CN114517092A - CSPbBr3Perovskite quantum dot and preparation method thereof - Google Patents

CSPbBr3Perovskite quantum dot and preparation method thereof Download PDF

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CN114517092A
CN114517092A CN202210078910.6A CN202210078910A CN114517092A CN 114517092 A CN114517092 A CN 114517092A CN 202210078910 A CN202210078910 A CN 202210078910A CN 114517092 A CN114517092 A CN 114517092A
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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 nano material, and provides CsPbBr3The invention relates to an inorganic perovskite quantum dot and a preparation method thereof, which utilize the advantages of a two-phase synthesis method, and adopt the reaction of a toluene solution of cesium oleate and aqueous solutions of bromide ions and lead ions under normal pressure to ensure that CsPbBr3The perovskite quantum dots nucleate and grow on the interface and are coated by the oleic acid ligand at the same time, and the generated CsPbBr3The perovskite quantum dots can be stably dispersed in organic solvents such as toluene and xylene, and strong green light can be observed. The green CsPbBr prepared by the invention3The perovskite quantum dots can be excited by ultraviolet, near ultraviolet and blue light, and have high color purity and high fluorescence quantum efficiency. The preparation method has simple preparation process, the preparation process is carried out in the air atmosphere at room temperature, and the requirement of traditional organic phase synthesis is avoidedUnder harsh conditions of high-temperature heating, inert gas atmosphere protection and the like, the perovskite quantum dots are successfully prepared on the two-phase interface of the water phase and the organic phase, and the rate of preparing the perovskite quantum dots and the size of the quantum dots are effectively controlled.

