CN109119544A - A kind of perovskite electroluminescent device of novel light-emitting layer structure and preparation method thereof - Google Patents
A kind of perovskite electroluminescent device of novel light-emitting layer structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses perovskite electroluminescent devices of a kind of novel light-emitting layer structure and preparation method thereof, including transparent conductive substrate, hole transmission layer, perovskite luminescent layer, electron transfer layer and electrode, transparent conductive substrate and hole transmission layer connect, hole transmission layer and perovskite luminescent layer connect, perovskite luminescent layer and electron transfer layer connect, and the electrode setting is on the electron transport layer；Preparation method includes: the cleaning of transparent conductive substrate；The preparation of hole transmission layer；The preparation of perovskite luminescent layer；The preparation of electron transfer layer and electrode, a kind of perovskite electroluminescent device and preparation method thereof of novel light-emitting layer structure of the invention, it can effectively improve the surface quality of perovskite luminescent layer, reduce the generation of needle pore defect, reduce the probability of carrier non-radiative recombination, the problems such as traditional perovskite LED current density is low, leakage current is strong is effectively solved, to improve the brightness and luminous efficiency of device.
Description
Technical field
The present invention relates to light emitting device technologies fields, and in particular to a kind of perovskite electroluminescent of novel light-emitting layer structure
Device and preparation method thereof.
Background technique
It is ABX that perovskite for making light emitting diode, which is with general structure,3A kind of bipolar semiconductor material,
Have many advantages, such as that rich reserves, low in cost, absorption coefficient is high, emission spectrum is narrow, band gap is suitable, fluorescence lifetime is long, possesses good
Good luminescent properties, have obtained the extensive concern of people in the potential application of light emitting device field.The electroluminescent hair of perovskite
Optical diode (PeLED) has had reached what Organic Light Emitting Diode just reached in past 20 years in terms of brightness and efficiency
It is horizontal.In addition, the luminescent layer of PeLED is spin coating can to prepare at low temperature (less than 150 °C), this simple technique is greatly
Reduce the production cost of PeLED.
Common PeLED has the structure of " sandwich ", by positive and negative electrode, hole transmission layer, electron transfer layer and hair
Photosphere composition.Determine that the key factor of PeLED performance is the quality of luminescent layer.Light emitting layer thickness is usually arrived in tens nanometers
Between several microns, the luminous layer film of uniform, the continuous densification of formation thickness is very difficult under so microcosmic scale,
It often will appear serious needle pore defect (the existing cavity between perovskite crystal grain).Therefore, the equal of layer film that shine is improved
Even property and compactness reduce needle pore defect, for reducing short circuit current, improve brightness and luminous efficiency, have great importance.
In reported device architecture, researcher is prepared for gathering using the method for polymer and perovskite mixed dissolution
Conjunction object/perovskite hybrid illuminating layer (Li G, Tan Z K, Di D, et al. Nano Letters, 2015,15 (4):
2640.；Li J, Bade S G R, Shan X, et al. Advanced Materials, 2015, 27(35):
5196.), the presence of polymer limits the growth of perovskite, help to obtain crystallite dimension is small but what coverage rate was big shines
Layer helps to improve the consistency of film, to be promoted in addition, the presence of polymer can effectively reduce the generation of needle pore defect
The luminous efficiency of device.However the insulating properties of insulating polymer make its in perovskite is mixed be incorporated as luminescent layer when, charge
It injects area to reduce, is unfavorable for the raising of device current density, the current efficiency of device declines therewith；And conducting polymer is led
Electrically make its in perovskite is mixed be incorporated as luminescent layer when, charge easily passes through from conducting polymer, so that it is existing to generate electric leakage
As the current efficiency of device can also decline therewith.
Summary of the invention
In view of this, the present invention provides a kind of novel light-emitting layer structures to solve above-mentioned the problems of the prior art
Perovskite electroluminescent device and preparation method thereof can effectively improve the surface quality of perovskite luminescent layer, reduces pin hole and lacks
Sunken generation, reduces the probability of carrier non-radiative recombination, and effectively the traditional perovskite LED current density of solution is low, leakage current is strong
The problems such as, to improve the brightness and luminous efficiency of device.
