CN114455837A - Perovskite quantum dot glass and preparation method and application thereof - Google Patents

Perovskite quantum dot glass and preparation method and application thereof Download PDF

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CN114455837A
CN114455837A CN202210220318.5A CN202210220318A CN114455837A CN 114455837 A CN114455837 A CN 114455837A CN 202210220318 A CN202210220318 A CN 202210220318A CN 114455837 A CN114455837 A CN 114455837A
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quantum dot
glass
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董敬一
郑策
张健
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Wuxi Utmolight Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00Compositions for glass with special properties
    • C03C4/12Compositions for glass with special properties for luminescent glass; for fluorescent glass
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/16Halogen containing crystalline phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material

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Abstract

The invention belongs to the field of solid luminescent materials, and particularly relates to perovskite quantum dot glass and a preparation method and application thereof. In addition, the annealing step and the high-temperature melting step are carried out in the same closed container, so that the rapid change of the temperature and the shape of the glass melt can be avoided, the thermal stress of the glass is reduced, the product yield is improved, the process operation is simpler and more convenient, the production repeatability is better, and the heat energy of the annealing step is saved, so that the preparation method disclosed by the invention can be suitable for industrial large-scale production.

Description

Perovskite quantum dot glass and preparation method and application thereof
Technical Field
The invention belongs to the field of solid luminescent materials, and particularly relates to a preparation method of perovskite quantum dot glass capable of improving the size uniformity of quantum dots.
Background
All-inorganic CsPbX3In recent years, perovskite quantum dots (X ═ Cl, Br, I) have attracted much attention because of their advantages of high quantum efficiency, tunable wavelength, simple synthesis method, high reproducibility, and the like. The perovskite quantum dots show wide application prospects in the fields of panel display, illumination, medical X-ray detection imaging, solar cells and the like. However, the perovskite quantum dots have poor stability and are extremely sensitive to moisture and high-temperature environments, so that the application of the perovskite quantum dots is severely limited.
Although many process strategies for stabilizing the perovskite quantum dots have been developed at present, from the feasibility point of view, the method of protecting the perovskite luminescent material in an all-around dead angle-free manner by using the shell coating most probably breaks through the bottleneck of the stability of the perovskite material, and promotes the commercialization of the perovskite quantum dots. In many perovskite quantum dot coating methods, the perovskite quantum dot is embedded in the glass to form the compound with low cost (the raw material is mostly SiO)2,B2O3The oxides are low in price) and high in stability (the compact network structure of the glass can effectively isolate quantum dots from the external environment, and the luminescent property has high stability), and the method is an advanced method at present.
At present, the preparation of quantum dot glass mainly adopts a high-temperature melting heating annealing treatment method to enable all-inorganic halide perovskite quantum dots to grow in situ in the glass. The conventional operation method comprises the following steps: uniformly mixing precursor material powder of perovskite and glass, melting at the high temperature of more than 1000 ℃ for 8-10min, pouring the molten mixture on a mould, cooling to obtain preformed glass, and annealing the preformed glass at the temperature of 400-600 ℃ to separate out perovskite crystals to obtain the microcrystalline glass coated with the perovskite quantum dots. The treated perovskite microcrystalline glass has excellent luminescence property, better physical and chemical stability, can effectively prevent the erosion of oxygen and water in the air, and has no any attenuation after being subjected to dry heating at 85 ℃ and water soaking. However, in the high-temperature melting process of the method, the perovskite precursor is volatilized continuously after reaching the boiling point, so that the concentration difference of the upper perovskite material and the lower perovskite material of the molten glass is large, and the components of the perovskite glass are not uniform; meanwhile, in order to avoid excessive volatilization of raw materials such as Cs, Pb, halogen and the like, the glass raw materials must be put in at high temperature and taken out at high temperature, and the glass raw materials cannot stay for more than 10 minutes at high temperature, which can cause incomplete melting of the glass raw materials. The uniformity of the quantum dot glass ceramics can be influenced by insufficient melting of glass raw materials and volatilization of precursor materials, and the quantum efficiency of the quantum dot glass can be reduced and the half-peak width can be widened due to the existence of dilution effect, quantum dot/glass interface defects and intrinsic defects (vacancies/interstitials and the like) in the inhomogeneous quantum dot glass. In addition, the volatilized materials such as Pb and halogen cause environmental pollution and waste of raw materials. In addition, cooling the molten mixture by pouring it onto a mold can subject the glass to drastic temperature and shape changes during the forming process, leaving thermal stresses in the glass that affect the compactness and stability of the glass envelope. The existing process is complex, parameters are difficult to control, product repeatability is poor, and yield is low.
