CN112358875A - Water-stable all-inorganic lead-halogen perovskite luminescent material and preparation method thereof - Google Patents

Water-stable all-inorganic lead-halogen perovskite luminescent material and preparation method thereof Download PDF

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CN112358875A
CN112358875A CN202011379978.5A CN202011379978A CN112358875A CN 112358875 A CN112358875 A CN 112358875A CN 202011379978 A CN202011379978 A CN 202011379978A CN 112358875 A CN112358875 A CN 112358875A
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谢毅
董浩
胡永飞
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Wuhan University of Technology WUT
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Abstract

The invention discloses a water-stable all-inorganic lead-halogen perovskite luminescent material, which is prepared by firstly adding a Pb-based precursor into an alcoholic solution of Cs salt for stirring reaction; then naturally drying the obtained mixed solution, grinding, adding the obtained powder into water, soaking and drying to obtain the product. According to the invention, the perovskite @ PbBr (OH) core-shell structure is adopted and the solvent evaporation and bubble water treatment process is further combined, so that the perovskite-based core-shell structure luminescent material has excellent stability in water, is expected to be applied to the fields of LED luminescent devices, fluorescent solar collectors and the like, and the related preparation method is simple, mild in reaction condition, convenient to operate, environment-friendly and suitable for popularization and application.

Description

Water-stable all-inorganic lead-halogen perovskite luminescent material and preparation method thereof
Technical Field
The invention belongs to the technical field of semiconductor nano material preparation and LED (light-emitting diode) luminescence application, and particularly relates to a water-stable all-inorganic lead-halogen perovskite luminescent material with enhanced fluorescence after soaking in water, and a preparation method and application thereof.
Background
The all-inorganic lead-halogen perovskite luminescent material becomes a research hotspot of a novel luminescent material due to the advantages of excellent luminescent performance, adjustable luminescent wavelength, narrower full width at half maximum of a fluorescence peak and the like. However, the poor stability of perovskite materials limits their practical applications. Perovskite is an ionic crystal, and the instability of the perovskite is mainly caused by the instability of the perovskite structure and the instability caused by the degradation of the perovskite by the environment.
Under an ideal state, the perovskite crystal belongs to a cubic crystal system, but lead halide octahedron arrangement is skewed due to various reasons, so that the symmetry of crystal lattices is reduced, orthogonal and rhombic crystal lattices are formed, and the uncontrollable octahedron distortion brings difficulties to practical application; the surface of the perovskite is unstable, which is mainly shown in that the ligand is easy to fall off and lose, and when the perovskite quantum dot is contacted with a polar solvent, the optical performance and the colloidal stability of the perovskite quantum dot are often lost, even the structural integrity of the perovskite quantum dot is damaged. It is well known that perovskites degrade rapidly on exposure to air due to the water oxygen sensitivity of the perovskite material, and while inert atmospheres can slow the degradation of perovskites, in practical applications, such as outdoor LEDs, they must operate in a real atmosphere. Therefore, environmental stability of perovskite materials is a concern.
At this stage, in order to solve the instability problem of perovskite materials, common methods include: the structural stability of the perovskite is improved through ion doping; surface modification is carried out, so that the surface stability of the perovskite is improved; the perovskite material is coated and packaged, and the environmental stability of the perovskite is improved. Patent CN 108504356 a discloses a manganese-doped inorganic halogen perovskite quantum dot, which greatly improves the thermal stability of the quantum dot and reduces the toxicity of lead halogen perovskite by manganese ion doping. Patent CN 111139059a discloses a method for improving the performance of perovskite quantum dots by short-chain alkyl carboxylic acid, which utilizes short-chain alkyl carboxylic acid to perform surface passivation on perovskite quantum dots to make the prepared quantum dots more stable and have better photoluminescence and electroluminescence performances. Patent CN 110511753A discloses a preparation method of a high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped chlorine lead cesium coated by silicon dioxide, and the prepared high-stability orange-red Mn2+-CsPbCl3/SiO2Luminescent materialThe perovskite white light LED is further manufactured by combining green fluorescent powder, and stable white light emission is realized. Liu Star team of Chinese academy of sciences (Liu Z, Zhang Y, Fan Y, Chen Z, Tang Z, Zhao J, lv Y, Lin J, Guo X, Zhang J, Liu X. Toward high project luminescence and Stabilized silicon-Coated Perovskite quant Dots through silicon Mixing and standing under Rom Temperature in Air [ J Z, Zhang Y, Lin J, Guo X, Zhang J, Liu X].ACS Applied Materials&The interface, 2018,10(15): 13053-13061) adopts an improved ligand-assisted reprecipitation method to synthesize the silica-coated perovskite quantum dot, and shows better environmental stability and thermal stability. However, the preparation conditions of the method are harsh, and the preparation process needs toxic ligands or high-temperature conditions, which does not meet the environment-friendly preparation requirements; on the other hand, although the above-mentioned production methods all improve the stability of perovskite luminescent materials to various degrees, improvements are still desired in terms of water resistance and the like.
