CN114591739A - Preparation method of perovskite quantum dot doped with metal sodium ions, product and application thereof - Google Patents

Preparation method of perovskite quantum dot doped with metal sodium ions, product and application thereof Download PDF

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CN114591739A
CN114591739A CN202210223839.6A CN202210223839A CN114591739A CN 114591739 A CN114591739 A CN 114591739A CN 202210223839 A CN202210223839 A CN 202210223839A CN 114591739 A CN114591739 A CN 114591739A
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precursor
quantum dot
perovskite quantum
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黄义
唐鹏飞
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Chongqing University of Post and Telecommunications
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • C09K11/664—Halogenides
    • C09K11/665—Halogenides with alkali or alkaline earth metals
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    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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Abstract

The invention relates to a preparation method of a perovskite quantum dot doped with metal sodium ions, a product and application thereof, belonging to the technical field of preparation of perovskite quantum dots. The invention discloses a preparation method of a perovskite quantum dot doped with metal sodium ions, which mainly comprises the steps of preparing a lead bromide precursor, an oil cesium-sodium precursor and FA+The precursor and the didecyl dimethyl ammonium bromide are mixed to prepare the perovskite quantum dot (Na: CsPbBr) doped with the metal sodium ions3). The preparation method is simple and controllable, and the prepared perovskite quantum dot (Na: CsPbBr) doped with metal sodium ions3) The optical material has good optical performance, higher photoluminescence efficiency and fewer defect states; has good application effect in the aspect of preparing the luminescent layer of the LED device and can enhance the LED devicePerformance, and external quantum efficiency of the LED device.