To this end, the prior art discloses a method for promoting crystallization of all-inorganic perovskite quantum dots in glass by adding fluoride to the raw materials, which utilizes fluoride to break the silicon-oxygen bonds in the glass to facilitate uniform distribution of the perovskite quantum dots in the glass. However, the method cannot fundamentally solve the problems of volatilization of the perovskite raw material and stress caused by rapid cooling of the glass on a mold.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems of non-controllable volatilization of raw materials and non-uniform size of quantum dots and low product yield caused by residual thermal stress of glass in the preparation process of the conventional perovskite quantum dot glass.
The purpose of the invention is realized by the following technical scheme:
on one hand, the invention provides a preparation method of perovskite quantum dot glass, which comprises the following steps:
s1, uniformly mixing the glass raw material and the quantum dot precursor raw material, and fully grinding;
s2, placing the ground raw material mixture into a closed cavity, controlling the temperature in the closed cavity to be 1100-1200 ℃ and the pressure to be 0.1-10MPa, and keeping the temperature and the pressure for 15-30 min;
s3, reducing the temperature in the closed cavity to 300-600 ℃, and annealing for 2-8 hours.
Preferably, in step S2, the pressure in the sealed chamber is controlled to be 2 to 8 MPa.
Preferably, in step S2, the pressure in the closed chamber is controlled to be 5 MPa.
Optionally, in step S2, the temperature is increased at a rate of 1-10 deg.C/min, preferably 5 deg.C/min.
Optionally, in step S2, the ground raw material mixture is placed in a sealed chamber, and then heated to 200-300 ℃ at a rate of 2-15 ℃/min (preferably 10 ℃/min), and then the temperature is maintained and vacuumized, and then heated to 1100-1200 ℃.
Preferably, in step S3, the annealing temperature is 500-550 ℃ and the annealing time is 4-8 h.
Optionally, in step S1, the quantum dot precursor raw materials are a cesium source compound, a lead source compound and a halogen compound, and a molar ratio of the cesium source compound, the lead source compound and the halogen compound is 2:1 (1-3).
Optionally, in step S1, the molar ratio of the quantum dot precursor raw material to the glass raw material is 1 (3-10).
Optionally, the method further comprises a step S4, wherein the perovskite quantum dot glass prepared in the step S3 is ground, sieved, ball-milled and dried to obtain glass powder with the particle size of 5-7 μm.
Alternatively, the furnaces that may provide a closed chamber include, but are not limited to, hot isostatic pressing furnaces, tube furnaces, atmospheric muffle furnaces, glass kilns, pressure vessels, and the like, high temperature-resistant, pressure-regulated, closed furnaces.
On the other hand, the invention also provides perovskite quantum dot glass prepared by the preparation method.
In a third aspect, the invention also provides application of the perovskite quantum dot glass, wherein the application comprises the application of the perovskite quantum dot glass prepared by the invention in photoelectric products.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. according to the preparation method provided by the embodiment of the invention, the perovskite quantum dot glass is prepared by adopting the high-temperature resistant closed container with adjustable pressure, the boiling point of the quantum dot precursor raw material can be improved by higher pressure, the volatilization of the raw material is reduced, and the closed environment is added, so that the volatilization of the quantum dot precursor raw material can be effectively controlled fundamentally, the uniformity of the size of the quantum dots in the glass is greatly improved, and the prepared perovskite quantum dot glass has narrower half-peak width and higher quantum efficiency, and the raw material and the environment can not be wasted. In addition, the annealing step and the high-temperature melting step are carried out in the same closed container, so that the rapid change of the temperature and the shape of the glass melt can be avoided, the thermal stress of the glass is reduced, and the product yield is improved.
2. The preparation method provided by the embodiment of the invention has wide raw material selection range, the applicable glass substrate can be any kind of inorganic glass, such as borosilicate glass, tellurate glass, phosphate glass, germanate glass, silicate glass, silicon-germanate glass, aluminosilicate glass and the like, and the halogen in the perovskite quantum dots can be any one or the mixture of at least two of Cl, Br and I (namely CsPbCl)xBryI3-x-yX is more than or equal to 0 and less than or equal to 3, y is more than or equal to 0 and less than or equal to 3, and x + y is more than or equal to 0 and less than or equal to 3), and the halogen is doped in any proportion to adjust the light-emitting wavelength, so that the perovskite quantum dot glass prepared by the method can emit light within the range of 400-700 nm.
3. According to the preparation method provided by the embodiment of the invention, the annealing and melting steps are carried out in the same closed container, the molten mixture does not need to be poured on a mould, and the additional heating and annealing are also not needed, so that the process operation is simpler and more convenient, the production repeatability is better, and the heat energy of the annealing step can be saved, so that the preparation method provided by the invention is more suitable for industrial large-scale production.