Disclosure of Invention
The invention mainly aims to provide a water-stable all-inorganic lead-halogen perovskite luminescent material with enhanced fluorescence after water soaking, and the perovskite @ PbBr (OH) core-shell structure is designed and further combined with a solvent evaporation and water soaking treatment process, so that the obtained perovskite-based core-shell structure luminescent material has excellent stability in water, is expected to be applied to the fields of LED luminescent devices, fluorescent solar collectors and the like, and the related preparation method is simple, convenient to operate, environment-friendly and suitable for popularization and application.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a water-stable all-inorganic lead-halogen perovskite luminescent material comprises the following steps:
1) at room temperature, dissolving Cs salt in an alcohol solvent to obtain a uniform Cs salt solution; then adding a Pb-based precursor into the solution, and stirring the solution;
2) naturally drying the mixed solution (without luminescence characteristic) obtained in the step 1), and then grinding to obtain orange yellow powder;
3) and adding water into the obtained orange powder, uniformly stirring, soaking, drying and grinding to obtain the water-stable all-inorganic lead-halogen perovskite luminescent material (perovskite-based core-shell structure luminescent material).
In the scheme, the alcohol solvent is methanol, ethanol, n-propanol or isopropanol.
In the above scheme, the Cs salt is Cs2CO3Or CsBr, wherein the concentration range of the introduced Cs ions in the alcohol is 0.67-40 mmol/L.
In the scheme, the Pb precursor in the step 1) is PbBr2And the molar ratio of the introduced Pb element to the introduced Cs element is (0.8-6): 1.
In the scheme, the stirring treatment time is 1-4 h.
In the scheme, the drying temperature adopted in the steps 2) and 3) is room temperature.
In the scheme, the water adding amount in the step 3) is preferably larger than that of the powder.
In the scheme, the water soaking time is more than 30 min.
The water-stable all-inorganic lead-halogen perovskite luminescent material prepared according to the scheme can still keep excellent luminescence stability under the condition of long-term exposure in water; the method can be applied to the fields of LED luminescent devices, fluorescent solar collectors and the like.
The invention provides a simple, novel and environment-friendly preparation method of a perovskite-based luminescent material, which takes alcohol as a reaction solvent, adopts an evaporation solvent method to promote the reaction between a Cs salt and a Pb-based precursor, and then carries out water soaking treatment to further promote single-phase CsPb and Pb2Br5Formation of luminescent material and PbBr (OH) shell in CsPb2Br5The phase surface is coated, so that the composite perovskite material can still keep excellent luminescence stability after being exposed in water for a long time.
Compared with the prior art, the invention has the beneficial effects that:
1) the reaction for preparing the perovskite-based core-shell structure luminescent material is carried out at room temperature and in an air environment, inert gas protection and complex experimental operation are not needed, and the method is easy to realize and simple and convenient to operate;
2) the perovskite-based core-shell structure luminescent material is prepared in an alcohol solvent without ligand assistance, and the reaction system is non-toxic and environment-friendly;
3) the perovskite-based core-shell structure luminescent material provided by the invention has excellent stability in air and even in water, provides a new idea for the research of high-stability perovskite, and has wide application prospects in the field of luminescent devices such as LEDs and the like.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) image of a perovskite-based core-shell structure luminescent material prepared in example 1.
Fig. 2 is a transmission electron microscope (HRTEM) image of the perovskite-based core-shell structure luminescent material prepared in example 1.
