CN106784396A - Organic electroluminescence device, transmission layer material, doping method and preparation method - Google Patents
Organic electroluminescence device, transmission layer material, doping method and preparation method Download PDFInfo
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- CN106784396A CN106784396A CN201611090306.6A CN201611090306A CN106784396A CN 106784396 A CN106784396 A CN 106784396A CN 201611090306 A CN201611090306 A CN 201611090306A CN 106784396 A CN106784396 A CN 106784396A
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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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/15—Hole transporting layers
- H10K50/155—Hole transporting layers comprising dopants
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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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
- H10K50/165—Electron transporting layers comprising dopants
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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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- 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
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
Abstract
The present invention discloses organic electroluminescence device, transmission layer material, doping method and preparation method, and doping method includes step：The material of main part and dopant material of transport layer are placed in cavity, and electroded substrate is placed in the cavity；The material of main part and dopant material of transport layer are made on substrate, and the doping concentration of dopant material is set and be gradually reduced to the mode that nonlinear change is sentenced away from substrate from substrate, complete non-linear doping.Non-linear doping techniques of the invention, substantially increase stock utilization, improve device current characteristic, power efficiency and device job stability, with feasibility and application prospect higher, so that its application in the opto-electronic device is more extensive.
Description
Technical field
The present invention relates to field of light emitting materials, more particularly to organic electroluminescence device, transmission layer material, doping method and
Preparation method.
Background technology
Organic electroluminescence device (Organic Light Emitting Devices, OLED) was used as a new generation in recent years
Display device, by the extensive concern of researcher.Organic electroluminescence device and liquid crystal display device（LCD）Compare, have
Brightness is high, active is luminous, visual angle is wide, fast response time the features such as, be the up-and-coming youngster of flat display field, show good
Development and application prospect.
At present, the OLED of most of high efficiency OLED and commercialization volume production is all the skill for employing doping
Art.Doping is by a certain amount of guest materials（Also referred to as dopant material）It is mixed into material of main part, by energy transmission or electric charge
Shift to obtain the technology of device performance higher.Doping is a kind of technology being widely used in OLED, and it is by guest materials
It is entrained in appropriate luminescent layer material of main part, electroluminescent efficiency can be made to be increased dramatically.And doping techniques are not only wide
General to be applied in luminescent layer, the p-i-n in transport layer is entrained in and has also obtained in-depth study nearly ten years.For example by p-type or n
Type dopant is entrained in the material of main part of corresponding hole or electron transfer layer respectively, can significantly improve the injection of carrier
With transmission characteristic, improve the power efficiency of device.
Generally, in the transport layer of application doping techniques, in order to improve carrier injection and transmission, the material for being used is all
It is Uniform Doped, as shown in figure 1, during with thickness change, doping rate is always maintained at constant, for example, adopted in transport layer
Adulterated with uniform p or N-shaped, although this method has been proved to that good device performance can be obtained, but still exists many
Problem.For example when the transport layer thickness of Uniform Doped is more than 2nm, electron injection efficiency can decline on the contrary.Because uniformly mixing
In acrobatics art, injection energy barrier is larger, hinders carrier injection and transmits, as shown in Fig. 2 wherein EFRepresent fermi level.
Generally speaking, its stability of current doping way is not high, and the aspect such as device performance such as current characteristics and efficiency is also
Have much room for improvement.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide organic electroluminescence device, transport layer material
Material, doping method and preparation method, it is intended to solve that existing doping way stability is high, device performance has much room for improvement asks
Topic.
Technical scheme is as follows：
A kind of organic electroluminescence device transmits the doping method of layer material, wherein, including step：
The material of main part and dopant material of transport layer are placed in cavity, and electroded substrate is placed in the cavity；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping.
Described organic electroluminescence device transmits the doping method of layer material, wherein, using mobile evaporation mode come real
Existing non-linear doping.
Described organic electroluminescence device transmits the doping method of layer material, wherein, during mobile evaporation, control
The substrate is moved between the evaporation source of different materials, completes non-linear doping.
Described organic electroluminescence device transmits the doping method of layer material, wherein, using the side of organic vapor phase deposition
Be deposited on different materials on substrate by formula, completes non-linear doping.
Described organic electroluminescence device transmits the doping method of layer material, wherein, to being passed through inert gas in cavity,
And the crucible for being loaded with different materials is flowed through, the material in corresponding crucible is incidentally played by the inert gas, and then make each
Material is sent at substrate and deposits, and in deposition process, the doping concentration of each material is controlled by adjusting inert gas flow velocity.
A kind of organic electroluminescence device transmits layer material, wherein, it is obtained using the doping method described in as above any one.