Description

CSPbBr3Perovskite 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 illumination, wide color gamut, ultrahigh-definition flexible display and the like. Although the performance of the QLED in terms of brightness, external quantum efficiency and the like is greatly improved, there are many fundamental problems to be solved in terms of synthesizing perovskite quantum dots with high brightness and good stability. In a QLED device, the performance of a quantum dot has an important influence on the technical indexes of the QLED, such as luminance, luminous efficiency, energy consumption, color rendering index, and the like, and therefore, the preparation of the quantum dot is one of the key technologies in the QLED and is widely concerned by researchers.
The perovskite quantum dots reported in the literature at present are mostly prepared by using polar solvents in high-temperature inert gas atmosphere (Nano Letters,2015,15(6): 3692-6), or prepared by using polar anti-solvents (ACS Nano,2015,9(4): 4533-42). the preparation methods can not control the size of the quantum dots, have poor reproducibility, are complex in process and have high preparation cost; in addition, the polar solvent can degrade the perovskite quantum dots and reduce the preparation yield of the perovskite quantum dots. 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 atmosphere3The method for preparing the perovskite quantum dots is characterized in that the perovskite quantum dots are prepared on a two-phase interface, the advantages of an interface synthesis method are utilized, the quantum dots are nucleated and grow on the interface, and the prepared quantum dots have good process reproducibility, controllable size, narrow size distribution, high fluorescence quantum efficiency, high color purity and good long-term stability of air atmosphere. The invention avoids the harsh conditions of high-temperature heating, inert gas atmosphere protection and the like required by the traditional organic phase synthesis, and successfully combines the organic phase and the aqueous phaseThe perovskite quantum dots are prepared by the two-phase interface of the organic phase, so that the rate of preparing the perovskite quantum dots and the size of the quantum dots are effectively controlled.
The invention provides high-quality CsPbBr3The preparation method of the green perovskite quantum dot comprises the following steps:
step S1, dissolving a cesium salt precursor compound in oleic acid under the condition of heating at the temperature of 120-185 ℃ in the 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 an organic solution A of cesium ions;
step S2, dissolving ammonium salt containing bromide ions in an organic solvent at room temperature in an air atmosphere to form an organic solution B with the bromide ion concentration of 0.09-0.11 mmol/ml;
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, after the solution A and the solution B are mixed according to the ratio of 1:1, the mixed solution of the solution A and the solution B is added into a container containing a solution C with the same volume as the mixed solution, and the interface of the water phase and the organic phase in the container can observe green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Further, in step S1, the cesium salt precursor compound is any one of cesium carbonate and cesium hydroxide.
Further, in the step S1, the organic solvent for dilution includes any one of toluene, xylene, dichloromethane, chloroform, and n-hexane.
Further, in step S2, the ammonium salt containing bromide ions includes any one of tetra-n-octylammonium bromide, tetra-n-butylammonium bromide, and dihexadecyldimethylammonium bromide.
Further, in the step S2, the organic solvent for dissolving the ammonium salt containing bromide ions includes any one of toluene, xylene, dichloromethane, chloroform, and n-hexane.
Preferably, in the step S1, the dissolution temperature of the cesium salt in oleic acid is 120 ℃ to 180 ℃.
More preferably, in step S1, the dissolution temperature of the cesium salt in oleic acid is 175 ℃ to 185 ℃.
More preferably, in the step S1, the heating temperature in the air atmosphere is 180 ℃.
Preferably, in the step S1, the organic solution a has a cesium salt precursor compound concentration of 0.1 mmol/ml.
Preferably, in the step S2, the bromide ion concentration in the organic solution B is 0.1 mmol/ml.
Preferably, in the step S3, the lead ion concentration in the aqueous solution C is 0.1 mmol/ml.
The chemical formula of the quantum dot prepared by the preparation method is CsPbBr3The crystal structure is monoclinic.
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 the air atmosphere, the protection of high-temperature inert gas atmosphere is not needed, and the cost is saved.
2. CsPbBr prepared according to technical scheme of the invention3The perovskite quantum dot has stronger green light emission and high fluorescence quantum efficiency, the emission peak of the perovskite quantum dot is near 502nm, the color purity is high, and the perovskite quantum dot has wide application prospect in the fields of wide color gamut, ultrahigh definition, flexible display and the like in the future.
3. CsPbBr prepared according to technical scheme of the invention3The perovskite quantum dots emit strong green light under the excitation of ultraviolet and near ultraviolet, and have 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 shows CsPbBr prepared in example 13X-ray diffraction spectrum of the perovskite quantum dots.
FIG. 2 isExample 1 CsPbBr prepared3Ultraviolet absorption and fluorescence emission spectra of perovskite quantum dots.
FIG. 3 is CsPbBr prepared in example 13Projection electron micrographs of perovskite quantum dots.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
this example preparation CsPbBr3The perovskite quantum dot is prepared by 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 an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, mixing the solution A and the solution B according to a ratio of 1:1, adding the mixed solution of 20ml of solution A and solution B into the beaker containing 20ml of solution C, and observing the interface of the aqueous phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
The CsPbBr3The perovskite quantum dot has good crystallinity, and the interplanar spacing d value and the relative strength of the diffraction front of the perovskite quantum dot and CsPbBr3The standard PDF card (18-0364) of perovskite quantum dots conforms to, and belongs to the monoclinic system, as shown in FIG. 1.
The CsPbBr3Near 365nm of perovskite quantum dotsUnder the excitation of ultraviolet light, the emission peak position is about 502nm, and the light is bright green light emission, as shown in figure 2. The CsPbBr3The perovskite quantum dots have regular cubic morphology and the size is about 11.6-13.5 nm, as shown in FIG. 3.
Example 2:
this example preparation CsPbBr3The perovskite quantum dot comprises the following specific preparation steps:
1. dissolving cesium hydroxide in oleic acid under the condition of heating at 180 ℃ in the air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 3:
this example preparation CsPbBr3The perovskite quantum dot is prepared by 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 an organic solution A of cesium ions;
2. dissolving dicetyl dimethyl ammonium bromide in toluene at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, and adding solution A and solution BMixing at a ratio of 1:1, adding 20ml of the mixture of solution A and solution B into a beaker containing 20ml of solution C, and observing the interface of the water phase and the organic phase in the beaker to obtain green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 4:
this example preparation CsPbBr3The perovskite quantum dot is prepared by the following specific steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in the air atmosphere, cooling to room temperature, and adding xylene to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in dimethylbenzene at room temperature in the air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 5:
this example preparation CsPbBr3The perovskite quantum dot is prepared by the following specific steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in the air atmosphere, cooling to room temperature, and adding trichloromethane to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetrabutylammonium bromide in chloroform at room temperature in the air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. 20ml of solution C were added to 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 the interface of the water phase and the organic phase in the beaker can observe green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 6:
this example preparation CsPbBr3The 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 dichloromethane to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in dichloromethane at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 7:
this example preparation CsPbBr3The perovskite quantum dot is prepared by the following specific steps:
1. dissolving cesium carbonate in oleic acid under the condition of heating at 180 ℃ in the air atmosphere, cooling to room temperature, and adding trichloromethane to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving dicetyl dimethyl ammonium bromide in chloroform at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. firstly, useAdding 20ml of solution C into a 50ml beaker, mixing the solution A and the solution B according to a ratio of 1:1, adding a mixed solution of 20ml of solution A and solution B into the beaker containing 20ml of solution C, and observing a green CsPbBr at the interface of an aqueous phase and an organic phase in the beaker3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 8:
this example preparation CsPbBr3The 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 an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene at room temperature in air atmosphere 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 lead ion concentration of 0.11 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 9:
this example preparation CsPbBr3The perovskite quantum dot is prepared by the following specific 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 an organic solution A of cesium ions;
2. dissolving dicetyl dimethyl ammonium bromide in n-hexane at room temperature in an air atmosphere 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 a water solution C with lead ion concentration of 0.09 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
Example 10:
this example preparation CsPbBr3The perovskite quantum dot is prepared by the following specific steps:
1. dissolving cesium hydroxide in oleic acid under heating at 120 ℃ in an air atmosphere, cooling to room temperature, and adding toluene to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in toluene at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beaker, 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 of 20ml into the beaker containing the solution C of 20ml, and observing the interface of the water phase and the organic phase in the beaker to obtain the green CsPbBr3Perovskite quantum dots are slowly generated and dissolved 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 dichloromethane to dilute to 0.1mmol/ml to prepare an organic solution A of cesium ions;
2. dissolving tetra-n-octyl ammonium bromide in dichloromethane at room temperature in air atmosphere 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 lead ion concentration of 0.1 mmol/ml;
4. adding 20ml of solution C into a 50ml beakerAfter 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 the interface of the water phase and the organic phase in the beaker can observe green CsPbBr3Perovskite quantum dots are slowly generated and dissolved in the organic phase.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims (10)

