CN114517092B - CSPbBr 3 Perovskite quantum dot and preparation method thereof - Google Patents

CSPbBr 3 Perovskite quantum dot and preparation method thereof Download PDF

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CN114517092B
CN114517092B CN202210078910.6A CN202210078910A CN114517092B CN 114517092 B CN114517092 B CN 114517092B CN 202210078910 A CN202210078910 A CN 202210078910A CN 114517092 B CN114517092 B CN 114517092B
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韦松
王令东
周迅伊
黄薛勇
缪菊红
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Nanjing University of Information Science and Technology
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Abstract

The invention designs a luminescent semiconductor nanomaterial and provides CsPbBr 3 The invention uses the advantages of two-phase synthesis method, adopts toluene solution of cesium oleate and aqueous solution of bromide ion and lead ion to react under normal pressure, and leads CsPbBr 3 Perovskite quantum dots nucleate and grow at the interface and are coated by oleic acid ligand at the same time, and generated CsPbBr 3 The perovskite quantum dots can be stably dispersed in organic solvents such as toluene, xylene and the like, and strong green light can be observed. The green CsPbBr prepared by the invention 3 The perovskite quantum dot can be excited by ultraviolet, near ultraviolet and blue light, and has high color purity and high fluorescence quantum efficiency. The preparation process is simple, the preparation process is carried out in an air atmosphere at room temperature, the harsh conditions that high-temperature heating, inert gas atmosphere protection and the like are required in the traditional organic phase synthesis are avoided, the perovskite quantum dots are successfully prepared at the two-phase interface of the water phase and the organic phase, and the speed for preparing the perovskite quantum dots and the size of the quantum dots are effectively controlled.