A kind of preparation method of organic electroluminescence device, wherein, including step：
First substrate is cleaned；
Device layers material and substrate are placed in cavity；Wherein, the transport layer of device includes material of main part and doping material
Material；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping；
By device, remaining layers of material is made on substrate.
The preparation method of described organic electroluminescence device, wherein, non-linear mixing is realized using mobile evaporation mode
It is miscellaneous.
The preparation method of described organic electroluminescence device, wherein, by different materials by the way of organic vapor phase deposition
Material is deposited on substrate, completes non-linear doping.
A kind of organic electroluminescence device, wherein, it is made of the preparation method described in as above any one.
Beneficial effect：Non-linear doping techniques of the invention, substantially increase stock utilization, improve device current special
Property, power efficiency and device job stability, with feasibility and application prospect higher, so that it is in the opto-electronic device
Using more extensive.
Brief description of the drawings
Fig. 1 is the doping concentration schematic diagram of Uniform Doped in the prior art.
Fig. 2 is the injection energy barrier schematic diagram of the transport layer of Uniform Doped in the prior art.
Fig. 3 is the doping concentration schematic diagram of non-linear doping in the present invention.
Fig. 4 is the injection energy barrier schematic diagram of the transport layer of non-linear doping in the present invention.
Fig. 5 is the schematic diagram of traditional vacuum thermal evaporation deposition.
Fig. 6 is the schematic diagram of mobile vapour deposition method in the present invention.
Fig. 7 is the schematic diagram of organic vapor phase deposition in the present invention.
Fig. 8 is a device architecture schematic diagram for specific embodiment in the present invention.
Fig. 9 is the doping ratio change schematic diagram of dopant material in Fig. 8 embodiments.
Specific embodiment
The present invention provides organic electroluminescence device, transmission layer material, doping method and preparation method, of the invention to make
Purpose, technical scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that this place is retouched
The specific embodiment stated only is used to explain the present invention, is not intended to limit the present invention.
A kind of organic electroluminescence device provided by the present invention transmits the doping method preferred embodiment of layer material, its bag
Include step：
The material of main part and dopant material of transport layer are placed in cavity, and electroded substrate is placed in the cavity；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping.
The present invention is according to transport layer（Can be hole transmission layer or electron transfer layer）The specific feature of doping, using non-thread
Property change doping method, doping concentration is from the substrate（I.e. at electrode）To at away from substrate（I.e. near luminescent layer）
It is gradually reduced in the way of nonlinear change, as shown in figure 3,100wt% of such as doping concentration from close substrate is with non-linear
The 0wt% that is down at the luminescent layer of trend, so as to improve device power efficiency.
By taking p-type doping as an example, the high-dopant concentration at anode can effectively improve the injection efficiency of device, and be close to
Low doping concentration at luminescent layer can not only ensure that carrier has mobility higher, while being also prevented from the expansion of dopant
Dissipate.Meanwhile, middle gradient doping can provide smooth transmission channel for carrier, and its operation principle is as shown in Figure 4.In sky
Cave transport layer or electron transfer layer can significantly improve the current characteristics and power efficiency of device using nonlinear change doping.
The method can not only improve the power efficiency of OLED, simultaneously because nonlinear change doping eliminates traditional carrier note
Enter obvious heterojunction structure present in mode, the stability of device work can be significantly improved.Big chi can also be realized simultaneously
Very little volume production.Volume production is also easily realized in nonlinear change doping simultaneously, with promotional value.
Similar with inorganic semiconductor doping, the change in concentration of organic semiconductor doping can also cause the movement of fermi level.
Transmitting state E μ and fermi level EFBetween distance can be measured by Seebeck effects.
In formula, κBIt is Boltzmann constant, e is elementary charge, and T is absolute temperature, and A is numerical factor.Seebeck measurements show
Fermi level and transmitting state spacing reduce with the increase of doping concentration.Under different levels of doping, fermi level, conductance
Rate and space charge layer thickness can all produce change.In general, high-concentration dopant can not only reduce injection energy barrier, may be used also
To effectively reduce space charge layer thickness.But after doping concentration is improved to a certain extent, although carrier injectability is obtained
Transmission to improvement, but carrier may be restricted.High-concentration dopant is easier the diffusion phenomena for dopant occur simultaneously, because
This, all the agent of Uniform Doped high-concentration dopant is not a preferable doping way in whole transport layer.
Conventional p-type and N-shaped doping concentration are all very low at present, and for example p-type dopant F4-TCNQ is in hole transport layer main body
Doping in material Meo-TPD is than generally 2-4mol%（By mole meter）, but injection energy barrier now is not minimum
Value, transport layer thickness is also up to 8nm, and is unfavorable for the injection of carrier.In order to the injection and transmission that consider carrier are asked
Be incorporated into the concept that nonlinear change is adulterated in transport layer by topic, the present invention.From unlike conventional uniform doping techniques, it is mixed
Miscellaneous concentration is not uniform constant in the whole transport layer for needing doping, due to doping concentration consecutive variations, therefore is not deposited
In obvious heterojunction boundary.And the doping concentration of this consecutive variations can adjust fermi level, hole can be in HOMO
Upper smooth transmission, as shown in Figure 4.