FIG. 3 is an X-ray diffraction (XRD) pattern of the perovskite-based core-shell structure luminescent material prepared in example 1 before being soaked in water for treatment.
FIG. 4 is an X-ray diffraction (XRD) pattern of the perovskite-based core-shell structure luminescent material prepared in example 1 after being treated by soaking in water.
FIG. 5 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 1.
FIG. 6 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 2.
FIG. 7 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 3.
FIG. 8 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 4.
FIG. 9 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 5.
FIG. 10 is a PL spectrum before and after soaking in water of the perovskite-based core-shell structure luminescent material prepared in example 6.
FIG. 11 is a PL spectrum of a perovskite-based core-shell structure luminescent material prepared in example 7 before and after soaking in water.
Detailed Description
In order to better understand the present invention, the following embodiments are further illustrated, but the present invention is not limited to the following embodiments.
Example 1
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3In a small 20mL beaker, 5mL of ethanol was pipetted into the beaker using a pipette gun, and the mixture was stirred well for 2h until Cs was present2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution (without luminescence characteristic) obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) and adding 5mL of water into the obtained orange powder, stirring and soaking for 7 days, naturally drying at room temperature, and grinding to obtain a yellow powder material with green luminescence.
The Transmission Electron Microscope (TEM), high resolution TEM (hrtem), and X-ray diffraction (XRD) results of the non-foamed powder material obtained in this example are shown in fig. 1 to 3, respectively. As can be seen from FIG. 1, the obtained nanoparticles have uniform size and an average particle diameter of 50-80 nm; as can be seen from fig. 2, the nanoparticles have a coating characteristic; XRD analysis in FIG. 3 shows that the diffraction peak of XRD of the sample without bubble water treatment contains PbBr (OH), CsPb2Br5、CsPbBr3And Cs4PbBr6And (4) phase(s).
The X-ray diffraction analysis result of the product after bubble water treatment obtained in this example is shown in FIG. 4, which shows that the XRD diffraction peak of the final product after bubble water treatment is CsPb-free2Br5And PbBr (OH) phase, with no other peaks, wherein the diffraction peaks at 16.66 ° and 24.03 ° respectively correspond to CsPb2Br5(002), (202) crystal plane (CsPb) of phase2Br5JCPDS No. 00-025-; diffraction peaks at 21.45 °, 26.48 °, 33.91 ° and 34.68 ° corresponding to (120), (111), (211), (031) crystal planes of pbbr (oh) phase (pbbr (oh)), JCPDS No. 00-030-; show the soaking water treatment toolThe process can simultaneously promote the further reaction of the system to generate single-phase CsPb2Br5A luminescent material.
FIG. 5 is a graph showing fluorescence spectra (PL) of powder samples before and after the soaking treatment obtained in this example under excitation of a 365nm ultraviolet lamp, and the results show that the PL peak positions of the samples before and after soaking are all about 519nm, and the full width at half maximum is about 20nm, but the PL intensity of the samples after soaking is improved by about 6 times as compared with the PL intensity of the samples before soaking.
As can be seen from the above, the crystal structure and CsPb of the final product obtained in this example2Br5Corresponding to PbBr (OH), is coated with CsPb by PbBr (OH)2Br5The core-shell structure green luminescent material.
Example 2
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3In a small 20mL beaker, 5mL of methanol was pipetted into the beaker using a pipette gun and stirred well for 2h until Cs2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for reaction for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) and adding 5mL of water into the obtained orange powder, stirring and soaking for 7 days, naturally drying at room temperature, and grinding to obtain a yellow powder material with green luminescence.
The PL spectrum of the sample before and after soaking in water obtained in this example under 365nm excitation is shown in FIG. 6. As can be seen from FIG. 6, the PL peak positions of the samples before and after soaking in water are all around 520nm, the full width at half maximum is about 20nm, and there is no obvious difference before and after soaking in water, but the PL intensity of the samples after soaking in water is greatly improved compared with that of the original samples, which shows that the fluorescence-enhanced green luminescent material with high stability in water environment can be obtained by using methanol instead of ethanol.
