CN110311060A - A kind of perovskite LED component and its preparation method for inhibiting crystalline size - Google Patents
A kind of perovskite LED component and its preparation method for inhibiting crystalline size Download PDFInfo
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- CN110311060A CN110311060A CN201910717228.5A CN201910717228A CN110311060A CN 110311060 A CN110311060 A CN 110311060A CN 201910717228 A CN201910717228 A CN 201910717228A CN 110311060 A CN110311060 A CN 110311060A
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- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
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Abstract
The present invention provides a kind of perovskite LED component and its preparation methods of inhibition crystalline size, are related to technical field of semiconductor luminescence.It includes that hole injection layer, hole transmission layer, perovskite luminescent layer, electron transfer layer and second electrode are sequentially depositing in the substrate for be provided with first electrode that perovskite LED component, which inhibits the preparation method of crystalline size,;Wherein, the perovskite luminescent layer is by including that the mixed solution film forming of perovskite precursor solution and polyethylene glycol oxide is made.Perovskite LED component and its preparation method of inhibition crystalline size can significantly inhibit the size of perovskite crystal grain, form nanoscale grain size, improve the performance of perovskite LED component.
Description
Technical field
The present invention relates to technical field of semiconductor luminescence, in particular to a kind of perovskite LED component and its suppression
The preparation method of crystalline size processed.
Background technique
Currently, perovskite light emitting diode (English abbreviation: " PeLED ") is a kind of very potential two pole of novel light-emitting
Pipe.Because perovskite material has, synthesis is simple, the narrow range of glow peak, forbidden bandwidth is adjustable, photoluminescence quantum yield
High, the advantages that colour purity is high, so that it has huge application potential on luminescent device.
But perovskite is easy to crystallization, with the increase of perovskite crystal particle, photovoltaic performance can enhance, and shine
Diode behavior can decrease up to decrease.
Therefore, how to inhibit the size of perovskite crystal to increase, prepare urgent need to resolve in perovskite LED component method
Technical problem.
Summary of the invention
The purpose of the present invention is to provide a kind of perovskite LED component and its preparation method of inhibition crystalline size, energy
The size of perovskite crystal grain is enough significantly inhibited, nanoscale grain size is formed, improves the performance of perovskite LED component.
The present invention provides a kind of technical solution:
A kind of perovskite LED component inhibits the preparation method of crystalline size, comprising:
Hole injection layer, hole transmission layer, perovskite luminescent layer, electricity are sequentially depositing in the substrate for be provided with first electrode
Sub- transport layer and second electrode;
Wherein, the perovskite luminescent layer is by including that the mixed solution of perovskite precursor solution and polyethylene glycol oxide forms a film
It is made.
Further, in the mixed solution, the mass ratio of the polyethylene glycol oxide and the perovskite precursor solution
Less than or equal to 1.5%.
Further, described that hole injection layer, hole transmission layer, calcium are sequentially depositing in the substrate for be provided with first electrode
Before titanium ore luminescent layer, electron transfer layer and second electrode, comprising:
Substrate is put in toluene, acetone and ethanol solution and is respectively cleaned by ultrasonic.
Further, described that hole injection layer, hole transmission layer, calcium are sequentially depositing in the substrate for be provided with first electrode
Titanium ore luminescent layer, electron transfer layer and second electrode, comprising:
The first electrode is made by thermal evaporation combination mask plate deposition on the substrate.
Further, described that hole injection layer, hole transmission layer, calcium are sequentially depositing in the substrate for be provided with first electrode
Titanium ore luminescent layer, electron transfer layer and second electrode, comprising:
The hole is made by Vacuum Coating method, magnetron sputtering method or low temperature solution polycondensation on the first electrode to inject
Layer.
Further, the hole injection layer uses inorganic MO3-x、V2O5-x、NiO1-xSemiconductor material or organic hole pass
Defeated material is made.
Further, described that hole injection layer, hole transmission layer, calcium are sequentially depositing in the substrate for be provided with first electrode
Titanium ore luminescent layer, electron transfer layer and second electrode, comprising:
The hole transmission layer is made by electron beam evaporation method, Vacuum Coating method deposition on the hole injection layer.