To achieve the above object, technical scheme is as follows.
A kind of perovskite electroluminescent device of novel light-emitting layer structure, including transparent conductive substrate, hole transmission layer, calcium
Titanium ore luminescent layer, electron transfer layer and electrode, the transparent conductive substrate and hole transmission layer connect, the hole transport
Layer is connected with perovskite luminescent layer, and the perovskite luminescent layer and electron transfer layer connect, and the electrode setting exists
On electron transfer layer.
Further, the perovskite luminescent layer is the double-layer structure of insulating polymer and conducting polymer, with a thickness of 160
~220nm show that the insulating polymer and electron transfer layer connect by the preparation of two step solwution methods, with a thickness of 10~
20nm, the conducting polymer and hole transmission layer connect, with a thickness of 150~200nm.
Further, the transparent conductive substrate is ito glass or FTO Conducting Glass, with a thickness of 1~3mm, resistance
For 60~150 Ω.
Further, the material of the hole transmission layer be mass fraction 1.0%~1.3% PEDOT:PSS aqueous solution,
One or more of ZnO, PVK, PolyTPD, TAPC, TCTA, CuSCN or CuI.
Further, the electron transfer layer is TPBI, CBP or TmPyPB, with a thickness of 80~100nm；The electrode
Material be Al, LiF Al, LiF one or more of Ag, AgNW, In-Ga or carbon nanotube, with a thickness of 80~100nm.
A kind of preparation method of the perovskite electroluminescent device of novel light-emitting layer structure, comprising the following steps:
The cleaning of step 1, transparent conductive substrate: transparent conductive substrate is successively surpassed with toluene, isopropanol and dehydrated alcohol
Sound cleaning using the preceding dehydrated alcohol for wiping glass surface with non-dust cloth, and cleans 30~40min in UV light cleaning machine；
The preparation of step 2, hole transmission layer: hole transmission layer is prepared using spin-coating method, is then made annealing treatment；
The preparation of step 3, perovskite luminescent layer: by PbBr2Powder and insulating polymer mixed dissolution, stir evenly, are coated in
On hole transmission layer, then made annealing treatment；It again by MABr powder and conducting polymer mixed dissolution, stirs evenly, applies
Overlay on insulating polymer and PbBr2On mixed layer, then made annealing treatment；
The preparation of step 4, electron transfer layer and electrode: electron transfer layer and electricity are prepared on perovskite luminescent layer using vapour deposition method
Pole.
Further, the ultrasonic cleaning time in the step 1 is 15~20min, is put into dehydrated alcohol and protects after cleaning
It deposits.
Further, the conducting polymer and PbBr in the step 32Powder is dissolved among polar solvent, described to lead
Electric polymer is polyoxyethylene PEO, polyacrylonitrile (PAN) or polypyrrole PPY, and the polar solvent is dimethylformamide or diformazan
Base sulfoxide, concentration of the conducting polymer in polar solvent are 10~40mg/ml.
Further, the insulating polymer in the step 3 and MABr are dissolved among expense polar solvent, and the insulation is poly-
Conjunction object is that polyethylene glycol PEG, polystyrene PS, polyisoprene PIP or polyvinylidene fluoride PVDF, the non-polar solution are
Isopropanol, toluene acetone living, concentration of the insulating polymer in non-polar solution are 10~40mg/ml.
Further, the coating method in the step 3 is spin-coating method, knife coating or spray coating method.
Compared with the prior art, the invention has the advantages that and the utility model has the advantages that
(1) luminescent device of the invention brightness with higher, excitation purity and luminous efficiency have pole in illumination and display field
Big advantage.
(2) luminescent device of the invention is comprehensive solves traditional perovskite luminescent device charge injection efficiency low-leakage current
The problems such as strong.
Detailed description of the invention
Fig. 1 is a kind of perovskite EL device structure schematic diagram of novel light-emitting layer structure of the invention.
Fig. 2 is polyoxyethylene PEO and CH3NH3PbBr3Perovskite hybrid illuminating layer film surface structure chart.
Fig. 3 is polyoxyethylene PEO and CH3NH3PbBr3Perovskite electroluminescent device is electroluminescent when operating voltage is 4V
Luminescent spectrum figure.