4. The half-peak width of the perovskite quantum dot glass prepared by the embodiment of the invention can be 25nm, the quantum efficiency can reach 45%, and the performance of the perovskite quantum dot glass is far superior to that of the perovskite quantum dot glass prepared by the prior art (the half-peak width is 35nm, and the quantum efficiency is 15%).
Drawings
FIG. 1 shows CsPbBr prepared in example 13Scanning electron microscope pictures of perovskite quantum dot glass;
FIG. 2 shows CsPbBr prepared in example 13A steady state emission spectrum of the perovskite quantum dot glass;
FIG. 3 is CsPbBr prepared in example 31.2I1.8Steady state emission spectra of perovskite quantum dot glass.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The preparation method of the perovskite quantum dot glass provided by the invention comprises the following steps:
(1) accurately weighing various raw materials according to the composition of each sample, mixing the weighed solid powder, pouring the mixture into a corundum mortar, uniformly grinding the mixture, sieving the mixture by a sieve with the particle size of 50 mu m, and placing the sieved powder into a graphite (or corundum) crucible;
(2) placing the graphite crucible filled with the raw material powder in a hot isostatic pressing furnace, after ensuring good tightness, heating to 200-300 ℃ from room temperature at the speed of 2-15 ℃/min, preserving heat for 20min, simultaneously opening a vacuum pump to pump vacuum, removing water and oxygen in the raw material and air, and avoiding oxidation of the graphite crucible and raw material;
(3) closing the vacuum pump, heating to 1100-1200 ℃ from 200-300 ℃ at a speed of 1-10 ℃/min, preserving the heat for 15-30min, filling argon (or nitrogen) to control the pressure in the cavity to be constant at 0.1-10MPa, increasing the pressure to increase the boiling point of the raw material and reduce the volatilization of the raw material, wherein the specific pressure can be regulated and controlled by referring to the Clausis-Clapeylon equation;
(4) reducing the temperature to 300-600 ℃, and annealing for 2-8h (gas does not need to be filled in the annealing process) to obtain the microcrystalline glass with the perovskite quantum dots;
(5) crushing and grinding the perovskite microcrystalline glass, sieving the crushed perovskite microcrystalline glass with a 50-mesh sieve (the size of a sieve pore is 270 mu m), putting the sieved glass particles into an agate ball milling tank, adding grinding balls with different sizes (the number ratio of the grinding balls with the sizes of 10mm, 6mm and 3mm is 1: 2: 4), taking ethanol as a ball milling aid, carrying out ball milling for 50h, drying the mixture, and sieving the dried mixture with a 1000-mesh sieve (the size of the sieve pore is 13 mu m) to finally obtain glass powder with the granularity of about 5-7 mu m.
The invention creatively utilizes the closed chamber with controllable pressure and atmosphere to prepare the perovskite quantum dot glass, ensures the full melting of the glass components, effectively controls the volatilization of the raw materials, improves the uniformity of the size of the quantum dots in the glass, simultaneously reduces the residual stress in the glass to the maximum extent, and ensures the compactness and the uniformity of the microcrystalline glass shell.
Example 1: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
Glass matrix raw materials and quantum dot precursor raw materials are mixed according to the mol ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning 5-NaBr, accurately weighing the raw materials, pouring the weighed solid powder into a corundum mortar, uniformly grinding, screening the powder with the particle size of 50 mu m, and placing the screened powder into a graphite crucible. And (3) placing the graphite crucible with the sample in a hot isostatic pressing furnace, after ensuring good tightness, heating to 300 ℃ from room temperature at the speed of 10 ℃/min, preserving heat for 20min, and simultaneously opening a vacuum pump to vacuumize, so as to remove water and oxygen in the raw materials. And (3) closing the vacuum pump, heating to 1200 ℃ from 300 ℃ at the speed of 5 ℃/min, controlling the pressure in the cavity to be constant at 5MPa by filling argon, and preserving the heat for 20min to completely melt the raw materials. Then the temperature is reduced to 500 ℃ for annealing, crystallization is carried out for 4h, and the CsPbBr can be obtained after cooling to the room temperature3Perovskite quantum dot fluorescent glass. The perovskite quantum dots are made of phosphorCrushing and grinding the optical glass, sieving the optical glass by a 50-mesh sieve, putting the sieved glass particles into an agate ball milling tank, adding grinding balls with different sizes, ball milling for 50 hours by using ethanol as a ball milling auxiliary agent, drying and sieving the glass particles by a 1000-mesh sieve, wherein the particle size of the glass powder is about 6 mu m, the luminescence peak position is 520nm, the half-peak width is 25nm, and the quantum efficiency is 45%.
CsPbBr prepared in example 13The scanning electron microscope result of the perovskite quantum dot glass is shown in figure 1, and the steady state luminescence spectrum is shown in figure 2.
Example 2: green light CsPbBr3Preparation of perovskite quantum dot phosphate glass
According to the molar ratio of 56P2O5-10SiO2-10Cs2CO3-5PbBr2-6Sr2CO3-3Al2O3Proportioning the raw materials according to the proportion of-10 NaBr, setting the melting temperature to 1150 ℃ due to a slightly lower melting point of phosphate glass, preserving the temperature for 20min, and finally annealing at 500 ℃ for 4h, wherein other steps are consistent with those in the example 1. The granularity of the glass powder after ball milling is about 6 μm, the luminescence peak position is 522nm, the half-peak width is 24nm, and the quantum efficiency is 42%.
