CN105932177A - Organic electroluminescent device, light-emitting layer material, doping method, and preparation method - Google Patents
Organic electroluminescent device, light-emitting layer material, doping method, and preparation method Download PDFInfo
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- CN105932177A CN105932177A CN201610320771.8A CN201610320771A CN105932177A CN 105932177 A CN105932177 A CN 105932177A CN 201610320771 A CN201610320771 A CN 201610320771A CN 105932177 A CN105932177 A CN 105932177A
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- doping
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- organic electroluminescence
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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
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Abstract
The invention discloses an organic electroluminescent device, a light-emitting layer material, a doping method, and a preparation method. The doping method comprises the steps: enabling the doping densities of at least two types of main materials to respectively change from high to low and from low to high in a linear manner, and achieving the linear doping. The linear doping mode is employed for making the light-emitting layer material. The doping method is good in uniformity, and is high in repeatability. The light-emitting efficiency of an OLED can be improved through employing the light-emitting layer material. The doping method reduces the efficiency roll-off and brightness decay, prolongs the service life of the device, greatly improves the performances of the device, and also can achieve the batch production of a large-size device.
Description
Technical field
The present invention relates to display material field, particularly relate to organic electroluminescence device, emitting layer material, doping method and
Preparation method.
Background technology
Organic luminescent device (Organic Light Emitting Devices, OLED) conduct display device of new generation,
Extensive concern by research worker.Organic electroluminescence device, compared with liquid crystal display device (LCD), has brightness high, main
Move the features such as luminescence, visual angle width, fast response time, be the up-and-coming youngster of flat display field, present development and application prospect.
At present, major part high efficiency OLED and be all utilized in mixing in luminescent layer in the product of commercialization volume production
Miscellaneous mode.Doping refers to be mixed in material of main part a certain amount of guest materials, is transmitted by energy or electric charge transfer comes
Obtain the technology of higher device performance.The appearance of host-guest system illumination mode is key factor fast-developing for OLED in recent years
One of, this is owing to which employs the material of main part various high fluorescence of collocation having superior carrier transmission characteristics and the characteristics of luminescence
Or the luminescent material of Phosphor efficiency, thus obtain efficient electroluminescent efficiency and different photochromic.Come from MOLECULE DESIGN angle
Saying, the transmission performance of a kind of material and luminous efficiency tend not to get both, and therefore use the mode of host-guest system, can be to not
The chief is respectively taken with types of material.In the device of host-guest system, why guest materials can be luminous efficiently, is because height
The light emitting host material of energy transfers energy in low-energy light emitting guest material.It addition, because produce on material of main part
Exciton to transfer energy to the higher object of luminous efficiency luminous on material, the degree of stability of device work is the highest.
As it is shown in figure 1, traditional doping process is all to be entrained in equably in guest materials by guest materials.In conjunction with Fig. 2
Shown in Fig. 3, this technology is in luminous layer structure (main body 1 generation in figure of the most common double emitting layers and hybrid agent structure
Table one material of main part, main body 2 represents another kind of material of main part, and object represents guest materials, and EML represents luminescent layer) in design
Device efficiency can be improved.Although this method has been proved to obtain good device performance, but still exists many
Problem, such as running voltage are high, external quantum efficiency is low, and current efficiency can gradually decay, and luminous efficiency is relatively low etc..
Therefore, prior art has yet to be improved and developed.
Summary 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, luminescent layer material
Material, doping method and preparation method, it is intended to solve existing doping method and still have that running voltage is high, external quantum efficiency is low, electricity
Stream efficiency can gradually decay, the problems such as luminous efficiency is relatively low.
Technical scheme is as follows:
A kind of doping method of organic electroluminescence device emitting layer material, wherein, including step:
The two of luminescent layer kinds of material of main parts and a kind of guest materials are placed in the cavity of evaporation, and will be used for depositing respectively
The substrate of layer material is placed in described cavity；
Then cavity is carried out evacuation process；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
To complete linear doping.
The doping method of described organic electroluminescence device emitting layer material, wherein, uses linear evaporation mode to come real
Existing linear doping.
The doping method of described organic electroluminescence device emitting layer material, wherein, during linear evaporation, controls
Described substrate moves between the evaporation source of different materials, completes linear doping.
The doping method of described organic electroluminescence device emitting layer material, wherein, uses the side of organic vapor phase deposition
Different materials is deposited on substrate by formula, completes linear doping.
The doping method of described organic electroluminescence device emitting layer material, wherein, is passed through noble gas in cavity,
And flow through the crucible being loaded with different materials, incidentally play the material in corresponding crucible by described noble gas, and then make each
Material is sent at substrate deposit, and in deposition process, is controlled the doping content of each material by regulation noble gas flow velocity.