Example 3
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3In a small 20mL beaker, 5mL of isopropanol was pipetted into the beaker using a pipette gun and stirred well for 2h until Cs2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) and adding 5mL of water into the obtained orange powder, stirring and soaking for 7 days, naturally drying at room temperature, and grinding to obtain a yellow powder material with green luminescence.
The PL spectra of the samples obtained in this example before and after soaking in water under 365nm wavelength excitation were measured by the method described in example 1, and the results are shown in FIG. 7. The result shows that the PL peak positions of the samples before and after soaking in water are all about 521nm, the full width at half maximum is about 20nm, but the PL intensity of the samples after soaking in water is greatly improved compared with the PL intensity of the original samples, which shows that the invention can also obtain the fluorescence-enhanced green luminescent material with high stability in the water environment by using isopropanol to replace ethanol.
Example 4
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3In a small 20mL beaker, 10mL of ethanol was pipetted into the beaker using a pipette gun, and the mixture was stirred well for 2h until Cs was present2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) and adding 5mL of water into the obtained orange powder, stirring and soaking for 7 days, naturally drying at room temperature, and grinding to obtain a yellow powder material with green luminescence.
The PL spectra of the samples obtained in this example before and after soaking in water under 365nm wavelength excitation were measured by the method described in example 1, and the results are shown in FIG. 8. The result shows that the PL peak positions of the samples before and after soaking in water are all about 521nm, the full width at half maximum is about 20nm, but the PL intensity of the samples after soaking in water is improved by about 5 times compared with the PL intensity of the original samples, and the product has higher stability in a water environment.
Example 5
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3In a small 20mL beaker, 5mL of ethanol was pipetted into the beaker using a pipette gun, and the mixture was stirred well for 2h until Cs was present2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) and adding 5mL of water into the obtained orange powder, stirring and soaking for 30min, naturally drying at room temperature, and grinding to obtain a green luminous yellow powder material.
The PL spectra of the samples obtained in this example before and after soaking in water under 365nm wavelength excitation were measured by the method described in example 1, and the results are shown in FIG. 9. The result shows that the PL peak positions of the samples before and after soaking in water are all about 520nm, and the full width at half maximum is about 20nm, but the PL intensity of the samples after soaking in water is greatly improved compared with the PL intensity of the original samples, which shows that the powder sample obtained by the invention can obtain the fluorescence-enhanced green luminescent material with high stability in the water environment even if the stirring time for soaking in water is only 30 min.
Example 6
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) weighing 11mg of Cs at room temperature using an electronic balance2CO3In a 20mL small beaker, and 100mL of ethanol was pipetted using a pipetteStirring thoroughly in the beaker for 2h until Cs2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) to the resulting orange-yellow powder was added 5mL of water, stirred and soaked for 7 days, and then naturally dried at room temperature and ground to obtain a yellow powder material having green luminescence.
The PL spectra of the samples obtained in this example before and after soaking in water under 365nm wavelength excitation were measured by the method described in example 1, and the results are shown in FIG. 10. The result shows that the PL peak position of the sample before soaking in water is about 522nm, the full width at half maximum is about 20nm, but the PL intensity of the sample after soaking in water is greatly improved compared with the PL intensity of the original sample, and the PL peak position of the sample after soaking in water is about 518 nm. This shows that the powder sample obtained in the low concentration Cs salt alcoholic solution (concentration of Cs ion is 0.67mmol/L) can also obtain the green luminescent material with enhanced fluorescence and high stability in water environment.
Example 7
A water-stable all-inorganic lead-halogen perovskite luminescent material is prepared by the following steps:
1) weighing 33mg of Cs at room temperature using an electronic balance2CO3In a small 20mL beaker, 5mL of ethanol was pipetted into the beaker using a pipette gun, and the mixture was stirred well for 2h until Cs was present2CO3Completely dissolving to obtain a Cs salt solution; 69mg of PbBr were weighed on an electronic balance2Adding the powder into the obtained Cs salt solution, and fully stirring for 2 hours;
2) naturally drying the mixed solution obtained in the step 1) for 48 hours, and grinding to obtain orange yellow powder;
3) to the resulting orange-yellow powder was added 5mL of water, stirred and soaked for 7 days, and then naturally dried at room temperature and ground to obtain a yellow powder material having green luminescence.
