CN115536059B - CsPbBr3Nanosheets, preparation method and application thereof - Google Patents

CsPbBr3Nanosheets, preparation method and application thereof Download PDF

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CN115536059B
CN115536059B CN202211315620.5A CN202211315620A CN115536059B CN 115536059 B CN115536059 B CN 115536059B CN 202211315620 A CN202211315620 A CN 202211315620A CN 115536059 B CN115536059 B CN 115536059B
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高妍
宋济安
胡桃
孟智超
江泽龙
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Wuyi University
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Abstract

The invention belongs to the technical field of nano materials, and provides a CsPbBr 3 nano sheet, a preparation method and application thereof, wherein a precursor solution containing Cs salt and Pb salt is firstly mixed and reacted, then a third precursor solution containing NiBr 2 is added, ion exchange and Ni-Br passivation are carried out during the reaction, the prepared CsPbBr 3 nano sheet has the characteristics of high blue light emission and luminous intensity, the fluorescence quantum yield can reach 78%, the stability is good, the CsPbBr 3 nano sheet is dispersed in the solution to show excellent stability, the emission intensity of not less than 86.3% can be maintained after the CsPbBr 3 nano sheet is stored at room temperature for 30 days, and the CsPbBr 3 nano sheet can be stored for a long time; in addition, the preparation method provided by the invention is simple, the preparation can be carried out at room temperature without external heat sources and inert gases, the reaction period is short, the raw material price is low, and the required equipment is simple.

