CN115851263A - Perovskite quantum dot and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of luminescent materials, in particular to a perovskite quantum dot and a preparation method thereof. The preparation method of the perovskite quantum dot comprises the following steps: will contain CsPbX 3 Mixing the solution of the quantum dots with a thiol ligand, and carrying out ligand exchange reaction to obtain the perovskite quantum dots; the CsPbX 3 In the quantum dots, X is selected from at least one of Cl, br and I; the thiol-based ligand includes an alkyl thiol. According to the invention, ligand exchange is carried out on the perovskite quantum dots and the thiol ligand, so that the fluorescence quantum yield, the blue light stability and the thermal stability of the perovskite quantum dots are obviously improved, and the method has the advantages of simple steps and high repeatability.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a perovskite quantum dot and a preparation method thereof.
Background
All inorganic halides (CsPbX) 3 Wherein X = Cl, br or I) Perovskite Quantum Dots (PQDs) are widely used in the field of optoelectronics such as Photovoltaics (PV), light Emitting Diodes (LED), photodetectors and lasers due to their advantages of tunable direct band gap, high photoluminescence quantum yield (PLQY), high absorption coefficient, high defect tolerance, etc.
At present, colloidal CsPbX 3 The perovskite quantum dots are relatively easy to synthesize and adjust the components after synthesis, and the thermal injection method is commonly used for CsPbX 3 A method for synthesizing perovskite quantum dots. Generally, oleic Acid (OA) and Oleylamine (OLA) are used as ligands for surface passivation of perovskite quantum dots; however, it is difficult to stabilize ionic perovskite quantum dots due to the formation of weak surface bonds. For example, csPbBr emitting green light 3 Perovskite quantum dots, while capable of > 90% photoluminescence quantum yields, lack long-term colloidal stability and reproducibility, especially under temperature, humidity and light conditions. This is almost CsPbX 3 The widespread barrier of perovskite quantum dots and devices has severely hampered the practical and commercial application of perovskite optoelectronic devices.
A method of improving the stability of a perovskite quantum dot, comprising: improved synthesis processes, metal doping, passivation with different ligands, core-shell structures, and encapsulation in a polymer matrix, among others. Wherein, by the pair CsPbX 3 After the perovskite quantum dots are subjected to post-treatment, ligands such as tri-n-octylphosphine, thiocyanate, zwitterion, octylphosphonic acid, didodecyldimethylammonium bromide and the like are introduced, so that the perovskite quantum dots with the storage stability of hours or days at room temperature are obtained, but the perovskite quantum dots still do not have long-term stability under the conditions of temperature (such as high temperature) or illumination (especially blue light irradiation).
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of perovskite quantum dots, which improves the luminous efficiency and stability of the perovskite quantum dots, and greatly improves the fluorescence quantum yield, blue light stability and thermal stability of the perovskite quantum dots.
The second purpose of the invention is to provide a perovskite quantum dot which has excellent luminous efficiency and stability, the luminous efficiency is more than or equal to 99%, and the perovskite quantum dot still has long-term stability under high temperature or illumination conditions.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a preparation method of perovskite quantum dots, which comprises the following steps:
will contain CsPbX 3 Mixing the solution of the quantum dots with a thiol ligand, and carrying out ligand exchange reaction to obtain the perovskite quantum dots;
the CsPbX 3 In the quantum dots, X is selected from at least one of Cl, br and I;
the thiol-based ligand includes an alkyl thiol.
Further, the number of carbon atoms of the alkanethiol is 6 to 18.
Further, the alkyl mercaptan includes at least one of hexanethiol, octanethiol, nonanethiol, n-dodecylmercaptan, tetradecylthiol, hexadecylthiol, octadecanethiol, 1, 6-hexanedithiol, 1, 8-octanethiol, 1, 9-nonanedithiol and 1, 10-decanedithiol.
Further, the composition contains CsPbX 3 CsPbX in solution of quantum dots 3 The molar ratio of the quantum dots to the thiol ligands is 1:1 to 6.
Further, the temperature of the ligand exchange reaction is 20-25 ℃; the time of the ligand exchange reaction is 0.5 to 2 hours.
Further, the composition contains CsPbX 3 The preparation method of the solution of the quantum dots comprises the following steps:
heating and vacuumizing a mixture of cesium source, lead source, 1-octadecene and oleic acid, mixing with oleylamine halide precursor, and reacting to obtain the CsPbX-containing material 3 A solution of quantum dots.
Further, the cesium source includes at least one of cesium carbonate, cesium acetate, cesium chloride, cesium bromide, and cesium iodide.
Further, the lead source includes at least one of lead oxide, lead acetate, lead chloride, lead bromide, and lead iodide.
Further, a production method of the perovskite quantum dot includes at least one of the following features (1) to (2):
(1) The temperature of the heating treatment is 120-150 ℃;
(2) The reaction temperature is 220-260 ℃.
The invention also provides a perovskite quantum dot prepared by the preparation method of the perovskite quantum dot.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the perovskite quantum dot, the perovskite quantum dot with the luminous efficiency more than or equal to 99% and high stability can be obtained by carrying out ligand exchange reaction on the perovskite quantum dot and the thiol ligand, and the perovskite quantum dot still has long-term stability under the condition of facing temperature (such as high temperature) or illumination (especially blue light illumination); according to the invention, the post-treatment of the thiol surface ligand greatly improves the fluorescence quantum yield, blue light stability and thermal stability of the perovskite quantum dot, and the method has simple steps and high repeatability.