Further, the material of the hole transmission layer is selected from nickel oxide nanoparticle, molybdenum oxide nanoparticles or oxidation
Tungsten nano particle.
Further, the forming direction of the electron transfer layer is contrary with the forming of the hole transmission layer.
Second of technical solution provided by the invention:
A kind of perovskite LED component includes substrate, hole injection layer, the hole transport being cascading on lower
Layer, perovskite luminescent layer, electron transfer layer and second electrode, wherein the perovskite luminescent layer is by including perovskite presoma
The mixed solution of solution and polyethylene glycol oxide film forming is made.
Perovskite LED component provided by the invention and its beneficial effect for inhibiting the preparation method of crystalline size are:
Compared to perovskite precursor solution direct formation of film at surface is used merely, perovskite luminescent layer is formed, is used in the present embodiment
Perovskite luminescent layer is made in the mixed solution of perovskite precursor solution and polyethylene glycol oxide film forming, can significantly inhibit perovskite
The size of crystal grain forms nanoscale grain size, improves the performance of perovskite LED component.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the structural schematic diagram of perovskite LED component provided in an embodiment of the present invention.
Fig. 2 is the flow chart for the preparation method that perovskite LED component provided in an embodiment of the present invention inhibits crystalline size.
Icon: 100- perovskite LED component;110- substrate;120- first electrode;130- hole injection layer;The hole 140-
Transport layer;150- perovskite luminescent layer;160- electron transfer layer;170- second electrode.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.
Therefore, the detailed description of the embodiment of the present invention provided in the accompanying drawings is not intended to limit below claimed
The scope of the present invention, but be merely representative of selected embodiment of the invention.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
It should also be noted that similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, does not then need that it is further defined and explained in subsequent attached drawing.
In the description of the present invention, it is to be understood that, term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, or be somebody's turn to do
Invention product using when the orientation or positional relationship usually put or those skilled in the art orientation or position that usually understand
Relationship is set, is merely for convenience of description of the present invention and simplification of the description, rather than the equipment of indication or suggestion meaning or element are necessary
It with specific orientation, is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be fixedly connected, may be a detachable connection or one
Connect to body;It can be mechanical connection, be also possible to be electrically connected;It can be directly connected, it can also be indirect by intermediary
It is connected, can be the connection inside two elements.For the ordinary skill in the art, on being understood with concrete condition
State the concrete meaning of term in the present invention.
Referring to Fig. 1, present embodiments providing a kind of perovskite LED component 100, perovskite LED component 100 includes under
On be cascading substrate 110, hole injection layer 130, hole transmission layer 140, perovskite luminescent layer 150, electronics pass
Defeated layer 160 and second electrode 170, wherein perovskite luminescent layer 150 is by including perovskite precursor solution and polyethylene glycol oxide
(PEO) mixed solution film forming is made.
By mixing perovskite precursor solution with polyethylene glycol oxide (PEO), mixed solution, preparation film forming are formed.This
There is the polymer P EO of three-dimensional interconnection in perovskite luminescent layer 150, can inhibit the presence of bulky grain crystal grain in sample, formed uniform
Little particle crystal grain, improve perovskite LED component 100 performance.
Referring to Fig. 2, the present embodiment also provides the preparation method that perovskite LED component inhibits crystalline size, comprising:
S1: preparation substrate 110
Substrate 110 can be made of aluminium oxide, and be polished to the two-sided of substrate 110.Substrate 110 is cleaned again, into
Row chemical cleaning step are as follows: substrate 110 is put in toluene, acetone and ethanol solution and is respectively cleaned by ultrasonic 10 minutes, recycling one
It is secondary;It is spare after high pure nitrogen dries up after using deionized water repeated flushing clean later.