A kind of organic electroluminescence device emitting layer material, wherein, uses doping method as above to prepare.
A kind of preparation method of organic electroluminescence device, wherein, including step:
First substrate is carried out, carries out after cleaning drying up process, then heating, drying；
Device layers material and substrate are placed in cavity, to cavity evacuation；The emitting layer material of device includes two kinds of masters
Body material and a kind of guest materials；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
Complete linear doping.
The preparation method of described organic electroluminescence device, wherein, uses linear evaporation mode to realize linear doping.
The preparation method of described organic electroluminescence device, wherein, uses the mode of organic vapor phase deposition by difference material
Material is deposited on substrate, completes linear doping.
A kind of organic electroluminescence device, wherein, makes including preparation method as above.
Beneficial effect: the present invention uses the mode of linear doping to make emitting layer material, and the method for the present invention has all
The feature that even property is good and repeatability is high, utilizes this emitting layer material can improve the luminous efficiency of OLED of preparation, reduces
Efficiency roll-off and brightness decay, extend device lifetime, and device performance is greatly enhanced, and also can realize large-size device simultaneously
Volume production.
Accompanying drawing explanation
Fig. 1 is Uniform Doped doping content schematic diagram in organic layer in prior art.
Fig. 2 is the doping way schematic diagram of Subjective and Objective material in double emitting layers structure in prior art.
Fig. 3 is the doping way schematic diagram of Subjective and Objective material in hybrid agent structure in prior art.
Fig. 4 is the doping content schematic diagram being linearly entrained in the present invention in organic layer.
Fig. 5 is the doping way schematic diagram of Subjective and Objective material in linear doped body tie structure in the present invention.
Fig. 6 is the schematic diagram of the hot vapour deposition method of traditional vacuum.
Fig. 7 is the schematic diagram of mobile vapour deposition method in the present invention.
Fig. 8 is the schematic diagram of organic vapor phase deposition in the present invention.
Fig. 9 is the device architecture schematic diagram of a specific embodiment in the present invention.
Figure 10 is the organic material energy diagram of Fig. 9 embodiment.
Figure 11 is the change of the doping content in linear doped body tie structure schematic diagram in Fig. 9 embodiment.
Detailed description of the invention
The present invention is provided with organic electroluminescence devices, emitting layer material, doping method and preparation method, for making the present invention's
Purpose, technical scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.Should be appreciated that this place is retouched
The specific embodiment stated only in order to explain the present invention, is not intended to limit the present invention.
The doping method of a kind of organic electroluminescence device emitting layer material provided by the present invention, it includes step:
The two of luminescent layer kinds of material of main parts and a kind of guest materials are placed in the cavity of evaporation, and will be used for depositing respectively
The substrate of layer material is placed in described cavity；
Then cavity is carried out evacuation process；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
To complete linear doping.
Such as the doping content of two kinds of material of main parts (is continuously reduced) from high to low and (increases continuously from low to high respectively
Linear change greatly), guest materials to be ensured is compared the doping content of luminescent layer total amount and is kept constant.
The doping method of the present invention can effectively widen Carrier composite, and along with the increase of electric current, this region
Also will widen further, therefore exciton recombination probability is greatly increased, and not only increases device efficiency, it is also possible to reduce phosphorescent OLED
Because of TTA(T-T annihilation in device) and TPQ(triplet-polaron cancellation) and the efficiency roll-off that causes.Isochrone
Property doping can also realize the volume production of large-size device, there is wide market application foreground.
Unlike conventional uniform doping techniques, linear doping technology employed in the present invention, its doping content is whole
The individual emitting layer material needing doping is not the most constant, as shown in Figure 4, along with the increase of thickness, at linear doping
In agent structure, the doping content of two kinds of material of main parts is also in change, and the doping content of guest materials is constant, as shown in Figure 5.
As applied in phosphor material by the doping method of the present invention, phosphor material has higher internal quantum efficiency than fluorescent material,
Device light emitting efficiency also can be higher.And one of main problem of phosphorescent OLED luminescence is exactly efficiency roll-off: along with electric current density
Increase, device current efficiency can gradually decay.This not only affects OLED application under high illumination, also can be because of white light
In OLED, different luminescent material efficiency roll-off are inconsistent and cause the colour cast under different electric current densities.Cause this efficiency roll-off
Principal element be exactly TTA and TPQ process.Both processes can represent by formulas below:
TTA:(1)
TPQ:(2)
In formula, D represents that alms giver, A represent acceptor.The triplet excited state of acceptor or cation and anion can make alms giver's
Triplet excited state returns to ground state in non-luminous mode, thus reduces device light emitting efficiency.