Example 3: red light CsPbBr1.2I1.8Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-2PbBr2-3PbI2Proportioning-2 NaBr-3NaI, keeping the melting temperature at 1200 ℃, keeping the temperature for 20min, and finally annealing at 530 ℃ for 4h, wherein other steps are consistent with those in the example 1. The particle size of the treated glass powder is about 6 μm, the luminescence peak position is 613nm, the half-peak width is 39nm, and the quantum efficiency is 38%.
CsPbBr prepared in example 31.2I1.8The steady state emission spectrum of the perovskite quantum dot borosilicate glass is shown in fig. 3.
Example 4: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning the materials with-5 NaBr, setting the melting temperature to be 1100 ℃, preserving the heat for 20min, and finally annealing at 500 ℃ for 4h, wherein other steps are consistent with those in the example 1. The granularity of the glass powder after ball milling is about 6 μm, the melting uniformity of the raw materials is slightly reduced due to the reduction of the high-temperature melting temperature, the raw materials are not completely and uniformly mixed, the luminous peak position is 522nm, the half-peak width is 28nm, and the quantum efficiency is 21%.
Example 5: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning the materials with-5 NaBr, setting the melting temperature to 1200 ℃, preserving the heat for 20min, and finally annealing at 550 ℃ for 4h, wherein other steps are consistent with those in the example 1. The particle size of the glass powder after ball milling is about 6 mu m, and as the annealing temperature is increased, the quantum dot material is separated out more quickly, so that the growth size of the perovskite quantum dot is larger, the light-emitting peak position is red-shifted to 527nm, the half-peak width is widened to 29nm, and the quantum efficiency is 41%.
Example 6: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning the materials with-5 NaBr, setting the melting temperature to be 1200 ℃, preserving the heat for 20min, and finally annealing at 500 ℃ for 8h, wherein other steps are consistent with those in the embodiment 1. The granularity of the glass powder after ball milling is about 6 mu m, and as the annealing time is prolonged and the quantum dots have more time to diffuse and separate out, the size of the generated quantum dots is larger, the luminous peak position is slightly red shifted to 524nm, the half-peak width is 25nm, and the quantum efficiency is 43%.
Example 7: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning the materials with-5 NaBr, setting the melting temperature to 1200 ℃, keeping the temperature for 8min, and finally annealing at 500 ℃ for 4h, wherein other steps are consistent with those in the example 1. After ball millingThe particle size of the glass powder is about 6 mu m, the raw materials are not completely and uniformly mixed due to too short high-temperature melting time, the size difference of the generated perovskite quantum dots is large, the luminescence peak position is 521nm, the half-peak width is 32nm, and the quantum efficiency is 26%.
Example 8: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr25NaBr, the pressure in the cavity during melting is set to be constant at 8MPa, and other steps are consistent with those in example 1. The granularity of the glass powder after ball milling is about 6 μm, the volatilization problem of the raw materials is controlled due to the improvement of the pressure during melting, the performance is excellent, the luminous peak position is 523nm, the half-peak width is 26nm, and the quantum efficiency is 44%.
Example 9: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
According to the molar ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr25NaBr, the pressure in the cavity during melting is set to be constant at 2MPa, and other steps are consistent with those in example 1. The granularity of the glass powder after ball milling is about 6 μm, the raw material has certain volatilization and performance reduction due to the reduction of the pressure during melting, the luminous peak position is 522nm, the half-peak width is 28nm, and the quantum efficiency is 35%.
Comparative example 1: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
Raw materials are mixed according to the mol ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning-5 NaBr, uniformly grinding, placing in a corundum crucible, then placing in a muffle furnace, melting for 8min at 1200 ℃, and pouring the melt into a brass mold to obtain a glass precursor; finally, heat treatment was carried out at 500 ℃ for 4 hours to induce CsPbBr3In-situ growth in glass matrix to obtain CsPbBr3Quantum dot glass.
Due to incomplete melting and uneven glass precursor, the quantum dots in different areas are different in precipitation difficulty degree, the glass is uneven, the luminous peak position is 525nm, the half-peak width is widened to 35nm, and the quantum efficiency of the treated glass powder is only 15%. In addition, residual thermal stresses in the glass are not effectively released due to the rapid cooling on the brass mold, and the glass precursor cracks during cooling.
Comparative example 2: green light CsPbBr3Preparation of perovskite quantum dot borosilicate glass
Raw materials are mixed according to the mol ratio of 30SiO2-30B2O3-20ZnO-10Cs2CO3-5PbBr2Proportioning 5NaBr, uniformly grinding, placing in a corundum crucible, placing in a muffle furnace, and melting at 1200 ℃ for 20min to obtain a uniform glass melt; then, pouring the melt into a brass mold to obtain a glass precursor; finally, heat treatment was carried out at 500 ℃ for 4 hours.
Although the raw materials are completely melted, the perovskite raw materials such as Cs, Pb, halogen and the like already emit light, so that perovskite quantum dots are not generated after annealing at 500 ℃, and the glass is colorless and transparent.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications derived therefrom are intended to be within the scope of the invention.