The PL spectra of the samples obtained in this example before and after soaking in water under 365nm wavelength excitation were measured by the method described in example 1, and the results are shown in FIG. 11. The result shows that the PL peak positions of the samples before soaking in water are all about 517nm, the full width at half maximum is about 20nm, the PL intensity of the samples after soaking in water is not much different from that of the original samples, but the PL peak positions of the samples after soaking in water are all about 513nm, the full width at half maximum is improved, and the effect is poor. This shows that the powder sample obtained in the higher concentration Cs salt alcoholic solution (the concentration of Cs ion is 40mmol/L) can obtain the green luminescent material which is stable in water environment.
Comparative example
With reference to the preparation method described in example 1, perovskite material was prepared by using conventional 1-octadecene as a solvent instead of an alcohol solvent, and the specific steps were as follows:
1) 22mg of Cs were weighed at room temperature using an electronic balance2CO3And 69mg of PbBr2Placing the powder in a small 20mL beaker, and using a pipette to pipette 5mL ODE (1-octadecene) into the beaker, and stirring thoroughly for 2 h;
2) centrifuging the mixed solution obtained in the step 1) for 5min at 6000rad/min (octadecene is an oil solvent, and only can be centrifuged to remove supernatant and then dried) to obtain precipitate, naturally drying for 48h, and grinding to obtain orange yellow powder;
3) to the resulting orange-yellow powder was added 5mL of water, stirred and soaked for 7 days, then naturally dried at room temperature and ground to obtain a white powder material.
Through the test: the yellow powder obtained in the step 2) has weak green fluorescence under the excitation of 365nm wavelength, but the fluorescence disappears after contacting with water, and the white powder material obtained in the step 3) has no fluorescence under the excitation of 365nm wavelength; this indicates that the yellow perovskite powder obtained in step 2) is water-free.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (8)

1. A preparation method of a water-stable all-inorganic lead-halogen perovskite luminescent material is characterized by comprising the following steps:
1) at room temperature, dissolving Cs salt in an alcohol solvent to obtain a uniform Cs salt solution; then adding a Pb-based precursor into the solution, and carrying out stirring reaction;
2) naturally drying the mixed solution obtained in the step 1), and then grinding to obtain orange yellow powder;
3) and adding water into the obtained orange powder, uniformly stirring, soaking, drying and grinding to obtain the water-stable all-inorganic lead-halogen perovskite luminescent material.
2. The method according to claim 1, wherein the alcohol solvent is methanol, ethanol, n-propanol or isopropanol.
3. The method of claim 1, wherein the Cs salt is Cs2CO3Or CsBr, wherein the concentration range of the introduced Cs ions in the alcohol is 0.67-40 mmol/L.
4. The method according to claim 1, wherein the Pb precursor in step 1) is PbBr2And the molar ratio of the introduced Pb element to the introduced Cs element is (0.8-6): 1.
5. The preparation method according to claim 1, wherein the stirring treatment reaction is carried out for 1 to 4 hours.
6. The method according to claim 1, wherein the drying temperature used in the steps 2) and 3) is room temperature.
7. The method according to claim 1, wherein the soaking time is 30min or more.
8. The water-stable all-inorganic lead-halogen perovskite luminescent material prepared by the preparation method of any one of claims 1 to 7.
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CN113173596A (en) * 2021-04-26 2021-07-27 齐鲁工业大学 High-stability random laser scattering material based on three-dimensional perovskite nanocrystalline, laser device and preparation method of laser device
CN113173596B (en) * 2021-04-26 2023-01-31 齐鲁工业大学 High-stability random laser scattering material based on three-dimensional perovskite nanocrystalline, laser device and preparation method of laser device
WO2022232229A1 (en) * 2021-04-27 2022-11-03 University Of Kentucky Research Foundation Dual-color cspbbr3 nanocrystals prepared by water
CN113480996A (en) * 2021-08-13 2021-10-08 河北工业大学 Crystalline state hydroxide coated perovskite nanocrystalline and preparation method and application thereof
CN115521784A (en) * 2022-09-30 2022-12-27 昆明理工大学 Water-stable all-inorganic perovskite quantum dot material and preparation method thereof
CN115537196A (en) * 2022-10-08 2022-12-30 武汉理工大学 High-stability perovskite material and preparation method and application thereof

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