As a kind of optional embodiment, its chemistry can be carved using the FTO glass of electrically conducting transparent as substrate 110
Erosion carries out chemical cleaning, specific cleaning step again are as follows: the area of FTO electro-conductive glass front unilateral side 3/4 is hidden using 3M adhesive tape,
Then a thin layer zinc slurry (the wet water stirring of zinc powder) is smeared on remaining 1/4 area.After zinc slurry is dry, electro-conductive glass is put into
Carry out chemical attack in the HC1 solution of 0.4mo1/L, after about 3min, reaction stops that there is no bubble formations, and electro-conductive glass is taken
Out, remaining zinc powder is cleaned with flowing water, removes 3M adhesive tape.Then the electro-conductive glass etched is put into acetone and is cleaned by ultrasonic
It takes out after l0min, is successively gently wiped with the swab stick for being moistened with acetone, remove the macroscopic impurity in surface.Finally successively going
Respectively it is cleaned by ultrasonic 5min~l0min in ionized water, acetone and isopropanol, is cleaned with deionized water, is dried with nitrogen stand-by.
S2: first electrode 120 is deposited in substrate 110
First electrode 120 is made of metal material, and first electrode 120 serves as anode electrode.First electrode 120 can lead to
Thermal evaporation combination mask plate deposition is crossed to be made.First electrode 120 is connected by conducting wire with the anode of power supply.
S3: the deposition of hole implanted layer 130 in first electrode 120
Hole injection layer 130 can use inorganic MO3-x、V2O5-x、NiO1-xEqual semiconductor materials or organic hole transmit material
Material is made.The preparation of hole injection layer 130 uses magnetron sputtering method, Vacuum Coating method or low temperature solution polycondensation, using magnetron sputtering
Sputter temperature when method is 80 DEG C~120 DEG C, specific steps are as follows:
NiO ceramic target is installed, the position between target and substrate is adjusted to 8 centimetres;Mechanical pump is opened, to sputter chamber
It vacuumizes, after chamber vacuum degree is lower than 10 Pascal, opens molecular pump and continue to vacuumize, until chamber vacuum degree is lower than 3.0*
10-3Pascal;Suitable high-purity hydrogen and oxygen are passed through into cavity, the flow proportional both adjusted to 5:1, so that cavity
Pressure is stablized in 1.0 Pascals;Radio frequency source is opened, is 130 watts by its power setting, and 110 temperature of substrate is set as 120
DEG C, sputtering time is set as 0.5 hour.
As a kind of optional embodiment, hole injection layer 130 can be made of MEH-PPV material, using 4000 turns
Spin coating 60 seconds, thickness was placed in 120 DEG C of thermal station and anneals 20 minutes in 10nm-40nm or so.
S4: the deposition of hole transport layer 140 on hole injection layer 130
Hole transmission layer 140 can be p-type structure.The material of hole transmission layer 140 is selected from nickel oxide nanoparticle, oxidation
Molybdenum nano particle or tungsten oxide nanoparticles.Hole transmission layer 140 can be deposited by electron beam evaporation method and is made.
S5: perovskite luminescent layer 150 is deposited on hole transmission layer 140
The preparation of perovskite luminescent layer 150, first by CH3NH3Br and PbBr2It is molten that powder mixing is dissolved in dimethylformamide
It in liquid, is stirred under the conditions of 70 DEG C with magnetic stirring apparatus, forms perovskite precursor solution;Then calcium is added in polyethylene glycol oxide
In titanium ore precursor solution, mixed solution is formed.In mixed solution, the mass ratio of polyethylene glycol oxide and perovskite precursor solution
Less than or equal to 1.5%.In such manner, it is possible to guarantee that polyethylene glycol oxide is dissolved completely in perovskite precursor solution.
The mode of the mixed solution prepared spin coating is uniformly spin-coated on hole transmission layer 140, spincoating conditions are
4000 rpms, the time is 30 seconds, is finally made annealing treatment in glove box to the sample after spin coating, annealing temperature 80
DEG C, the time is 20 minutes.
Perovskite material (CH in perovskite luminescent layer 1503NH3PbBr3) there is direct band gap, high internal quantum efficiency, hair
The advantages that spectrum line is narrow, preparation cost is low, compatible with flexible substrates 110.