Description

CsPbBr 3 nano-sheet, and preparation method and application thereof
Technical Field
The invention relates to the technical field of nano materials, in particular to a CsPbBr 3 nano sheet, a preparation method and application thereof.
Background
The all-inorganic perovskite nanocrystals have the advantages of high fluorescence quantum yield, adjustable luminescence spectrum, high color purity and the like, and are widely focused by scientific researchers, so that the all-inorganic perovskite nanocrystals have good application prospects in the fields of display, illumination, solar cells and the like. Blue light emitting perovskite is more commonly CsPbCl 3 nanocrystals or CsPbCl XBr3-X nanocrystals, but all suffer from poor stability and low fluorescence quantum yield. And the two-dimensional CsPbBr 3 nano-sheet is limited in a certain dimension in the growth process and is influenced by quantum confinement effect, so that the band gap is enlarged, the emission peak is blue-shifted, and more obvious exciton absorption and narrower half-peak width are shown. Therefore, the blue light emission of the CsPbBr 3 nano-sheet is purer, and the stability is greatly improved. However, the light-emitting intensity of the common CsPbBr 3 nano-sheet is weaker, mainly due to the defect increase caused by the larger surface volume ratio, the possibility of capturing excitons by the defect becomes large, and the fluorescence quantum yield is reduced, and the value is usually less than 40%. Therefore, development of a blue light emitting CsPbBr 3 nano-sheet with high luminous intensity is needed.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the CsPbBr 3 nano-sheet, the preparation method and the application thereof are provided, the prepared CsPbBr 3 nano-sheet not only has blue light emission, but also has high fluorescence quantum yield of more than or equal to 40 percent and even 78 percent, the luminous intensity is high, the stability is good, the CsPbBr 3 nano-sheet is dispersed in the solution to show excellent stability, and the emission intensity of not less than 86.3 percent can be maintained after the CsPbBr 3 nano-sheet is stored for 30 days at room temperature.
The first aspect of the invention provides a preparation method of CsPbBr 3 nano-sheets.
Specifically, the preparation method of the CsPbBr 3 nano-sheet comprises the following steps:
(1) Dissolving Cs salt in a first solvent to prepare a first precursor solution; dissolving Pb salt in a second solvent, and adding oleic acid and oleylamine to prepare a second precursor solution; dissolving NiBr 2 in a third solvent to prepare a third precursor solution;
(2) Mixing the first precursor solution and the second precursor solution, reacting, adding an organic solvent, adding a third precursor solution, continuing the reaction, adding a precipitant, and centrifuging to obtain the CsPbBr 3 nano-sheet.
According to the preparation method, the precursor solution is prepared by using Cs salt and Pb salt respectively, the Cs salt and the Pb salt are mixed and react, the nanosheets nucleate and grow, oleic acid and oleylamine are used as surface ligands to protect the nanosheets, then a third precursor solution containing NiBr 2 is added, ion exchange and surface Ni-Br passivation are carried out during the process, on one hand, ni with smaller atomic radius replaces Pb with larger radius, the crystal structure is contracted, and the binding force between Ni-Br is higher than that of Pb-Br, so that the stability of the nanosheets is improved to a certain extent; on the other hand, the additional Br ions passivate halogen vacancies on the surface of the CsPbBr 3 nano-sheet, reduce defect density, improve fluorescence quantum yield, and finally precipitate the crystallized nano-sheet from the solution by adding a precipitant to obtain the CsPbBr 3 nano-sheet. The CsPbBr 3 perovskite nano sheet prepared by the invention not only has blue light emission, but also has high fluorescence quantum yield, high luminous intensity and good stability.
Preferably, the molar ratio of the Ni element in the NiBr 2 to the Pb element in the Pb salt is 1:1-50.
More preferably, the molar ratio of the Ni element in the NiBr 2 to the Pb element in the Pb salt is 1:2-40.
Further preferably, the molar ratio of the Ni element in the NiBr 2 to the Pb element in the Pb salt is 1: 40. 1: 10. 1:5.7, 1:4 or 1: 3.1.
Preferably, the Cs salt is Cs 2CO3 and/or cesium acetate.
Preferably, the Pb salt is PbBr 2.
Preferably, the first solvent is octanoic acid and/or oleic acid.
Preferably, the second solvent is toluene.
Preferably, the third solvent is hydrobromic acid.
Preferably, in step (2), before mixing the first precursor solution and the second precursor solution, the method further comprises the steps of pouring the second precursor solution into the reaction vessel, stirring at a speed of 1000-1400 rpm, and pouring the second precursor solution into the first precursor solution in a time of 1-5 seconds. The invention adopts a faster stirring rate to stir the second precursor solution and then rapidly adds the second precursor solution into the first precursor solution, so as to ensure that the components are better and evenly mixed and be beneficial to the growth of the nano-sheets.
Preferably, in step (2), the reaction time is 10-50s after the first precursor solution and the second precursor solution are mixed.
Preferably, in step (2), the reaction is continued at a temperature of 20-30℃for a period of 20-40 minutes.
More preferably, in step (2), the reaction is continued at a temperature of 25℃for a period of 30 minutes.
Preferably, the precipitant is one or more of ethyl acetate, acetone and acetonitrile. The precipitant has the function of separating nano sheet from solution and purifying.
More preferably, the precipitant is ethyl acetate. Acetone and acetonitrile have larger polarity.
A second aspect of the invention provides a CsPbBr 3 nanoplatelet.
A CsPbBr 3 nano-sheet, the fluorescence quantum yield of the CsPbBr 3 nano-sheet is more than or equal to 40%.
Preferably, the CsPbBr 3 nanosheets have a fluorescence quantum yield of 40-78%.
More preferably, the CsPbBr 3 nanosheets have a fluorescence quantum yield of 55.5-78%.
A third aspect of the invention provides the use of CsPbBr 3 nanoplatelets.
An application of CsPbBr 3 nano-sheet in the fields of display, illumination and solar cells.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the preparation method, the precursor solution is prepared by using Cs salt and Pb salt respectively, the Cs salt and the Pb salt are mixed and reacted, then the precursor solution containing NiBr 2 is added, and ion exchange and Ni-Br passivation are carried out during the process, so that the luminous intensity of the prepared CsPbBr 3 nanosheets is improved;
(2) The CsPbBr 3 nano-sheet prepared by the invention has blue light emission, high fluorescence quantum yield which can reach 78%, high luminous intensity, good stability and narrow half-peak width which is not more than 14.1nm, and can be observed to have obvious improvement of the luminous intensity in the reaction process; the CsPbBr 3 nano-sheet obtained by the reaction shows excellent stability when being dispersed in a solution, can maintain the emission intensity of not less than 86.3% after being stored for 30 days at room temperature, and can be stored for a long time.