Description

CSPbBr 3 Perovskite quantum dot and preparation method thereof
Technical Field
The invention belongs to the technical field of perovskite quantum dot preparation, and particularly relates to a CSPbBr3 perovskite quantum dot and a preparation method thereof.
Background
The quantum dot light emitting diode (QLED) belongs to an active self-luminous device, has the characteristics of low energy consumption, high color purity, low preparation cost, simple process and the like, and has wide application prospect in the fields of solid-state lighting, wide color gamut, ultrahigh-definition flexible display and the like. Although the QLED has greatly improved performances such as brightness and external quantum efficiency, many basic problems need to be solved in the aspects of synthesizing perovskite quantum dots with high brightness and good stability. In a QLED device, the performance of the quantum dot has important influence on technical indexes such as brightness, luminous efficiency, energy consumption, color rendering index and the like of the QLED, so that the preparation of the quantum dot is one of key technologies in the QLED and is widely focused by scientific researchers.
The perovskite quantum dots reported in the prior literature are mostly prepared by using a polar solvent in a high-temperature inert gas atmosphere (Nano Letters,2015,15 (6): 3692-6.), or prepared by using a polar antisolvent (ACS Nano,2015,9 (4): 4533-42.), and the preparation methods cannot control the size of the quantum dots, have poor reproducibility, complex process and high preparation cost; in addition, polar solvents can degrade perovskite quantum dots, reducing their production yields. These factors severely affect and limit the large-scale fabrication and commercial application of perovskite light emitting devices. Therefore, it is important to develop a preparation method with good process reproducibility, low preparation cost, high yield and stable quantum dot performance.
Disclosure of Invention
The invention aims to provide a method for preparing CsPbBr in room temperature air atmosphere 3 The method for preparing the perovskite quantum dot is characterized in that the perovskite quantum dot is prepared at a two-phase interface, the quantum dot is nucleated and grown at the interface by utilizing the advantages of an interface synthesis method, the prepared quantum dot has good process reproducibility, controllable size, narrow size distribution, high fluorescence quantum efficiency, high color purity and good air atmosphere long-term stability. The method avoids the harsh conditions of high-temperature heating, inert gas atmosphere protection and the like required by the traditional organic phase synthesis, successfully prepares the perovskite quantum dots at the two-phase interface of the water phase and the organic phase, and effectively controls the speed of preparing the perovskite quantum dots and the size of the quantum dots.
The invention provides a high-quality CsPbBr 3 The preparation method of the green perovskite quantum dot comprises the following steps:
s1, dissolving cesium salt precursor compound in oleic acid under the condition of heating at 120-185 ℃ in an air atmosphere, removing impurity water contained in the oleic acid in the temperature range, cooling to room temperature, adding an organic solvent to dilute to 0.09-0.11mmol/ml, and preparing organic solution A of cesium ions;
s2, dissolving ammonium salt containing bromide ions in an organic solvent under the air atmosphere at room temperature to form an organic solution B with the concentration of bromide ions of 0.09-0.11 mmol/ml;
step S3, ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.09-0.11 mmol/ml;
step S4, mixing the solution A and the solution B according to a ratio of 1:1, adding the mixed solution of the solution A and the solution B into a container containing the solution C with the volume equal to that of the mixed solution, and observing the green CsPbBr at the interface between the water phase and the organic phase in the container 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Further, in the step S1, the cesium salt precursor compound is any one of cesium carbonate and cesium hydroxide.
Further, in the step S1, the organic solvent used for dilution includes any one of toluene, xylene, methylene chloride, chloroform, and n-hexane.
Further, in the step S2, the ammonium salt containing bromide ion includes any one of tetra-n-octyl ammonium bromide, tetra-n-butyl ammonium bromide and bi-hexadecyl dimethyl ammonium bromide.
Further, in the step S2, the organic solvent for dissolving the ammonium salt containing bromide ion includes any one of toluene, xylene, methylene chloride, chloroform, and n-hexane.
Preferably, in said step S1, the cesium salt has a dissolution temperature in oleic acid of 120 ℃ to 180 ℃.
More preferably, in step S1, the cesium salt has a dissolution temperature in oleic acid of 175 ℃ to 185 ℃.
More preferably, in the step S1, the heating temperature of the air atmosphere is 180 ℃.
Preferably, in the step S1, the concentration of the cesium salt precursor compound of the organic solution A is 0.1mmol/ml.
Preferably, in the step S2, the concentration of bromide ions in the organic solution B is 0.1mmol/ml.
Preferably, in the step S3, the concentration of lead ions in the aqueous solution C is 0.1mmol/ml.
The quantum prepared by the preparation methodThe chemical formula of the dot is CsPbBr 3 The crystal structure is a monoclinic phase.
Compared with the prior art, the invention has the following remarkable advantages:
1. the preparation process is simple, the whole reaction is carried out in an air atmosphere, the protection of a high-temperature inert gas atmosphere is not needed, and the cost is saved.
2. CsPbBr prepared according to the technical scheme of the invention 3 The perovskite quantum dot has stronger green light emission, high fluorescence quantum efficiency, emission peak near 502nm and high color purity, and has wide application prospect in the fields of wide color gamut, ultra-high definition, flexible display and the like in the future.
3. CsPbBr prepared according to the technical scheme of the invention 3 The perovskite quantum dot emits strong green light under ultraviolet and near ultraviolet excitation, and has good long-term stability of air atmosphere.
4. According to the technical scheme of the invention, the synthesis rate of the perovskite quantum dots and the growth size of the quantum dots can be effectively controlled by changing the concentration of the precursor in the aqueous phase or the organic phase solution.
Drawings
FIG. 1 is CsPbBr prepared in example 1 3 X-ray diffraction pattern of perovskite quantum dots.
FIG. 2 is CsPbBr prepared in example 1 3 Ultraviolet absorption and fluorescence emission spectra of perovskite quantum dots.
FIG. 3 is CsPbBr prepared in example 1 3 Projection electron micrograph of perovskite quantum dots.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
this example prepares CsPbBr 3 Calcium titaniumThe preparation method of the mineral quantum dots comprises the following specific steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
The CsPbBr 3 The perovskite quantum dot has good crystallinity, and the interplanar spacing d value and the relative strength of the diffraction front and CsPbBr 3 The standard PDF card (18-0364) of the perovskite quantum dot accords with the standard PDF card, belongs to a monoclinic system and is shown in figure 1.
The CsPbBr 3 Under the excitation of 365nm near ultraviolet light, the perovskite quantum dot emits bright green light with the emission peak position of about 502nm, as shown in fig. 2. The CsPbBr 3 The perovskite quantum dot has regular cube morphology and the size is about 11.6-13.5 nm, as shown in figure 3.
Example 2:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium hydroxide in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 3:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving dicetyl dimethyl ammonium bromide in toluene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 4:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding dimethylbenzene to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in xylene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 5:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding chloroform to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. tetrabutylammonium bromide is dissolved in chloroform under the air atmosphere at room temperature to form an organic solution B with the concentration of bromide ion of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 6:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding methylene dichloride to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in methylene dichloride under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 7:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in an air atmosphere, cooling to room temperature, and adding chloroform to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving ditetyl dimethyl ammonium bromide in chloroform under room temperature air atmosphere to form an organic solution B with the concentration of bromide ion of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 8:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium hydroxide in oleic acid under the condition of heating at 175 ℃ in an air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.11mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.11 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.11 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 9:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 185 ℃ in an air atmosphere, cooling to room temperature, and adding n-hexane to dilute to 0.09mmol/ml to prepare organic solution A of cesium ions;
2. dissolving dicetyl dimethyl ammonium bromide in n-hexane under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.09 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.09 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 10:
this example prepares CsPbBr 3 The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium hydroxide in oleic acid under the condition of heating at 120 ℃ in an air atmosphere, cooling to room temperature, and then adding toluene to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
Example 11:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 185 ℃ in an air atmosphere, cooling to room temperature, and adding methylene dichloride to dilute to 0.1mmol/ml to prepare organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in methylene dichloride under the air atmosphere at room temperature to form an organic solution B with the bromide ion concentration of 0.1 mmol/ml;
3. ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
4. firstly, 20ml of solution C is added into a 50ml beaker, then, after the solution A and the solution B are mixed according to the ratio of 1:1, 20ml of mixed solution of the solution A and the solution B is added into a beaker containing 20ml of solution C, and green CsPbBr can be observed at the interface of water phase and organic phase in the beaker 3 Perovskite quantum dots are slowly generated and dissolve in the organic phase.
The above description is only of the preferred embodiments of the present invention; the scope of the invention is not limited in this respect. Any person skilled in the art, within the technical scope of the present disclosure, may apply to the present invention, and the technical solution and the improvement thereof are all covered by the protection scope of the present invention.