Description

Preparation method of perovskite quantum dot doped with metal sodium ions, product and application thereof
Technical Field
The invention belongs to the technical field of perovskite quantum dot preparation, and relates to a preparation method of a perovskite quantum dot doped with metal sodium ions, and a product and application thereof.
Background
In recent years, lead perovskite halide is becoming a popular semiconductor in the field of optoelectronics due to its excellent optoelectronic properties, i.e., high photoluminescence quantum yield, narrow emission peak, tunable band gap, efficient charge generation and broad band absorption. However, defect states in perovskite quantum dots have been a major factor hindering their practical application.
Currently, ion doping or surface modification is considered as the main method to solve the defect state in quantum dots. In recent years, some research has focused on CsPbX3Pb in Quantum dots2+And (4) replacement of the position. By means of metal ions (e.g. Zn)2+,Cd2+,Mn2+,Sn2+Etc.) substituted CsPbX3Pb in Quantum dots2+Thus preparing the metal ion doped CsPbBr with low defect density and high performance3And (4) quantum dots.
Thus, a metal sodium ion (Na) can be studied+) The method for doping perovskite quantum dots synthesizes the sodium ion doped perovskite quantum dots.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a perovskite quantum dot doped with sodium metal ions; the second purpose of the invention is to provide a perovskite quantum dot doped with metallic sodium ions; the invention also aims to provide application of the perovskite quantum dot doped with metal sodium ions in preparation of a light emitting layer of an LED device.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of perovskite quantum dots doped with metal sodium ions comprises the following steps:
(1) adding an oleocesium-sodium precursor and FA to a lead bromide precursor+Stirring and mixing the precursor uniformly, adding a Didecyl Dimethyl Ammonium Bromide (DDAB) solution, and continuously stirring, mixing and dissolving to obtain a mixed solution;
(2) taking the supernatant of the mixed solution in the step (1), adding ethyl acetate, and carrying out rotary centrifugation to obtain a precipitate I;
(3) firstly, adding toluene and ethyl acetate into the precipitate I obtained in the step (2), and obtaining the perovskite quantum dot (Na: CsPbBr) doped with metal sodium ions after rotary centrifugation3)。
Preferably, in the step (1), the lead bromide precursor is prepared according to the following method: mixing lead bromide and tetraoctyl ammonium bromide (TOAB) according to a molar ratio of 1:20, and adding toluene to dissolve the lead bromide and the tetraoctyl ammonium bromide (TOAB) to obtain a lead bromide precursor;
the oil cesium-sodium precursor is prepared as follows: adding cesium carbonate (Cs)2CO3) Mixing with sodium acetate (NaOA) according to the mass ratio of 24.375:15.2, and dissolving in n-octanoic acid to form a precursor of oil cesium-sodium;
the FA+The precursor is prepared according to the following method: dissolving formamidine acetate in n-octanoic acid according to the molar volume ratio of 0.2:1, mmol: mL to form FA+A precursor of (a);
the Didecyl Dimethyl Ammonium Bromide (DDAB) solution was prepared as follows: the Didecyl Dimethyl Ammonium Bromide (DDAB) is dissolved in toluene according to the mass-volume ratio of 10:1, mg: mL to obtain a Didecyl Dimethyl Ammonium Bromide (DDAB) solution.
Preferably, in step (1), the lead bromide precursor, the cesium-sodium oleoyl precursor and FA are used+The volume ratio of the precursor to the Didecyl Dimethyl Ammonium Bromide (DDAB) was 9:0.85:0.15: 3.
Preferably, in the step (2), the volume ratio of the supernatant to the ethyl acetate is 1: 2.
Preferably, in the step (3), the mass-to-volume ratio of the precipitate I, the toluene and the ethyl acetate is 0.5:1:2, and the mg: mL: mL.
Preferably, the rotary centrifugation is specifically: centrifuge in a centrifuge at 9000rpm for 5 min.
2. The perovskite quantum dot doped with the metal sodium ions is prepared according to the preparation method.
3. The perovskite quantum dot doped with the metal sodium ions is applied to the preparation of the light-emitting layer of the LED device.
4. A preparation method of a light emitting layer of an LED device comprises the following specific steps:
in N2In a glove box, the solution formed by dissolving the perovskite quantum dots doped with the metal sodium ions in N-hexane is spin-coated on the PTAA layer for 40s at the speed of 2000rpm, and N is added2Retreat at 60 ℃ in glove boxForming a luminescent layer after firing for 10 min.
5. The LED device luminescent layer prepared according to the preparation method.