Drawings
FIG. 1 is a graph showing fluorescence spectra of CsPbBr 3 nanoplatelets prepared in examples 1-5 and comparative example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) image of CsPbBr 3 nano-sheets prepared in comparative example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of CsPbBr 3 nanosheets prepared in example 3 of the present invention;
FIG. 4 is a transmission electron microscope image of CsPbBr 3 nanosheets (side thickness) prepared in example 3 of the present invention;
FIG. 5 is a graph of X-ray diffraction (XRD) contrast of CsPbBr 3 nanoplatelets prepared in examples 1-5 and comparative example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
The raw materials of Cs 2CO3 (cesium carbonate), lead bromide (PbBr 2)、NiBr2 (nickel bromide), toluene, isopropyl alcohol, oleic acid, oleylamine, ethyl acetate, and the like used in each of the following examples and comparative examples were all analytically pure reagents, and the power of the ultrasonic cleaner used was 450W, and the power was adjustable.
Example 1
A preparation method of CsPbBr 3 nano-sheets comprises the following steps:
(1) Dissolving 0.04mmol of Cs 2CO3 in 2mL of octanoic acid, and performing ultrasonic treatment until the powder is completely dissolved to prepare a first precursor solution;
(2) Dissolving 0.2mmol of PbBr 2 in 8mL of toluene, adding 1mL of oleic acid and 1mL of oleylamine, performing ultrasonic dissolution until all powder is dissolved, and preparing a second precursor solution;
(3) Dissolving 0.2mmol of NiBr 2 in 0.2mL of hydrobromic acid until all the solution is dissolved, so as to prepare a third precursor solution;
(4) 1mL of the second precursor solution is added into a 20mL reaction bottle, and is vigorously stirred at the speed of 1200 revolutions per minute, then 75uL of the first precursor solution is quickly injected into the reaction bottle filled with the second precursor solution within 5 seconds, 100uL of isopropanol is injected after 30 seconds of reaction for continuous reaction for 60 seconds, then 0.5uL of the third precursor solution (the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 is 1:40) is added, the reaction is continued for 30 minutes, and finally 3mL of ethyl acetate is injected into the reaction solution, and the obtained crude solution is centrifuged to obtain the Ni-Br passivated CsPbBr 3 nanosheets.
Example 2
This example differs from example 1 in that 2uL of the third precursor solution was added, and the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 was 1:10.
Example 3
This example differs from example 1 in that 3.5uL of the third precursor solution was added, the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 being 1:5.7.
Example 4
This example differs from example 1 in that 5uL of the third precursor solution was added, and the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 was 1:4.
Example 5
This example differs from example 1 in that 6.5uL of the third precursor solution was added, the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 being 1:3.1.
Comparative example 1
A preparation method of CsPbBr 3 nano-sheets comprises the following steps:
(1) Dissolving 0.04mmol Cs 2CO3 in 2mL octanoic acid, and performing ultrasonic treatment until the Cs 2CO3 are completely dissolved to prepare a required precursor solution;
(2) Dissolving 0.2mmol of PbBr 2 in 8mL of toluene, adding 1mL of oleic acid and 1mL of oleylamine, and performing ultrasonic dissolution until the solution is transparent to prepare a required precursor solution;
(3) 1mL of the solution in the step (2) is added into a 20mL reaction bottle and is vigorously stirred, 75uL of the solution in the step (1) is rapidly injected, 100uL of isopropanol is injected for continuous reaction for 60s after reaction for 30s, 3mL of ethyl acetate is injected into the reaction solution, and the obtained crude solution is centrifuged to obtain CsPbBr 3 nano-sheets (namely original CsPbBr 3 nano-sheets).
Product effect test
1. Fluorescence properties and morphology
As shown in FIG. 1, the luminescent intensities of the CsPbBr 3 nano-sheets prepared in examples 1-5 are higher than those of the nano-sheets prepared in comparative example 1, and the crystal structure is the same as that of comparative example 1, and the cubic phase crystal structure is still maintained. The fluorescence quantum yields of examples 1-5 and comparative example 1 were 56.2%, 63.4%, 78%, 66%, 55.5%, 33.2%, respectively, wherein the luminescence intensity of the CsPbBr 3 nanoplatelets prepared in example 3 was optimal, and the fluorescence quantum yield reached 78%. In addition, the passivated CsPbBr 3 nano-sheets prepared in the embodiments 1-5 of the invention show higher fluorescence emission characteristics compared with the comparative example 1, which shows that the defects of the CsPbBr 3 nano-sheets are effectively passivated, the half-peak width is smaller, and the color purity is higher. In FIG. 1, the Intensity is the Intensity, and the Wavelength is the Wavelength.
From fig. 2, it is apparent that the morphology, size and size of the CsPbBr 3 nano-sheet prepared in comparative example 1 are not uniform.
As is apparent from fig. 3, the morphology of the CsPbBr 3 nanoplatelets prepared in example 5 of the present invention, the nanoplatelets prepared in example 5 demonstrate better dimensional uniformity than the nanoplatelets prepared in comparative example 1 of fig. 2.
From fig. 4, it can be seen that the lateral dimension of the CsPbBr 3 nano-sheet prepared in example 3 is smaller (about 3 nm) than the exciton bohr radius (7 nm) of CsPbBr 3 nano-crystal, which is also the reason that the CsPbBr 3 nano-sheet prepared in the invention can better realize blue light emission.
From fig. 5, it can be seen that the Ni-Br passivation strategy of the present invention does not change the crystal structure of CsPbBr 3 nanoplatelets, while Ni 2+, which is also demonstrated by the corresponding shift of the crystal planes toward high angles, successfully replaces part of Pb 2+. In FIG. 5, the Intensity is the Intensity, the diffraction angle is 2. Theta. And the degree is the degree.
2. Stability test
(1) Test method
Dispersing the CsPbBr 3 nano-sheets prepared in the above in toluene, storing in a transparent glass bottle, placing the glass bottle in air without special protection, and performing spectrum measurement by using a spectrometer at different days.
(2) Test results
The results show that the CsPbBr 3 nano-sheets obtained by the reaction in example 3 show excellent stability when dispersed in a solution, and can maintain the emission intensity of not less than 86.3% after being stored at room temperature for 30 days (the initial emission intensity of the CsPbBr 3 nano-sheets is considered to be 100%, and the intensity generally gradually decreases with the time), so that the CsPbBr 3 nano-sheets can be stored for a long time.