Fig. 4 polyoxyethylene PEO and CH3NH3PbBr3The current -voltage curve figure of perovskite electroluminescent device.
Fig. 5 is a kind of perovskite electroluminescent device preparation flow figure of novel light-emitting layer structure of the invention.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with attached drawing and specific embodiment.It may be noted that
It is that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments, based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
As shown in Figure 1, a kind of structural schematic diagram of the perovskite electroluminescent device for novel light-emitting layer structure, including it is saturating
Bright conductive substrates 10, hole transmission layer 11, perovskite luminescent layer 12, electron transfer layer 13 and electrode 14, the electrically conducting transparent lining
Bottom 10 and hole transmission layer 11 connect, and the hole transmission layer 11 is connected with perovskite luminescent layer 12, the calcium titanium
Mine luminescent layer 12 and electron transfer layer 13 connect, and the electrode 14 is arranged on electron transfer layer 13.
Preferably, the perovskite luminescent layer 12 is the double-layer structure of insulating polymer and conducting polymer, with a thickness of 160
~220nm show that the insulating polymer and electron transfer layer 13 connect, with a thickness of 10 by the preparation of two step solwution methods
~20nm, the conducting polymer and hole transmission layer 11 connect, with a thickness of 150~200nm.
Preferably, the transparent conductive substrate 10 is ito glass or FTO Conducting Glass, with a thickness of 1~3mm, resistance
For 60~150 Ω.
Preferably, the material of the hole transmission layer 11 be mass fraction 1.0%~1.3% PEDOT:PSS aqueous solution,
One or more of ZnO, PVK, PolyTPD, TAPC, TCTA, CuSCN or CuI.
Preferably, the electron transfer layer 13 is TPBI, CBP or TmPyPB, with a thickness of 80~100nm；The electrode 14
Material be Al, LiF Al, LiF one or more of Ag, AgNW, In-Ga or carbon nanotube, with a thickness of 80~100nm.
As shown in figure 5, the flow chart of the preparation method for a kind of perovskite electroluminescent device of novel light-emitting layer structure,
The following steps are included:
The cleaning of step 1, transparent conductive substrate 10: to transparent conductive substrate 10 successively with toluene, isopropanol and dehydrated alcohol into
Row ultrasonic cleaning；
The preparation of step 2, hole transmission layer 11: hole transmission layer 11 is prepared using spin-coating method, is then made annealing treatment；
The preparation of step 3, perovskite luminescent layer 12: by PbBr2Powder and insulating polymer mixed dissolution, stir evenly, and coat
On hole transmission layer 11, then made annealing treatment；Again by MABr powder and conducting polymer mixed dissolution, stirring is equal
It is even, it is coated in insulating polymer and PbBr2On mixed layer, then made annealing treatment；
The preparation of step 4, electron transfer layer 13 and electrode 14: electron-transport is prepared on perovskite luminescent layer 12 using vapour deposition method
Layer 13 and electrode 14.
Preferably, the ultrasonic cleaning time in the step 1 is 15~20min, is put into dehydrated alcohol and saves after cleaning.
Preferably, the conducting polymer and PbBr in the step 32Powder is dissolved among polar solvent, the conduction
Polymer is polyoxyethylene PEO, polyacrylonitrile (PAN) or polypyrrole PPY, and the polar solvent is dimethylformamide or dimethyl
Sulfoxide, concentration of the conducting polymer in polar solvent are 10~40mg/ml.
Preferably, the insulating polymer in the step 3 and MABr are dissolved among expense polar solvent, the insulation polymerization
Object is polyethylene glycol PEG, polystyrene PS, polyisoprene PIP or polyvinylidene fluoride PVDF, and the non-polar solution is different
Propyl alcohol, toluene acetone living, concentration of the insulating polymer in non-polar solution are 10~40mg/ml.
Preferably, the coating method in the step 3 is spin-coating method, knife coating or spray coating method.
Embodiment 1
A kind of preparation method of the perovskite electroluminescent device of novel light-emitting layer structure, comprising the following steps:
(1) cleaning of transparent conductive substrate: successively using following solvents and time to the ito glass of commercialization 2 cm × 2 cm into
Row ultrasonic cleaning: toluene (15 min) → isopropanol (15 min) → dehydrated alcohol (15 min).