The invention has the beneficial effects that:
the invention discloses a preparation method of perovskite quantum dots doped with metal sodium ions, which mainly comprises the steps of preparing a lead bromide precursor, an oil cesium-sodium precursor and FA+The precursor and the didecyl dimethyl ammonium bromide are mixed to prepare the perovskite quantum dot (Na: CsPbBr) doped with the metal sodium ions3). The preparation method is simple and controllable, and the prepared perovskite quantum dot (Na: CsPbBr) doped with metal sodium ions3) The optical material has good optical performance, higher photoluminescence efficiency and fewer defect states; the method has good application effect in the aspect of preparing the luminescent layer of the LED device, and can enhance the performance of the LED device and improve the external quantum efficiency of the LED device.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 shows CsPbBr3Transmission scanning electron microscopy images of quantum dots;
FIG. 2 shows the metallic sodium ion-doped perovskite quantum dot (Na: CsPbBr) prepared in example 13) Transmission scanning electron microscopy images of (a);
FIG. 3 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) A photoluminescence spectrum of (a);
FIG. 4 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) Ultraviolet-visible absorption spectrum of (1);
FIG. 5 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) A photoluminescence efficiency map of (a);
FIG. 6 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) X-ray photoelectron spectroscopy of (1);
FIG. 7 shows the metallic sodium ion-doped perovskite quantum dot (Na: CsPbBr) prepared in example 13) An X-ray photoelectron spectrum Na spectrographic chart of (1);
fig. 8 is a structural view of an LED device using the metallic sodium ion-doped perovskite quantum dots prepared in example 1 as a light emitting layer;
FIG. 9 is an electroluminescence diagram of an LED device using as a light emitting layer the perovskite quantum dots doped with metallic sodium ions prepared in example 1;
FIG. 10 shows CsPbBr respectively3Quantum dot and metal sodium ion doped perovskite quantum dot prepared in example 1 are external quantum efficiency maps of LED devices of the light emitting layer.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Perovskite quantum dot (Na: CsPbBr) doped with metallic sodium ions3) The preparation method comprises the following steps:
(1) preparing a lead bromide precursor: mixing lead bromide and tetraoctyl ammonium bromide (TOAB) according to a molar ratio of 1:20, and adding toluene to dissolve the lead bromide and the tetraoctyl ammonium bromide (TOAB) to obtain a lead bromide precursor;
(2) preparation of an oleocesium-sodium precursor: adding cesium carbonate (Cs)2CO3) Andmixing sodium acetate (NaOA) according to the mass ratio of 24.375:15.2, and dissolving the mixture in n-octanoic acid to form a precursor of oil cesium-sodium;
(3) preparation of FA+(formamidine acetate) precursor: dissolving formamidine acetate in n-octanoic acid according to the molar volume ratio of 0.2:1, mmol: mL to form FA+A precursor of (a);
(4) preparation of a solution of Didecyl Dimethyl Ammonium Bromide (DDAB): dissolving Didecyl Dimethyl Ammonium Bromide (DDAB) into toluene according to the mass-volume ratio of 10:1, mg: mL to obtain a Didecyl Dimethyl Ammonium Bromide (DDAB) solution;
(5) preparation of perovskite quantum dot (Na: CsPbBr) doped with metallic sodium ion3): putting 9ml of lead bromide precursor into a beaker, adding 0.85ml of cesium-sodium precursor and 0.15ml of FA+Magnetically stirring a precursor of (formamidine acetate) for 5min, adding 3ml of Didecyl Dimethyl Ammonium Bromide (DDAB) solution, magnetically stirring for 2min, taking 3ml of supernatant, adding 6ml of ethyl acetate, putting the supernatant into a centrifuge, centrifuging at 9000rpm for 5min to obtain a precipitate I, adding 1ml of toluene and 2ml of ethyl acetate, centrifuging at 9000rpm for 5min to obtain the perovskite quantum dots (Na: CsPbBr) doped with metal sodium ions3)。
And (3) performance testing:
FIG. 1 shows CsPbBr3FIG. 2 is a transmission scanning electron microscope image of the quantum dot, and FIG. 1 shows the metal sodium ion doped perovskite quantum dot (Na: CsPbBr) prepared in example 13) Transmission scanning electron microscopy images of (a). As can be seen from the comparison of FIG. 1 and FIG. 2, the perovskite quantum dot (Na: CsPbBr) doped with metallic sodium ions prepared by the invention3) The size of the particles is more uniform, and the dispersibility is better.