Claims (3)

1. The preparation method of the CsPbBr 3 nano sheet is characterized by comprising the following steps of:
(1) Dissolving 0.04mmol of Cs 2CO3 in 2mL of octanoic acid, and performing ultrasonic treatment until the powder is completely dissolved to prepare a first precursor solution;
(2) Dissolving 0.2mmol of PbBr 2 in 8mL of toluene, adding 1mL of oleic acid and 1mL of oleylamine, performing ultrasonic dissolution until all powder is dissolved, and preparing a second precursor solution;
(3) Dissolving 0.2mmol of NiBr 2 in 0.2mL of hydrobromic acid until all the solution is dissolved, so as to prepare a third precursor solution;
(4) 1mL of the second precursor solution is taken and added into a 20mL reaction bottle, and is vigorously stirred at a speed of 1200 revolutions per minute, then 75uL of the first precursor solution is quickly injected into the reaction bottle filled with the second precursor solution within 5 seconds, 100uL of isopropanol is injected for continuous reaction for 60 seconds after 30 seconds, 3.5uL of the third precursor solution is added, and the molar ratio of Ni element in NiBr 2 to Pb element in PbBr 2 is 1: and 5.7, continuing to react for 30 minutes, finally injecting 3mL of ethyl acetate into the reaction solution, and centrifuging the obtained crude solution to obtain the Ni-Br passivated CsPbBr 3 nano-sheet.
2. The CsPbBr 3 nano-sheet prepared by the preparation method of claim 1, wherein the fluorescence quantum yield of the CsPbBr 3 nano-sheet is more than or equal to 40%.
3. Use of the CsPbBr 3 nanoplatelet of claim 1 in the field of display, lighting or solar cells.
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