(2) preparation of hole transmission layer: hole transport layer material selects PEDOT:PSS aqueous solution, and suitable isopropyl is added
Alcohol adjusts viscosity (PEDOT:PSS: isopropanol=20:1), changes its adhesiveness, enhances quality of forming film.Using it is preceding with 0.22um or
The filtering head of 0.45um is filtered processing to mixed solution, filtered solution is spin-coated on ito glass, spin coating parameters are adopted
With dropwise addition at 1200 turns, 10 s of time；2000 turns of speed of prewhirling, continue 20 s；4000 turns of spin speed, continue 30 s.Spin coating
15 min are heated under 120 °C again afterwards to be made annealing treatment.
(3) preparation of perovskite luminescent layer: by the PbBr of 0.1757 g2The conducting polymer PEO of powder and 0.032 g are mixed
Conjunction is dissolved in 2ml dimethylformamide, and 12 h or more of magnetic agitation is then spin coated on hole transmission layer, spin coating parameters
Mixed solution is added dropwise when being 1200 turns, then reaches 3000 turns with 500 revs/min of acceleration, continues 50 s.It anneals later
Processing, in 75 °C of 10 min of heating.Again by the insulating polymer PEG mixed dissolution of the MABr powder of 0.0803 g and 0.032 g
In the isopropanol of 2 ml, 12 h or more of magnetic agitation.It is then spin coated onto conducting polymer PEO and PbBr2On mixed layer, rotation
It applies when parameter is 1200 turns and mixed solution is added dropwise, reach 3000 turns later with 500 revs/min of acceleration, continue 50 s.Finally exist
75 °C of 3 min of heating, are made annealing treatment.The surface texture figure of the luminous layer film of perovskite after annealing is as shown in Fig. 2.
(4) preparation of electron transfer layer and electrode: by electron transport layer materials TPBi vapor deposition on luminescent layer, thickness 80
nm；Electrode is LiF/Al, and preparation method is that first vapor deposition LiF is on TPBi layers, with a thickness of 1 nm, then be deposited the Al of 100 nm in
On LiF layers, with a thickness of 100 nm.
It is the green of 540 nm that the perovskite luminescent device of preparation, which issues dominant wavelength in the case where direct current power source voltage is 4 V,
Light, half-peak breadth are 20 nm, and the spectrogram for emitting light is as shown in Fig. 3.The current-voltage of device in normal operation is bent
Line is as shown in Fig. 4.
Above-mentioned preparation step is carried out with flow chart, as shown in Fig. 5.
Embodiment 2
A kind of preparation method of the perovskite electroluminescent device of novel light-emitting layer structure, comprising the following steps:
Preparation step is same as Example 1, is different in and insulating polymer by conducting polymer PEO replaces with conducting polymer
Object PAN.
Embodiment 3
A kind of preparation method of the perovskite electroluminescent device of novel light-emitting layer structure, comprising the following steps:
Preparation step is same as Example 1, be different in conducting polymer by insulating polymer PEG replace with insulation polymerize
Object PIP.
Embodiment 4
A kind of preparation method of the perovskite electroluminescent device of novel light-emitting layer structure, comprising the following steps:
Preparation step is same as Example 1, is different in using commercial transparent conducting glass FTO as transparent conductive substrate
10.FTO glass with a thickness of 2mm, resistivity is 2.7 × 10-3 ohmcm.
This embodiment is characterized in that reducing the system of prepared perovskite green light LED using FTO electro-conductive glass as substrate
Standby cost.
In conclusion a kind of perovskite electroluminescent device and preparation method thereof of novel light-emitting layer structure of the invention,
The surface quality that can effectively improve perovskite luminescent layer reduces the generation of needle pore defect, reduces carrier non-radiative recombination
Probability effectively solves the problems such as traditional perovskite LED current density is low, leakage current is strong, to improve the brightness of device and shine
Efficiency.
Claims (10)
1. a kind of perovskite electroluminescent device of novel light-emitting layer structure, it is characterised in that: successively include transparent from the bottom to top
Conductive substrates (10), hole transmission layer (11), perovskite luminescent layer (12), electron transfer layer (13) and electrode (14).