In the present invention, doping method is particularly important, according to traditional vacuum thermal evaporation, as shown in figure 5, it is to pass through
Temperature of the regulation different materials in silica crucible, so as to control evaporation rate（By crystal-vibration-chip monitor in real time）To realize certain ratio
The doping of example, but its stock utilization is very low, and most of material is all wasted in the cavity beyond substrate.Further, since warm
The other factors such as degree control, evaporation rate is difficult precise control, so being not to be best suitable for making non-linear doping device.The present invention
Non-linear doping can be realized using mobile mobile evaporation mode.Due to the material of hot evaporation be with taper diverging in the form of to
Upper evaporation, so during mobile evaporation, as shown in fig. 6, control base board with a certain speed different materials evaporation source
Between move, and the evaporation rate and ratio of material of main part and dopant material are set, so as to complete non-linear doping, its uniformity
Height, repeatability is high.
In addition, the present invention can also use organic vapor phase deposition mode（OVPD）Different materials are deposited on substrate, come real
Existing non-linear doping.Organic vapor phase deposition can also well overcome the defect of traditional hot evaporation method, and be equally applicable to
The volume production of large-size substrate.Especially by regulation inert gas flow velocity control doping ratio.Its operation principle as shown in fig. 7, to
Inert gas, inert gas such as N are passed through in cavity2Flow through the crucible for being loaded with different materials of heating and incidentally play corresponding crucible
In organic material, and then make organic material be transferred at substrate deposit, in deposition process, sedimentation rate can be easy to
Ground adjusted by flow controller, as long as therefore regulation inert gas flow velocity can just control doping ratio, it is easy to prepare non-
Linear doping device.
The present invention also provides a kind of organic electroluminescence device transmission layer material preferred embodiment, and it uses as above any one
Described doping method is obtained.
The present invention also provides a kind of preparation method preferred embodiment of organic electroluminescence device, and it includes step：
First substrate is cleaned；
Device layers material and substrate are placed in cavity；Wherein, the transport layer of device includes material of main part and doping material
Material；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping；
By device, remaining layers of material is made on substrate.
Further, non-linear doping is realized using mobile evaporation mode.Or will by the way of organic vapor phase deposition
Different materials are deposited on substrate, complete non-linear doping.
The present invention also provides a kind of organic electroluminescence device preferred embodiment, and it uses the preparation described in as above any one
Method is made.
A specific embodiment is provided below specifically to retouch organic electroluminescence device preparation process of the invention
State.
Ultrasonic cleaning treatment is carried out with glass cleaner, acetone and isopropanol respectively in order to ito substrate first, it is each
The ultrasonic cleaning process time of step is 15 minutes, is cleaned by ultrasonic after terminating with deionized water rinsing ito substrate to remove residual
Solution, then dries up with high pure nitrogen rapidly and continues heating, drying.
Then by layers of material, such as EIL（Electron injecting layer）, ETL（Electron transfer layer）, EML（Luminescent layer）, HTL（Hole
Transport layer）, HIL（Hole injection layer）And negative electrode, and ito substrate is all placed in cavity, cavity is vacuumized, until vacuum
Degree is reduced to 5 × 10−6Below Torr can start evaporation, and not opening cavity in preparation process carries out vacuum breaker action.
The device architecture that the present embodiment is used, as shown in figure 8, being specially：ITO/HTL/CBP:Ir(ppy)3(20nm,
8wt%)/BPhen (50 nm)/Liq (1 nm)/Al (100 nm)。
The wherein dopant material of HTL（Nonlinear way is adulterated）It is F4-TCNQ, the structure of material of main part NBP, HTL is F4-
TCNQ(2nm)/NPB:F4-TCNQ(y nm,40wt%)/ NPB:F4-TCNQ (5 nm, 10wt%)/NPB (45-y nm), y can be with
It is 5,15,25 or 35 to be.Liq/BPhen is electron injection and transmission structure, and luminescent layer employs material of main part CBP（Doping is green
Color phosphor material Ir (ppy)3）.The doping ratio change of nonlinear change doping transport layer is as shown in figure 9, in system in the present invention
In different time during standby, hole transmission layer material of main part NPB and other organic materials are set into evaporation rate 0.1 ~ 2
In the range of/s, dopant material F4-TCNQ sets evaporation rate difference according to doping ratio 40wt% and 10wt% in hole transmission layer
It is 0.04-0.8/s and 0.01-0.2/s, metal electrode material（Al）Evaporation rate be 5 ~ 10/s.These evaporation speed
Rate can be according to quartz crystal real-time monitoring.
