CN107978688A - Electroluminescent LED and preparation method based on vulcanized lead cladding perovskite quantum dot - Google Patents
Electroluminescent LED and preparation method based on vulcanized lead cladding perovskite quantum dot Download PDFInfo
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Abstract
The present invention relates to a kind of electroluminescent LED and preparation method based on vulcanized lead cladding perovskite quantum dot.The electroluminescent LED includes：Ito glass is as bottom electrode；N-shaped ZnO/ polyethyleneimines are as electron transfer layer (ETL) and hole blocking layer (HBL)；PbS coats perovskite quantum dot as luminescent layer；P-type 4,4 ', 4 " three (9 base of carbazole) aniline film is as hole transmission layer (HTL) and electronic barrier layer (EBL)；MoO3/ Au is as top electrodes.Its preparation method includes：Prepare caesium oleic acid solutions first, after through prepare PbS cladding CsPbI3Quantum dot, electron transfer layer and hole blocking layer, luminescent layer, hole transmission layer and electronic barrier layer, obtain PbS cladding perovskite quanta point electroluminescents LED.The present invention coats perovskite quantum dot by using PbS, improves perovskite quantum dot light electrical property, while ensures its stability and keep its good semiconducting behavior, and the electroluminescent LED of efficient stable is prepared in this, as luminescent layer.
Description
Technical field
The present invention relates to a kind of preparation of new light emitting diode with quantum dots, and in particular to one kind is based on vulcanized lead (PbS)
The electroluminescent diode (Light-Emitting Diode, LED) and preparation method of perovskite quantum dot are coated, belongs to electroluminescent
Light emitting device field.
Background technology
In recent years, perovskite quantum dot is due to its unique optical property, such as high color purity, high-fluorescence quantum yield, face
The outstanding features such as color is adjustable, narrow emission peak, are with a wide range of applications in field of photoelectric devices such as light emitting diodes.But
Be, perovskite light emitting diode with quantum dots show two it is main the problem of：First, perovskite quantum dot is there is surface defect,
Cause the external quantum efficiency of the LED of preparation relatively low；Second, the aerial stability of perovskite quantum dot is poor, cause what is prepared
The stability of LED is to be improved.At present, mainly changed using processing methods such as the control of surface ligand concentration, interface engineerings with this
The performance of kind perovskite quanta point electroluminescent LED, makes its external quantum efficiency (EQE) bring up to 8-9% from less than 1%.However,
The problems such as these modes are usually reduced with the decline of quantum dot fluorescence quantum yield, stability, hinders theirs significantly
Practical application.On the other hand, people are using silica, polymer, polyhedral oligomeric silsesquioxane (polyhedral
Oligomeric silsesquioxane, POSS) cladding perovskite quantum dot, to improve its stability.However, these are handled
Method can damage the semiconducting behavior of perovskite quantum dot, make them be not suitable for preparing electroluminescent device.
To solve the above-mentioned problems, the present invention propose using PbS cladding perovskite quantum dot, be passivated its surface defect,
While improving optical property and ensure quantum dot stability, its semiconducting behavior is kept.PbS cladding perovskite quantum dots are made
The performances such as the electroluminescent LED prepared for luminescent layer, its external quantum efficiency and stability are significantly improved.Through searching, adopt
Improve its photoelectric properties and stability with PbS cladding perovskite quantum dots, and luminescent layer system is used as using this new quanta point material
Standby perovskite quanta point electroluminescent LED, not disclosed report.