2. a kind of perovskite electroluminescent device of novel light-emitting layer structure according to claim 1, it is characterised in that: institute
Stating perovskite luminescent layer (12) is the double-layer structure with insulating polymer and conducting polymer, with a thickness of 160~220nm；Institute
It states insulating polymer and electron transfer layer (13) connects, with a thickness of 10~20nm, the conducting polymer and hole transport
Layer (11) connects, with a thickness of 150~200nm.
3. a kind of perovskite electroluminescent device of novel light-emitting layer structure according to claim 1, it is characterised in that: institute
Stating transparent conductive substrate (10) is ito glass or FTO Conducting Glass, and with a thickness of 1~3mm, resistance is 60~150 Ω.
4. a kind of perovskite electroluminescent device of novel light-emitting layer structure according to claim 1, it is characterised in that: institute
State hole transmission layer (11) material be the PEDOT:PSS aqueous solution of mass fraction 1.0%~1.3%, ZnO, PVK, PolyTPD,
One or more of TAPC, TCTA, CuSCN or CuI.
5. a kind of perovskite electroluminescent device of novel light-emitting layer structure according to claim 1, it is characterised in that: institute
Stating electron transfer layer (13) is TPBI, CBP or TmPyPB, with a thickness of 80~100nm；The material of the electrode (14) be Al,
LiF Al, LiF one or more of Ag, AgNW, In-Ga or carbon nanotube, with a thickness of 80~100nm.
6. preparing a kind of method of the perovskite electroluminescent device of novel light-emitting layer structure described in claim 1, feature exists
In, comprising the following steps:
The cleaning of step 1, transparent conductive substrate (10): toluene, isopropanol and anhydrous second are successively used to transparent conductive substrate (10)
Alcohol is cleaned by ultrasonic；
The preparation of step 2, hole transmission layer (11): hole transmission layer (11) are prepared using spin-coating method, are then made annealing treatment；
The preparation of step 3, perovskite luminescent layer (12): it is obtained by the preparation of two step solwution methods, by PbBr2Powder polymerize with insulation
Object mixed dissolution, stirs evenly, and is coated on hole transmission layer (11), is then made annealing treatment, annealing region is
60~80℃；It again by MABr powder and conducting polymer mixed dissolution, stirs evenly, is coated in insulating polymer and is mixed with PbBr2
It on layer, is then made annealing treatment, annealing region is 60 ~ 80 DEG C；
The preparation of step 4, electron transfer layer (13) and electrode (14): electricity is prepared on perovskite luminescent layer (12) using vapour deposition method
Sub- transport layer (13) and electrode (14).
7. a kind of method of the perovskite electroluminescent device according to claim 6 for preparing novel light-emitting layer structure,
Be characterized in that: the ultrasonic cleaning time in the step 1 is 15~20min, is put into dehydrated alcohol and saves after cleaning, before use
The dehydrated alcohol of glass surface is wiped with non-dust cloth, and 30~40min is cleaned in UV light cleaning machine.
8. a kind of method of the perovskite electroluminescent device according to claim 6 for preparing novel light-emitting layer structure,
It is characterized in that: conducting polymer and PbBr in the step 32Powder is dissolved among polar solvent, the conducting polymer
For polyoxyethylene PEO, polyacrylonitrile (PAN) or polypyrrole PPY, the polar solvent is dimethylformamide or dimethyl sulfoxide,
Concentration of the conducting polymer in polar solvent is 10~40mg/ml.
9. a kind of method of the perovskite electroluminescent device according to claim 6 for preparing novel light-emitting layer structure,
Be characterized in that: insulating polymer and MABr in the step 3 are dissolved among expense polar solvent, and the insulating polymer is poly-
Ethylene glycol PEG, polystyrene PS, polyisoprene PIP or polyvinylidene fluoride PVDF, the non-polar solution be isopropanol,
Toluene work acetone, concentration of the insulating polymer in non-polar solution are 10~40mg/ml.
10. a kind of method of the perovskite electroluminescent device according to claim 6 for preparing novel light-emitting layer structure,
Be characterized in that: the coating method in the step 3 is spin-coating method, knife coating or spray coating method.
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