FIG. 3 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) Photoluminescence spectrum of (a). As can be seen from FIG. 3, in CsPbBr3Doping sodium ions in the quantum dots to form perovskite quantum dots (Na: CsPbBr) doped with metallic sodium ions3) Then, the peak value appears blue shift, and the photoluminescence color of the quantum dot material is influenced.
FIG. 4 shows CsPbBr3Quantum dotsAnd the metallic sodium ion-doped perovskite quantum dot (Na: CsPbBr) prepared in example 13) Ultraviolet and visible absorption spectrum of (1). As can be seen from FIG. 4, the doping of the metal sodium ions adopted by the invention has little influence on the band gap of the prepared quantum dot material.
FIG. 5 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) Photoluminescence efficiency map of (a). As can be seen from FIG. 5, compared to CsPbBr3Photoluminescence efficiency of 77.34% for Quantum dots, metallic sodium ion doped perovskite Quantum dots prepared in example 1 (Na: CsPbBr)3) The photoluminescence efficiency of the phosphor was increased to 94.74%, which is illustrated by the increase in CsPbBr3The quantum dots are doped with sodium ions, so that the photoluminescence efficiency can be obviously improved.
FIG. 6 shows CsPbBr3Quantum dots and metallic sodium ion doped perovskite quantum dots prepared in example 1 (Na: CsPbBr)3) X-ray photoelectron spectroscopy. As can be seen from FIG. 6, CsPbBr was doped with sodium ions according to the present invention 34f of Pb in Quantum dots5/2And 4f of Pb7/2The signal peak is shifted by 0.5eV and Br by 3d3/2And 3d5/2The signal peak of (2) is shifted by 0.3eV, thereby showing that the chemical environment inside the material is changed after the quantum dot material is doped by sodium ions.
FIG. 7 shows the metallic sodium ion-doped perovskite quantum dot (Na: CsPbBr) prepared in example 13) The X-ray photoelectron spectrum Na spectrogram. As can be seen from FIG. 7, in Na+Ion doped CsPbBr3Na 1s signals detected in quantum dot samples prove that the preparation method can successfully dope sodium ions into CsPbBr3Quantum dot materials.
An LED device (the structure of which is shown in fig. 8) using the perovskite quantum dot doped with metal sodium ions prepared in example 1 as a light emitting layer is specifically prepared by the following steps:
(1) spin-coating the washed ITO glass with a PEDOT/PSS solution at 4000rpm for 1min, and annealing at 140 ℃ in air for 15min to obtain a PEDOT/PSS layer;
(2) then in N2In a glove box, 8mg/ml of PTAA chlorobenzene solution was spin-coated onto the PEDOT: PSS layer for 40s at 2000rpm on N2Annealing in a glove box at 120 ℃ for 15min to obtain a PTAA layer;
(3) in N2In a glove box, the perovskite quantum dot solution doped with the metal sodium ions is spin-coated on the PTAA layer for 40s at the speed of 2000rpm, and N is added2Annealing in a glove box at 60 ℃ for 10min to obtain a QDs luminescent layer;
(4) and under the vacuum environment, TPBi is continuously deposited through thermal evaporation to be used as an electron transport layer, and LiF/Al is used as a cathode to obtain the LED device.
Fig. 9 is an electroluminescence diagram of an LED device using the metallic sodium ion-doped perovskite quantum dots prepared in example 1 as a light emitting layer. As can be seen from fig. 9, the LED device containing the perovskite quantum dot doped with metal sodium ion as the light emitting layer has a light emission peak of 516nm, and the strongest light emission luminance is obtained at a driving voltage of 6.2V.
FIG. 10 shows CsPbBr respectively3Quantum dot and metal sodium ion doped perovskite quantum dot prepared in example 1 are external quantum efficiency maps of LED devices of the light emitting layer. As can be seen from FIG. 10, CsPbBr of light emitting layer material in LED device3The quantum dots are doped with metal sodium ions, and the external quantum efficiency of the formed LED device is improved from 4.74% to 8.97%.
In summary, the invention discloses a preparation method of a perovskite quantum dot doped with metal sodium ions, which mainly comprises the steps of preparing a lead bromide precursor, an oil cesium-sodium precursor and FA+The precursor and the didecyl dimethyl ammonium bromide are mixed to prepare the perovskite quantum dot (Na: CsPbBr) doped with the metal sodium ions3). The preparation method is simple and controllable, and the prepared perovskite quantum dot (Na: CsPbBr) doped with metal sodium ions3) The optical material has good optical performance, higher photoluminescence efficiency and fewer defect states; the method has good application effect in the aspect of preparing the luminescent layer of the LED device, and can enhance the performance of the LED device and improve the external quantum efficiency of the LED device.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.