Because exciton typically can be combined in the interface of luminescent layer and transport layer in single luminous layer structure, recombination region is the narrowest
And cause device performance the best.So the most a lot of devices use double emitting layers and hybrid agent structure to improve the luminous effect of device
Rate and life-span, both structures can balance hole and electron concentration in luminescent layer, widen recombination region, be effectively improved device
Efficiency roll-off problem, can be effectively improved device performance, but in double emitting layers structure, luminescent layer is divided into two-layer, uses respectively
Two kinds of different material of main parts, owing to both storerooms exist energy barrier, therefore exciton trends towards at two kinds of main body materials of luminescent layer
The interface of material is combined, and recombination region is the narrowest.It addition, carrier can accumulate at two kinds of different light emitting host storerooms,
Add TTA and TPQ odds.And hybrid agent structure is by luminescent material and two or more in single luminescent layer
The structure that material of main part is blended, due to the difference of two kinds of material of main part doping ratios, therefore hole or electronics in luminescent layer
Injection efficiency can not all reach optimum.
Linear doping method of the present invention, then the advantage combining above two agent structure, and compensate for
Each not enough, hole and electronics can respectively on two kinds of material of main parts to luminescent layer internal transmission, so can effectively adjust
Joint exciton recombination region, therefore, in the linear agent structure that the present invention is formed, exciton recombination region is wider, TTA and TPQ
Can also be effectively suppressed.
In the present invention, doping method is particularly important, and according to traditional vacuum thermal evaporation, as shown in Figure 6, it is to pass through
Regulation different materials temperature in silica crucible, thus control evaporation rate to realize a certain proportion of doping, but its material
Utilization rate is the lowest, and major part material is all wasted in the cavity beyond substrate.Further, since other factors such as temperature control,
Evaporation rate is difficult to accurately control, so being not to be best suitable for making linear doping device.The present invention can use linear evaporation mode
Realize linear doping.Owing to the material of heat evaporation is that the form dissipated with taper is upwards evaporated, so being linearly deposited with
Cheng Zhong, as it is shown in fig. 7, control substrate move between the evaporation source of different materials with a certain speed, and arrange material of main part and
The evaporation rate of guest materials and ratio, thus complete linear doping, its uniformity is high, and repeatability is high.
It addition, the present invention also can use organic vapor phase deposition mode (OVPD) to be deposited on substrate by different materials, come real
Existing linear doping.Organic vapor phase deposition can also well overcome the defect of conventional thermal evaporation coating method, and is equally applicable to big
The volume production of size substrate.Doping ratio is controlled especially by regulation noble gas flow velocity.Its operation principle as shown in Figure 8, to chamber
Body is passed through noble gas, noble gas such as N2Flow through the crucible being loaded with different materials of heating and incidentally rise in corresponding crucible
Organic material, and then make organic material be transferred at substrate deposit, in deposition process, sedimentation rate can be easily
Regulated by flow controller, as long as therefore regulation noble gas flow velocity just can control doping ratio, it is easy to preparation is linear
Doping device.
The present invention also provides for a kind of organic electroluminescence device emitting layer material, and it uses doping method system as above
?.
The present invention also provides for the preparation method of a kind of organic electroluminescence device, and it includes step:
First substrate is carried out, carries out after cleaning drying up process, then heating, drying；
Device layers material and substrate are placed in cavity, to cavity evacuation；The emitting layer material of device includes two kinds of masters
Body material and a kind of guest materials；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
Complete linear doping.
Further, use linear evaporation mode to realize linear doping.
Or, use the mode of organic vapor phase deposition to be deposited on substrate by different materials, complete linear doping.
The present invention also provides for a kind of organic electroluminescence device, and it includes that preparation method as above is made.
Provide below a specific embodiment organic electroluminescence device preparation process of the present invention is specifically retouched
State.
First ito substrate is carried out ultrasonic cleaning process with glass cleaner, acetone and isopropanol the most respectively, each
The ultrasonic cleaning process time of step is 15 minutes, and ultrasonic cleaning uses deionized water rinsing ito substrate to remove residual after terminating
Solution, the rapidest high pure nitrogen dries up and continues heating, drying.
Then by layers of material, such as EIL(electron injecting layer), ETL(electron transfer layer), EML(luminescent layer) and, HTL(hole
Transport layer), HIL(hole injection layer) and negative electrode, and ito substrate is all placed in cavity, to cavity evacuation, until vacuum
Degree reduces to 5 × 10−6Below Torr can start evaporation, is not switched on cavity and carries out vacuum breaker action in preparation process.