The content of the invention
Existing in the prior art in order to solve the problems, such as, present invention proposition is a kind of to coat perovskite quantum dot based on vulcanized lead
Electroluminescent LED and preparation method.Perovskite quantum dot is coated by using PbS, improves perovskite quantum dot light electrical property, together
When ensure its stability and keep its good semiconducting behavior, and prepare in this, as luminescent layer the electroluminescent of efficient stable
LED。
The present invention uses following scheme, is described with reference to the drawings as follows：
A kind of electroluminescent LED based on vulcanized lead cladding perovskite quantum dot, is changed using PbS cladding perovskite quantum dots
It is apt to its photoelectric properties and stability, and perovskite quanta point electroluminescent LED is prepared using this quanta point material as luminescent layer；Institute
The structure of the perovskite quantum dot LED of PbS claddings is stated refering to shown in Fig. 1.Including：Ito glass is as bottom electrode；N-shaped ZnO/
Polyethyleneimine (C2H5N, Polyethylenimine, abbreviation PEI) it is used as electron transfer layer (ETL) and hole blocking layer
(HBL)；PbS coats perovskite quantum dot as luminescent layer；P-type 4,4 ', 4 "-three (carbazole -9- bases) aniline (C54H36N4, 4,4',
4 "-tris (carbazol-9-yl) triphenylamine, TCTA) film is as hole transmission layer (HTL) and electronic barrier layer
(EBL)；MoO3/ Au is as top electrodes.
A kind of preparation method based on PbS cladding perovskite quanta point electroluminescents LED, comprises the following steps that：
The first step, the CsPbI for preparing PbS claddings3Quantum dot；
Second step, successively carefully clean ITO electro-conductive glass with soap, deionized water, ethanol, chloroform, acetone, isopropanol,
And UV ozone processing is carried out, ITO is as bottom electrode；
3rd step, with 1000 turns per minute of rotating speed, ZnO quantum dot solution is spin-coated on ito glass, spin-coating time is
1 minute, then in atmosphere to anneal 10 minutes at a temperature of 150 DEG C；Above-mentioned film is transferred to N again2In glove box,
At a temperature of 110 DEG C, it is thin that PEI (being dissolved in 2-methyl cellosolve solution) is spin-coated on by ZnO with 3000 turns per minute of rotating speed
On film, the time is 10 minutes, and ZnO/PEI layers are used as electron transfer layer and hole blocking layer；
4th step, with 1000 turns per minute of speed, the PbS prepared is coated into CsPbI3Quantum dot is spin-coated on ZnO/
On PEI layers, spin-coating time is 1 minute, as luminescent layer；
5th step, by previous step obtain structure be transferred in vacuum chamber (vacuum be 1 × 10-7Torr), pass sequentially through
Thermal evaporation deposition TCTA, MoO3With Au film layers, wherein TCTA layers is used as hole transmission layer and electronic barrier layer, MoO3/ Au layers of work
For top electrodes；It is derived from PbS cladding perovskite quanta point electroluminescents LED.
The CsPbI of PbS claddings is prepared described in the first step3The method of quantum dot, comprises the following steps that：
Thioacetamide is added sulphur presoma is obtained in oleyl amine, by octadecane alkene and PbI2It is added in three-necked bottle, true
It is empty, at 120 DEG C degassing and it is dry 1 it is small when, at this temperature, dried oleic acid and sulphur presoma are injected into three-necked bottle
In, after solution is apparent from, temperature is increased to 160 DEG C, and injects caesium oleic acid solutions rapidly, after 5s, will be reacted using ice-water bath
Mixture is cooled to room temperature, and obtains the CsPbI of PbS claddings3Quantum dot.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention has been passivated the surface defect of perovskite quantum dot, has been significantly improved using PbS cladding perovskite quantum dots
The luminous efficiency and stability of quantum dot.The electroluminescent LED prepared using this quantum dot as luminescent layer, external quantum efficiency reach
11.1%, this is the perovskite quantum dot LED that performance is best so far.In addition, under conditions of unencapsulated, prepared by the present invention
The stability of PbS claddings perovskite quanta point electroluminescent LED significantly improve.