Claims (10)

1. A preparation method of perovskite quantum dot glass comprises the following steps:
s1, uniformly mixing the glass raw material and the quantum dot precursor raw material, and fully grinding;
s2, placing the ground raw material mixture into a closed cavity, controlling the temperature in the closed cavity to be 1100-1200 ℃ and the pressure to be 0.1-10MPa, and keeping the temperature and the pressure for 15-30 min;
s3, reducing the temperature in the closed cavity to 300-600 ℃, and annealing for 2-8 hours.
2. The method for preparing perovskite quantum dot glass according to claim 1, wherein in step S2, the pressure in the closed cavity is controlled to be 2-8 MPa.
3. The method for producing a perovskite quantum dot glass according to claim 1 or 2, wherein in step S2, the temperature is raised at a rate of 1 to 10 ℃/min, preferably 5 ℃/min.
4. The method for preparing perovskite quantum dot glass according to any one of claims 1 to 3, wherein in step S2, the ground raw material mixture is placed in a closed chamber, and then heated to 200 to 300 ℃ at a rate of 2 to 15 ℃/min, and then the temperature is maintained and vacuumized, and then heated to 1100 to 1200 ℃.
5. The method for producing a perovskite quantum dot glass according to any one of claims 1 to 4, wherein in step S3, the annealing temperature is 500 to 550 ℃ and the annealing time is 4 to 8 hours.
6. The method for producing a perovskite quantum dot glass according to any one of claims 1 to 5, wherein in step S1, the quantum dot precursor raw materials are a cesium source compound, a lead source compound and a halogen compound, and the molar ratio of the cesium source compound, the lead source compound and the halogen compound is 2:1 (1 to 3).
7. The method for producing a perovskite quantum dot glass according to any one of claims 1 to 6, wherein in step S1, the molar ratio of the quantum dot precursor raw material to the glass raw material is 1 (3-10).
8. The method for preparing perovskite quantum dot glass according to any one of claims 1 to 7, further comprising a step S4, wherein the perovskite quantum dot glass prepared in the step S3 is ground, sieved, ball-milled and dried to obtain glass powder with the particle size of 5-7 μm.
9. A perovskite quantum dot glass produced by the method for producing a perovskite quantum dot glass according to any one of claims 1 to 8.
10. Use of a perovskite quantum dot glass, comprising the use of a perovskite quantum dot glass according to claim 9 in an optoelectronic product.
CN202210220318.5A 2022-03-08 2022-03-08 Perovskite quantum dot glass and preparation method and application thereof Pending CN114455837A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115504673A (en) * 2022-09-27 2022-12-23 中国科学院上海光学精密机械研究所 CsPbBr 3 Quantum dot glass ceramic and preparation method thereof

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