The device architecture that the present embodiment is used, as it is shown in figure 9, particularly as follows: ITO/MoO3(1 nm)/mCP(50 nm)/
EML (20 nm)/TPBi (50 nm)/LiF (1 nm)/Al (100 nm).This device organic material energy diagram, such as Figure 10 institute
Showing, wherein TPBi/LiF is that electronics injects and transmission structure, and TPBi is as electron transfer layer, simultaneously as light emitting host material,
Hole transmission layer also using light emitting host material mCP to reduce the hole accummulation of interface, Ir (tfmppy)2(tpip) conduct
Light emitting guest material (i.e. dopant material), this light emitting guest material doping ratio in all EML is 10 wt%.The present invention
In doping content change schematic diagram in linear doped body tie structure as shown in figure 11, in preparation process, luminous in luminescent layer
The doping ratio of material of main part mCP:TPBi is 3:1 (8 nm)/1:1 (4 nm)/1:3 (8 nm), by light emitting host material
In the range of the evaporation rate of mCP and TPBi is arranged on 0.1 ~ 2/s, the evaporation rate such as mCP and TPBi can be respectively set to
(1.8/s:0.6/s)/(0.4/s:0.4/s)/(0.6/s:1.8/s), dopant material Ir (tfmppy)2(tpip) root
Arranging evaporation rate according to doping ratio 10wt% is 0.011-0.22/s(such as 0.1/s).The evaporation rate of metal electrode material
It is 5 ~ 10/s(such as 7/s).These evaporation rate can be monitored in real time according to quartz crystal.When employing is linearly deposited with,
Ito substrate translational speed may be provided at 2-10cm/s(such as 5cm/s) move between different evaporation sources；Using organic gas
When deposition is deposited with mutually, noble gas N used2Pressure can be 100Pa, and noble gas flow velocity may be configured as 0.1-1m/s(such as
0.5 m/s), thus drive organic material to deposit on an ito substrate.
In sum, the present invention uses the mode of linear doping to make emitting layer material, and the method for the present invention has all
The feature that even property is good and repeatability is high, utilizes this emitting layer material can improve the luminous efficiency of OLED of preparation, reduces
Efficiency roll-off and brightness decay, extend device lifetime, and device performance is greatly enhanced, and also can realize large-size device simultaneously
Volume production.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved according to the above description or to convert, all these modifications and variations all should belong to the guarantor of claims of the present invention
Protect scope.
Claims (10)
1. the doping method of an organic electroluminescence device emitting layer material, it is characterised in that include step:
The two of luminescent layer kinds of material of main parts and a kind of guest materials are placed in the cavity of evaporation, and will be used for depositing respectively
The substrate of layer material is placed in described cavity；
Then cavity is carried out evacuation process；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
To complete linear doping.
The doping method of organic electroluminescence device emitting layer material the most according to claim 1, it is characterised in that use
Linear evaporation mode realizes linear doping.
The doping method of organic electroluminescence device emitting layer material the most according to claim 2, it is characterised in that online
Property evaporation during, controlling described substrate moves between the evaporation source of different materials, completes linear doping.
The doping method of organic electroluminescence device emitting layer material the most according to claim 1, it is characterised in that use
Different materials is deposited on substrate by the mode of organic vapor phase deposition, completes linear doping.
The doping method of organic electroluminescence device emitting layer material the most according to claim 4, it is characterised in that to chamber
Body is passed through noble gas, and flows through the crucible being loaded with different materials, incidentally play corresponding crucible by described noble gas
In material, and then make each material be sent at substrate to deposit, in deposition process, control each by regulation noble gas flow velocity
The doping content of material.
6. an organic electroluminescence device emitting layer material, it is characterised in that use as described in any one of claim 1 ~ 5
Doping method prepares.
7. the preparation method of an organic electroluminescence device, it is characterised in that include step:
First substrate is carried out, carries out after cleaning drying up process, then heating, drying；
Device layers material and substrate are placed in cavity, to cavity evacuation；The emitting layer material of device includes two kinds of masters
Body material and a kind of guest materials；
Starting evaporation after being evacuated to predetermined vacuum degree again, during evaporation, the doping content arranging the two material of main part is divided
Increase the most continuously and be continuously reduced, described guest materials being set simultaneously and keeps constant relative to the doping content of luminescent layer total amount,
Complete linear doping.
The preparation method of organic electroluminescence device the most according to claim 7, it is characterised in that use the linearly side of evaporation
Formula realizes linear doping.
The preparation method of organic electroluminescence device the most according to claim 7, it is characterised in that use organic vapors to sink
Different materials is deposited on substrate by long-pending mode, completes linear doping.
10. an organic electroluminescence device, it is characterised in that include the preparation method as described in any one of claim 7 ~ 9
Make.
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| WO2021077486A1 (en) * | 2019-10-22 | 2021-04-29 | Tcl华星光电技术有限公司 | Oled display panel and display device |
| CN114318296A (en) * | 2022-02-17 | 2022-04-12 | 广东思泉新材料股份有限公司 | Vacuum coating equipment |
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Application publication date: 20160907 |