Brief description of the drawings
The structure chart of electroluminescent LED based on PbS cladding perovskite quantum dots in Fig. 1 present invention；
CsPbI in Fig. 2 present invention3Quantum dot and PbS claddings CsPbI3The absorption spectrum of quantum dot；
CsPbI in Fig. 3 present invention3Quantum dot and PbS claddings CsPbI3The photoluminescence spectra of quantum dot；
CsPbI in Fig. 4 present invention3Quantum dot and PbS claddings CsPbI3The time resolution photoluminescence spectra figure of quantum dot；
PbS coats CsPbI in Fig. 5 present invention3The images of transmissive electron microscope (a) and high resolution transmission electron microscopy of quantum dot
Image (b)；
PbS coats the level-density parameter structure of each functional layer in perovskite quantum dot LED in Fig. 6 present invention；
PbS coats CsPbI in Fig. 7 present invention3Current density-voltage-brightness (J-V-L) curve map of quantum dot LED, is inserted
Figure is the photo of LED component；
PbS coats CsPbI in Fig. 8 present invention3The external quantum efficiency of quantum dot LED, luminous efficiency, current efficiency respectively with
Graph of a relation between brightness；
PbS coats CsPbI in Fig. 9 present invention3The photoluminescence spectra and electroluminescent spectrum of quantum dot LED；
PbS coats CsPbI in Figure 10 present invention3Quantum dot stores the absorption spectrum after 20 days in atmosphere；
PbS coats CsPbI in Figure 11 present invention3Quantum dot stores the photoluminescence spectra after 20 days in atmosphere；
PbS coats CsPbI in Figure 12 present invention3Quantum dot film stores the X-ray diffraction after 33 days at ambient temperature
Collection of illustrative plates；
CsPbI in Figure 13 present invention3Quantum dot LED and PbS coat CsPbI3Quantum dot LED electroluminescent intensity and storage
The graph of a relation of time, illustration are shown in CsPbI under the identical voltage of 2.5V3Quantum dot LED and PbS coat CsPbI3Quantum dot LED
Electroluminescent intensity and the relation curve of lighting time.
Embodiment
The particular content and embodiment of the present invention is further illustrated with reference to example：
1st, CsPbI is coated based on PbS3The preparation scheme of quanta point electroluminescent LED is as follows, but protection scope of the present invention
It is not limited to following embodiments.
The first step, prepare PbS claddings CsPbI3Quantum dot, step are as follows：
Caesium oleic acid solutions are prepared first：By cesium carbonate Cs2CO3(0.814 gram), oleic acid OA (2.5mL), and octadecane alkene ODE
(30mL) is put into the three-necked bottle of 100mL, in 120 DEG C of deaerated under vacuum and small drying 1.Then in N2It is middle to add mixture
Heat is to 150 DEG C, until obtaining clearly solution.
Secondly PbS claddings CsPbI is prepared3Quantum dot：0.0028g thioacetamides are added in 1mL oleyl amines OLA, as
The presoma (S-OLA) of sulphur.By 10mL ODE and 0.168g PbI2It is added in 50mL three-necked bottles, deaerates at vacuum, 120 DEG C
With dry 1 it is small when.At this temperature, dried 1mL OA and 1mL S-OLA is injected into three-necked bottle.Solution becomes clear
After clear, temperature is increased to 160 DEG C, and injects 1mL caesium oleic acid solutions rapidly.After 5s, reaction mixture is cooled down using ice-water bath
To room temperature.
Second step, successively carefully clean ITO electro-conductive glass with soap, deionized water, ethanol, chloroform, acetone, isopropanol,
And carry out UV ozone and handle 15 minutes.
3rd step, on ito glass by ZnO quantum dot solution with 1000 turns per minute of rotating speed spin coating 1 minute, and in sky
Anneal 10 minutes at a temperature of 150 DEG C in gas；Then substrate is transferred to N2In glove box.By PEI (dissolvings on ZnO film
In 2-methyl cellosolve solution) spin coating with 3000 turns per minute of rotating speed, 110 DEG C at a temperature of spin coating 10 minutes, ZnO/PEI
Layer is used as electron transfer layer and hole blocking layer；
4th step, with 1000 turns per minute of speed, the PbS prepared is coated into CsPbI3Quantum dot is spin-coated on ZnO/
On PEI layers, as luminescent layer；
5th step, will previous step obtain object on be transferred in vacuum chamber (vacuum be 1 × 10-7Torr), heat is passed through
Evaporation is sequentially depositing TCTA, MoO3With Au layers, wherein TCTA layers is used as hole transmission layer and electronic barrier layer, MoO3/ Au layers of conduct
Top electrodes；It is derived from PbS cladding perovskite quanta point electroluminescents LED.