S6: electron transfer layer 160 is deposited on perovskite luminescent layer 150
Electron transfer layer 160 can be N-shaped structure.It the forming direction of electron transfer layer 160 can be with hole transmission layer 140
Forming it is contrary.The material of electron transfer layer 160 is selected from Zinc oxide nanoparticle, Titanium dioxide nanoparticle or oxidation sijna
Rice grain.
S7: second electrode 170 is deposited on electron transfer layer 160
Second electrode 170 is made of transparent material, can tin oxide or graphene selected from tin indium oxide, fluorine doped.The
Two electrodes 170 can be deposited by electron beam evaporation method and are made, and second electrode 170 serves as second electrode.Simultaneously using thermal evaporation
Second electrode 170 is deposited on electron transfer layer 160 in conjunction with mask plate.Second electrode 170 is connected by conducting wire with power cathode.
Perovskite LED component 100 provided in this embodiment and its beneficial effect for inhibiting the preparation method of crystalline size are:
Compared to perovskite precursor solution direct formation of film at surface is used merely, perovskite luminescent layer 150 is formed, is adopted in the present embodiment
Perovskite luminescent layer 150 is made with the mixed solution of perovskite precursor solution and polyethylene glycol oxide film forming, can significantly inhibit
The size of perovskite crystal grain forms nanoscale grain size, improves the performance of perovskite LED component 100.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. the preparation method that a kind of perovskite LED component inhibits crystalline size characterized by comprising
Hole injection layer (130), hole transmission layer are sequentially depositing in the substrate (110) for being provided with first electrode (120)
(140), perovskite luminescent layer (150), electron transfer layer (160) and second electrode (170);
Wherein, the perovskite luminescent layer (150) by include perovskite precursor solution and polyethylene glycol oxide mixed solution at
Film is made.
2. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
In mixed solution, the mass ratio of the polyethylene glycol oxide and the perovskite precursor solution is less than or equal to 1.5%.
3. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
Hole injection layer (130), hole transmission layer (140), calcium are sequentially depositing in the substrate (110) for being provided with first electrode (120)
Before titanium ore luminescent layer (150), electron transfer layer (160) and second electrode (170), comprising:
Substrate (110) is put in toluene, acetone and ethanol solution and is respectively cleaned by ultrasonic.
4. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
Hole injection layer (130), hole transmission layer (140), calcium are sequentially depositing in the substrate (110) for being provided with first electrode (120)
Titanium ore luminescent layer (150), electron transfer layer (160) and second electrode (170), comprising:
The first electrode (120) are made by thermal evaporation combination mask plate deposition on the substrate (110).
5. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
Hole injection layer (130), hole transmission layer (140), calcium are sequentially depositing in the substrate (110) for being provided with first electrode (120)
Titanium ore luminescent layer (150), electron transfer layer (160) and second electrode (170), comprising:
The hole is made by Vacuum Coating method, magnetron sputtering method or low temperature solution polycondensation on the first electrode (120) to infuse
Enter layer (130).
6. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
Hole injection layer (130) uses inorganic MO3-x、V2O5-x、NiO1-xSemiconductor material or organic hole transport material are made.
7. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
Hole injection layer (130), hole transmission layer (140), calcium are sequentially depositing in the substrate (110) for being provided with first electrode (120)
Titanium ore luminescent layer (150), electron transfer layer (160) and second electrode (170), comprising:
The hole transmission layer is made by electron beam evaporation method, Vacuum Coating method deposition on the hole injection layer (130)
(140)。
8. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
The material of hole transmission layer (140) is selected from nickel oxide nanoparticle, molybdenum oxide nanoparticles or tungsten oxide nanoparticles.
9. the preparation method that perovskite LED component according to claim 1 inhibits crystalline size, which is characterized in that described
The forming direction of electron transfer layer (160) is contrary with the forming of the hole transmission layer (140).
10. a kind of perovskite LED component, which is characterized in that including be cascading on lower substrate (110), hole
Implanted layer (130), hole transmission layer (140), perovskite luminescent layer (150), electron transfer layer (160) and second electrode (170),
Wherein, the perovskite luminescent layer (150) is by including that the mixed solution film forming of perovskite precursor solution and polyethylene glycol oxide is made
At.
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