Claims (4)

1. CsPbBr 3 The preparation method of the perovskite quantum dot is characterized by comprising the following steps of: the method comprisesThe green perovskite quantum dot is prepared by the following method:
s1, dissolving a cesium salt precursor compound in oleic acid under the condition of heating at 120-185 ℃ in an air atmosphere, cooling to room temperature, and adding an organic solvent to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
s2, dissolving ammonium salt containing bromide ions in an organic solvent under the air atmosphere at room temperature to form an organic solution B with the concentration of bromide ions of 0.1 mmol/ml;
step S3, ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with the lead ion concentration of 0.1 mmol/ml;
s4, mixing the solution A and the solution B according to a ratio of 1:1, adding the mixed solution of the solution A and the solution B into a container containing a solution C with the same volume as the mixed solution, wherein perovskite quantum dots are generated at the interface between a water phase and an organic phase in the container, and the perovskite quantum dots are dissolved in the organic phase;
in the step S1, the organic solvent used for dilution includes any one of toluene, xylene, methylene chloride, chloroform and n-hexane; in the step S2, the ammonium salt containing bromide ion includes any one of tetra-n-octyl ammonium bromide, tetra-n-butyl ammonium bromide and bi-hexadecyl dimethyl ammonium bromide, and the organic solvent used for dissolving the ammonium salt containing bromide ion includes any one of toluene, xylene, methylene dichloride, chloroform and n-hexane.
2. A CsPbBr according to claim 1 3 The preparation method of the perovskite quantum dot is characterized by comprising the following steps of: in the step S1, the cesium salt precursor compound is any one of cesium carbonate and cesium hydroxide.
3. A CsPbBr according to claim 2 3 The preparation method of the perovskite quantum dot is characterized by comprising the following steps of: in the step S1, the heating temperature in the air atmosphere is 180 ℃.
4. CsPbBr 3 Perovskite quantum dot, its specialThe method is characterized in that: the chemical formula of the quantum dot is CsPbBr 3 The crystalline structure is a monoclinic phase, and is prepared by the preparation method according to any one of claims 1 to 3.
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