1. CsPbBr3The preparation method of the perovskite quantum dot is characterized in that;
the green-light perovskite quantum dot is prepared by the following method:
step S1, dissolving a cesium salt precursor compound in oleic acid under the condition of heating at the temperature of 120-185 ℃ in the air atmosphere, cooling to room temperature, adding an organic solvent to dilute to 0.09-0.11mmol/ml, and preparing an organic solution A of cesium ions;
step S2, dissolving ammonium salt containing bromide ions in an organic solvent at room temperature in the air atmosphere to form an organic solution B with bromide ion concentration of 0.09-0.11 mmol/ml;
step S3, ultrasonically dissolving lead acetate in deionized water to form an aqueous solution C with lead ion concentration of 0.09-0.11 mmol/ml;
and step S4, mixing the solution A and the solution B according to the 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, and generating perovskite quantum dots at the interface of an aqueous phase and an organic phase in the container and dissolving the perovskite quantum dots in the organic phase.
2. The CsPbBr of claim 13The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in step S1, the cesium salt precursor compound is any one of cesium carbonate and cesium hydroxide.
3. A CsPbBr according to claim 23The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S1, the organic solvent used for dilution includes any one of toluene, xylene, dichloromethane, chloroform, and n-hexane.
4. A CsPbBr according to claim 33The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S2, the ammonium salt containing bromide ions includes any one of tetra-n-octylammonium bromide, tetra-n-butylammonium bromide, and dihexadecyldimethylammonium bromide.
5. A CsPbBr according to claim 43The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S2, the organic solvent for dissolving the ammonium salt containing bromide ions includes any one of toluene, xylene, dichloromethane, chloroform, and n-hexane.
6. A CsPbBr according to claim 53The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S1, the heating temperature in the air atmosphere is 180 ℃.
7. The CsPbBr of claim 63The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in step S1, the organic solution a has a cesium salt precursor compound concentration of 0.1 mmol/ml.
8. A CsPbBr according to claim 73The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S2, the bromide ion concentration in the organic solution B is 0.1 mmol/ml.
9. A CsPbBr according to claim 83The preparation method of the perovskite quantum dot is characterized by comprising the following steps: in the step S3, the water is usedThe lead ion concentration in the solution C was 0.1 mmol/ml.
10. CsPbBr3A perovskite quantum dot characterized by: the chemical formula of the quantum dot is CsPbBr3The crystalline structure is a monoclinic phase, and is prepared by the preparation method of any one of claims 1 to 9.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN115651636A (en) * 2022-11-14 2023-01-31 昆明理工大学 Perovskite quantum dot film and preparation method thereof

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