2020-09-22 | 2024-10-08 | Oti Lumionics Inc. | Device incorporating an IR signal transmissive region |
| DE102020215067A1 (en) | 2020-11-30 | 2022-06-02 | Robert Bosch Gesellschaft mit beschränkter Haftung | Display device for displaying at least one image, method for producing a display device and method for operating a display device |
| WO2022123431A1 (en) | 2020-12-07 | 2022-06-16 | Oti Lumionics Inc. | Patterning a conductive deposited layer using a nucleation inhibiting coating and an underlying metallic coating |
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| JP2009205981A (en) * | 2008-02-28 | 2009-09-10 | Fujifilm Corp | Organic electroluminescent element and its manufacturing method |
| KR101147428B1 (en) * | 2009-02-09 | 2012-05-23 | 삼성모바일디스플레이주식회사 | Organic light emitting diode display |
| JP5986992B2 (en) * | 2010-06-14 | 2016-09-06 | ノヴァレッド ゲーエムベーハー | Organic light emitting device |
| TWI451611B (en) * | 2011-05-19 | 2014-09-01 | Au Optronics Corp | Organic emitting device |
| CN104508855B (en) * | 2012-05-31 | 2017-06-23 | 乐金显示有限公司 | Organic light emitting diode |
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