Claims (10)

1. A preparation method of a perovskite quantum dot doped with metal sodium ions is characterized by comprising the following steps:
(1) adding an oleocesium-sodium precursor and FA to a lead bromide precursor+Stirring and mixing the precursor uniformly, adding a didecyl dimethyl ammonium bromide solution, and continuously stirring, mixing and dissolving to obtain a mixed solution;
(2) taking the supernatant of the mixed solution in the step (1), adding ethyl acetate, and carrying out rotary centrifugation to obtain a precipitate I;
(3) adding toluene and ethyl acetate into the precipitate I obtained in the step (2), and carrying out rotary centrifugation to obtain the perovskite quantum dot doped with metal sodium ions.
2. The production method according to claim 1, wherein, in the step (1), the lead bromide precursor is produced as follows: mixing lead bromide and tetraoctyl ammonium bromide according to a molar ratio of 1:20, and adding toluene to dissolve the lead bromide and the tetraoctyl ammonium bromide to obtain a lead bromide precursor;
the oil cesium-sodium precursor is prepared as follows: mixing cesium carbonate and sodium acetate according to the mass ratio of 24.375:15.2, and dissolving the mixture in n-octanoic acid to form a precursor of oil cesium-sodium;
the FA+The precursor is prepared according to the following method: dissolving formamidine acetate in n-octanoic acid according to the molar volume ratio of 0.2:1, mmol: mL to form FA+A precursor of (a);
the didecyl dimethyl ammonium bromide solution is prepared according to the following method: the didecyl dimethyl ammonium bromide is dissolved in toluene according to the mass-volume ratio of 10:1, mg: mL to obtain the didecyl dimethyl ammonium bromide solution.
3. The method according to claim 1, wherein in the step (1), the lead bromide precursor, the cesium-sodium precursor, and FA are used+The volume ratio of the precursor to the didecyl dimethyl ammonium bromide is 9:0.85:0.15: 3.
4. The method according to claim 1, wherein in the step (2), the volume ratio of the supernatant to the ethyl acetate is 1: 2.
5. The preparation method according to claim 1, wherein in the step (3), the mass-to-volume ratio of the precipitate I, the toluene and the ethyl acetate is 0.5:1:2, mg: mL: mL.
6. The method for preparing according to claim 1, wherein the rotary centrifugation is specifically: centrifuge in a centrifuge at 9000rpm for 5 min.
7. The perovskite quantum dot doped with the metallic sodium ions prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the metallic sodium ion doped perovskite quantum dot of claim 7 in the preparation of an LED device light emitting layer.
9. A preparation method of a light emitting layer of an LED device is characterized by comprising the following specific steps:
in N2In a glove box, the solution of the perovskite quantum dot doped with metallic sodium ions of claim 7 dissolved in N-hexane was spin-coated on the PTAA layer at 2000rpm for 40s2Annealing at 60 deg.C for 10min in glove box to form luminescent layer.
10. The light-emitting layer of the LED device prepared by the preparation method according to claim 9.
CN202210223839.6A 2022-03-09 2022-03-09 Preparation method of perovskite quantum dot doped with metal sodium ions, product and application thereof Pending CN114591739A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115594413A (en) * 2022-10-21 2023-01-13 榆林学院（Cn） Preparation method of sodium-doped two-dimensional perovskite thin film
CN115612492A (en) * 2022-11-10 2023-01-17 吉林大学 Preparation method and application of high-entropy alloy-doped perovskite nanocrystalline synthesized at room temperature
WO2023197435A1 (en) * 2022-04-12 2023-10-19 重庆邮电大学 Preparation method for sodium and copper co-doped cesium-lead-bromine perovskite quantum dots, product thereof and application thereof
CN116925742A (en) * 2023-07-26 2023-10-24 桑若(厦门)光伏产业有限公司 Preparation method of ligand self-coated perovskite quantum dot

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YI HUANG ET AL.: "Sodium doping for enhanced performance by highly efficient CsPbBr3 quantum dot-based electroluminescent light-emitting diodes" *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023197435A1 (en) * 2022-04-12 2023-10-19 重庆邮电大学 Preparation method for sodium and copper co-doped cesium-lead-bromine perovskite quantum dots, product thereof and application thereof
CN115594413A (en) * 2022-10-21 2023-01-13 榆林学院（Cn） Preparation method of sodium-doped two-dimensional perovskite thin film
CN115594413B (en) * 2022-10-21 2023-12-29 榆林学院 Preparation method of sodium-doped two-dimensional perovskite film
CN115612492A (en) * 2022-11-10 2023-01-17 吉林大学 Preparation method and application of high-entropy alloy-doped perovskite nanocrystalline synthesized at room temperature
CN115612492B (en) * 2022-11-10 2023-09-26 吉林大学 Preparation method and application of high-entropy alloy doped perovskite nanocrystalline synthesized at room temperature
CN116925742A (en) * 2023-07-26 2023-10-24 桑若(厦门)光伏产业有限公司 Preparation method of ligand self-coated perovskite quantum dot
CN116925742B (en) * 2023-07-26 2024-01-30 桑若(厦门)光伏产业有限公司 Preparation method of ligand self-coated perovskite quantum dot

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