2nd, experiment and test result
In order to verify the performance of electroluminescent LED of the present invention based on PbS cladding perovskite quantum dots, the present invention carries out
Test below：
(1) as shown in figure 4, the present invention is to CsPbI3Quantum dot and PbS claddings CsPbI3The time resolved spectroscopy of quantum dot
(TRPL) contrast test is carried out.We are it can be found that quantum dot average life span increases to 23.1ns from 21.1ns, in addition, PbS bags
Cover CsPbI3The photoluminescence spectra of quantum dot narrows, fluorescence quantum yield increase, it was demonstrated that CsPbI3The surface defect of quantum dot is
Successfully it is passivated.
(2) as shown in Figure 7, Figure 8, under 2.8V voltages, PbS claddings CsPbI3The external quantum efficiency of quantum dot LED reaches
11.1%, this is the peak that perovskite quantum dot LED is reported at present.Peak point current efficiency (the η of deviceA) and luminous efficiency
(ηL) it is respectively 0.93cd/A and 0.76lm/W.It is indicated above that same CsPbI3Quanta point electroluminescent LED compares, PbS claddings
CsPbI3Quanta point electroluminescent LED has good performance.
(3) as shown in Figure 10, Figure 11, after placing 3 days in atmosphere, CsPbI3Quantum dot solution color is become by peony
Yellow, stability are poor.In contrast, PbS coats CsPbI3The color keep of quantum dot solution is constant (peony)；Putting
After putting 20 days, PbS claddings CsPbI3The absorption of quantum dot solution and photoluminescence spectra only have slight red shift, show PbS bags
Cover CsPbI3Quantum dot solution stability significantly improves.In addition, as shown in figure 12, PbS claddings CsPbI3The X of quantum dot film is penetrated
Ray diffraction diagram picture shows, after storing 33 days at ambient temperature, PbS claddings CsPbI3Quantum dot keeps Emission in Cubic, and crystalline phase is stablized
Property be improved significantly.
(4) CsPbI is coated to storing unencapsulated PbS3Quantum dot LED stability is tested, as shown in figure 13.Storing
After hiding 35 days, PbS claddings CsPbI3Quantum dot LED electroluminescent luminous intensities have almost no change, and CsPbI3Quantum dot is electroluminescent
Emitting led luminous intensity have dropped 30-40% after 3 days.Under 2.5V voltages, after 600s is lighted, CsPbI3Quantum dot
LED electroluminescent intensity drops to the 48% of initial value, and PbS coats CsPbI3Quantum dot LED electroluminescent intensity is without obvious drop
It is low.It is indicated above that PbS coats CsPbI3The stability of quanta point electroluminescent LED is improved significantly.To sum up, we have been
Show, in CsPbI3Quantum dot outer cladding PbS shells, can be passivated CsPbI3The surface defect of quantum dot, improves its optical property
And stability.CsPbI is coated by PbS3Electroluminescent LED prepared by quantum dot, its external quantum efficiency reach 11.1%, and performance obtains
To raising；Meanwhile stability also has clear improvement.It is noted that it can also be answered using the PbS perovskite quantum dots coated
For other devices, such as solar cell, photodetector and laser.
Claims (3)
- A kind of 1. electroluminescent LED based on vulcanized lead cladding perovskite quantum dot, it is characterised in that：Its photoelectric properties and stability are improved using PbS cladding perovskite quantum dots, and luminescent layer is used as using this quanta point material Prepare perovskite quanta point electroluminescent LED；The structure of the perovskite quantum dot LED of the PbS claddings includes：Ito glass is made For bottom electrode；N-shaped ZnO/ polyethyleneimines are as electron transfer layer and hole blocking layer；The perovskite quantum dot of PbS claddings As luminescent layer；P-type 4,4 ', 4 "-three (carbazole -9- bases) aniline film is as hole transmission layer and electronic barrier layer；MoO3/Au As top electrodes.