When using mobile evaporation, the settable translational speed with 1-10cm/s of substrate is moved between evaporation source；
When being deposited with using organic vapor phase deposition, inert gas N used2Pressure can be 100Pa, and gas flow rate may be configured as 0.1-
1m/s, so that drive organic material to be deposited on substrate, it is final that required device architecture is obtained.
In sum, in the nonlinear change doping of transport layer, the high-concentration dopant at electrode can be carried effectively
The injection efficiency of high carrier, and the low concentration doping at luminescent layer can not only ensure that carrier has migration higher
Rate, while being also prevented from the diffusion of dopant.Meanwhile, the gradient doping of zone line can provide smooth biography for carrier
Defeated passage.The present invention can not only improve the power efficiency of OLED, simultaneously because nonlinear change doping eliminates tradition
Obvious heterojunction structure present in carrier injection mode, can significantly improve the stability of device work.Simultaneously can also
Realize the volume production of large scale product.
It should be appreciated that application of the invention is not limited to above-mentioned citing, and for those of ordinary skills, can
To be improved according to the above description or converted, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Shield scope.
Claims (10)
1. a kind of organic electroluminescence device transmits the doping method of layer material, it is characterised in that including step：
The material of main part and dopant material of transport layer are placed in cavity, and electroded substrate is placed in the cavity；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping.
2. organic electroluminescence device according to claim 1 transmits the doping method of layer material, it is characterised in that use
Evaporation mode is moved to realize non-linear doping.
3. organic electroluminescence device according to claim 2 transmits the doping method of layer material, it is characterised in that moving
During dynamic evaporation, control the substrate to be moved between the evaporation source of different materials, complete non-linear doping.
4. organic electroluminescence device according to claim 1 transmits the doping method of layer material, it is characterised in that use
Be deposited on different materials on substrate by the mode of organic vapor phase deposition, completes non-linear doping.
5. organic electroluminescence device according to claim 4 transmits the doping method of layer material, it is characterised in that to chamber
Inert gas is passed through in body, and flows through the crucible for being loaded with different materials, corresponding crucible is incidentally played by the inert gas
In material, and then make each material be sent at substrate to deposit, in deposition process, by adjust inert gas flow velocity control it is each
The doping concentration of material.
6. a kind of organic electroluminescence device transmits layer material, it is characterised in that using as described in any one of claim 1 ~ 5
Doping method is obtained.
7. a kind of preparation method of organic electroluminescence device, it is characterised in that including step：
First substrate is cleaned；
Device layers material and substrate are placed in cavity；Wherein, the transport layer of device includes material of main part and doping material
Material；
The material of main part and dopant material of transport layer are made on substrate, and set the doping concentration of dopant material from
It is gradually reduced to the mode for sentencing nonlinear change away from substrate at substrate, completes non-linear doping；
By device, remaining layers of material is made on substrate.
8. the preparation method of organic electroluminescence device according to claim 7, it is characterised in that using mobile evaporation side
Formula realizes non-linear doping.
9. the preparation method of organic electroluminescence device according to claim 7, it is characterised in that sunk using organic vapors
Be deposited on different materials on substrate by long-pending mode, completes non-linear doping.
10. a kind of organic electroluminescence device, it is characterised in that using the preparation method as described in any one of claim 7 ~ 9
It is made.
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| CN201611090306.6A CN106784396A (en) | 2016-12-01 | 2016-12-01 | Organic electroluminescence device, transmission layer material, doping method and preparation method |
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| CN201611090306.6A CN106784396A (en) | 2016-12-01 | 2016-12-01 | Organic electroluminescence device, transmission layer material, doping method and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110718636A (en) * | 2018-07-11 | 2020-01-21 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN111384279A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Quantum dot light-emitting diode |
| WO2022116653A1 (en) * | 2020-12-04 | 2022-06-09 | 昆山国显光电有限公司 | Display panel and evaporation method therefor |
-
2016
- 2016-12-01 CN CN201611090306.6A patent/CN106784396A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 王经: "渐变掺杂技术在有机发光二极管中的应用", 《上海交通大学硕士学位论文》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110718636A (en) * | 2018-07-11 | 2020-01-21 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN111384279A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Quantum dot light-emitting diode |
| CN111384279B (en) * | 2018-12-29 | 2021-06-22 | Tcl科技集团股份有限公司 | Quantum dot light-emitting diode |
| WO2022116653A1 (en) * | 2020-12-04 | 2022-06-09 | 昆山国显光电有限公司 | Display panel and evaporation method therefor |
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Application publication date: 20170531 |