- 2. a kind of preparation method based on vulcanized lead cladding perovskite quanta point electroluminescent LED as claimed in claim 1, tool Body step is as follows：The first step, the CsPbI for preparing PbS claddings3Quantum dot；Second step, successively carefully clean ITO electro-conductive glass with soap, deionized water, ethanol, chloroform, acetone, isopropanol, goes forward side by side The processing of row UV ozone, ITO is as bottom electrode；3rd step, with 1000 turns per minute of rotating speed, ZnO quantum dot solution is spin-coated on ito glass, spin-coating time is 1 point Clock, then in atmosphere with 150 DEG C of annealing temperature 10 minutes；Above-mentioned film is transferred to N again2In glove box, at 110 DEG C At a temperature of, it is spin-coated on the PEI that 3000 turns per minute of rotating speed is dissolved in 2-methyl cellosolve solution on ZnO film, when Between be 10 minutes, ZnO/PEI layers are used as electron transfer layer and hole blocking layer；4th step, with 1000 turns per minute of speed, the PbS prepared is coated into CsPbI3Quantum dot is spin-coated on ZnO/PEI layers On, spin-coating time is 1 minute, as luminescent layer；5th step, by the structure that previous step obtains be transferred to vacuum as 1 × 10-7In the vacuum chamber of torr, hot steaming is passed sequentially through Hair deposition TCTA, MoO3With Au film layers, wherein TCTA layers is used as hole transmission layer and electronic barrier layer, MoO3/ Au layers as top Portion's electrode；It is derived from PbS cladding perovskite quanta point electroluminescents LED.
- 3. a kind of preparation method based on vulcanized lead cladding perovskite quanta point electroluminescent LED as claimed in claim 2, it is special Sign is：The CsPbI of PbS claddings is prepared described in the first step3The method of quantum dot, comprises the following steps that：Thioacetamide is added sulphur presoma is obtained in oleyl amine, by octadecane alkene and PbI2It is added in three-necked bottle, in vacuum, 120 Deaerate at DEG C and it is dry 1 it is small when, at this temperature, dried oleic acid and sulphur presoma are injected into three-necked bottle, solution After being apparent from, temperature is increased to 160 DEG C, and injects caesium oleic acid solutions rapidly, using ice-water bath that reaction mixture is cold after 5s But to room temperature, the CsPbI that PbS is coated is obtained3Quantum dot.
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| CN108832012A (en) * | 2018-06-19 | 2018-11-16 | 吉林大学 | A kind of the perovskite quantum dot LED and preparation method of spontaneity Ag doping and passivation |
| CN108832010A (en) * | 2018-05-29 | 2018-11-16 | 合肥工业大学 | A kind of perovskite light emitting diode and preparation method thereof of ionic liquid as electric charge injection layer |
| CN109256494A (en) * | 2018-09-10 | 2019-01-22 | 吉林大学 | SrCl2Perovskite quantum dot High Efficiency Luminescence LED of doping and preparation method thereof |
| CN110963711A (en) * | 2019-12-13 | 2020-04-07 | 深圳第三代半导体研究院 | Composite quantum dot glass and preparation method thereof |
| CN111433321A (en) * | 2018-05-17 | 2020-07-17 | 李良 | Metal ion pair compound coated quantum dot and preparation method thereof |
| WO2021010897A1 (en) * | 2019-07-15 | 2021-01-21 | National University Of Singapore | Near infra-red light emitting diodes |
| CN114420856A (en) * | 2022-01-21 | 2022-04-29 | 吉林大学 | Ethyl cellulose enhanced CsPbI3Method for stabilizing and flexibility of quantum dot film |
| CN115093845A (en) * | 2022-06-22 | 2022-09-23 | 吉林大学 | Conductive perovskite core-shell quantum dot and synthesis method thereof |
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| CN109256494A (en) * | 2018-09-10 | 2019-01-22 | 吉林大学 | SrCl2Perovskite quantum dot High Efficiency Luminescence LED of doping and preparation method thereof |
| WO2021010897A1 (en) * | 2019-07-15 | 2021-01-21 | National University Of Singapore | Near infra-red light emitting diodes |
| CN110963711A (en) * | 2019-12-13 | 2020-04-07 | 深圳第三代半导体研究院 | Composite quantum dot glass and preparation method thereof |
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| CN114420856A (en) * | 2022-01-21 | 2022-04-29 | 吉林大学 | Ethyl cellulose enhanced CsPbI3Method for stabilizing and flexibility of quantum dot film |
| CN115093845A (en) * | 2022-06-22 | 2022-09-23 | 吉林大学 | Conductive perovskite core-shell quantum dot and synthesis method thereof |
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