After the perovskite quantum dots are treated by the thiol ligand, the thiol ligand can generate thioether or thiolate through addition reaction, the thioether or thiolate is coordinated with lead atoms on the surfaces of the perovskite quantum dots, and the formation of metal lead particles is inhibited, so that the fluorescence quantum yield of the perovskite quantum dots is improved; in addition, the thioether or thiolate greatly enhances the binding force between the ligand and the perovskite quantum dot, so that the perovskite quantum dot has high stability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic diagram of a preparation method of a perovskite quantum dot of embodiment 1 of the present invention.
Fig. 2 is a graph showing the fluorescence efficiency of the perovskite quantum dots prepared in example 1 of the present invention and comparative example 1.
Fig. 3 is a graph comparing the blue light stability of the perovskite quantum dots prepared according to example 1 of the present invention and comparative example 1.
Fig. 4 is a graph comparing thermal stability of perovskite quantum dots prepared in example 1 of the present invention and comparative example 1.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are a part of the embodiments of the present invention, rather than all of the embodiments, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under 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.
The perovskite quantum dot and the preparation method thereof according to the embodiment of the invention are specifically described below.
In some embodiments of the present invention, there is provided a method for preparing a perovskite quantum dot, comprising the steps of:
will contain CsPbX 3 Mixing the solution of the quantum dots with a thiol ligand, and carrying out ligand exchange reaction to obtain perovskite quantum dots;
CsPbX 3 in the quantum dots, X is selected from at least one of Cl, br and I;
the thiol-based ligand includes an alkyl thiol.
The surface passivation with different ligands is to improve CsPbX 3 Perovskite quantum dot light emission and stability are one of the simple and effective methods. In particular, post-synthesis treatment, which is a surface ligand post-treatment of perovskite quantum dots, allows the modulation of surface chemistry without re-optimizing the synthesis conditions for each surface ligand.
According to the invention, the perovskite quantum dots with the luminous efficiency of more than or equal to 99% and high stability can be obtained by carrying out ligand exchange reaction on the perovskite quantum dots and the thiol ligands, the perovskite quantum dots still have long-term stability under the condition of high temperature or illumination, and the luminous efficiency, blue light stability and thermal stability of the perovskite quantum dots are obviously improved.
The thiol ligand can generate thioether or thiolate with oleic acid, oleylamine or octadecene through addition reaction, and the thioether or thiolate can be combined with uncoordinated lead atoms on the surface of the perovskite quantum dot on one hand to inhibit the formation of metal lead particles, so that the luminous efficiency is improved; on the other hand, the thioether or thiolate has stronger binding force relative to carboxylate, can replace the original carboxylic acid ligand on the surface of the quantum dot as a high-stability ligand, greatly enhances the binding force between the ligand and the perovskite quantum dot, and has high stability, thereby improving the blue light stability and the thermal stability of the perovskite quantum dot.
In some embodiments of the invention, the number of carbon atoms in the alkyl thiol is from 6 to 18. Preferably, the number of carbon atoms of the monofunctional alkyl thiol is from 6 to 18; the number of carbon atoms of the bifunctional alkylthiol is 6 to 10.
In some embodiments of the invention, the alkyl mercaptan comprises at least one of hexanethiol, octanethiol, nonanethiol, n-dodecylmercaptan, tetradecylthiol, hexadecylthiol, octadecanethiol, 1, 6-hexanedithiol, 1, 8-octanethiol, 1, 9-nonanedithiol, and 1, 10-decanedithiol.
The surface of the perovskite quantum dot can be better protected by adopting the mercaptan with a longer alkyl chain; if the alkyl chain length is too short, the perovskite quantum dots may be finally destroyed due to too strong polarity, so that the light emitting efficiency is poor. The bifunctional mercaptan can be better subjected to multidentate coordination with the surface of the perovskite quantum dot, so that the surface of the perovskite quantum dot is protected.
In some embodiments of the invention, csPbX is included 3 CsPbX in solution of quantum dots 3 The molar ratio of the quantum dots to the thiol ligands is 1:1 to 6; typically but not exclusively, containing CsPbX, for example 3 CsPbX in solution of quantum dots 3 The molar ratio of the quantum dots to the thiol ligands is 1: 1. 1: 2. 1: 3. 1: 4. 1:5 or 1:6, and so on.
In some embodiments of the invention, the temperature of the ligand exchange reaction is 20 to 25 ℃; the time of ligand exchange reaction is 0.5-2 h; typically, but not by way of limitation, the ligand exchange reaction is carried out for a period of time, for example, 0.5h, 1h, 1.5h, or 2h, and the like.
The ligand exchange reaction of the invention can be reacted by stirring for a period of time at room temperature, and has simple operation and strong repeatability.
In some embodiments of the invention, the ligand exchange reaction is followed by centrifugation. Preferably, centrifugal purification comprises centrifugation after addition of a solvent; more preferably, the solvent comprises n-hexane and/or ethyl acetate.
In some embodiments of the invention, csPbX is included 3 The preparation method of the solution of the quantum dots comprises the following steps:
heating and vacuumizing a mixture of cesium source, lead source, 1-Octadecene (ODE) and Oleic Acid (OA), mixing with oleylamine halide precursor, and reacting to obtain the compound containing CsPbX 3 A solution of quantum dots.
In some embodiments of the invention, the cesium source comprises cesium carbonate (Cs) 2 CO 3 ) At least one of cesium acetate, cesium chloride, cesium bromide and cesium iodide.
In some embodiments of the invention, the lead source comprises at least one of lead oxide (PbO), lead acetate, lead chloride, lead bromide, and lead iodide.
In some embodiments of the invention, the oleylamine halide comprises oleylamine chloride, oleylamine bromide or oleylamine iodide.
In some embodiments of the invention, the mixture of cesium source, lead source, 1-octadecene and oleic acid is subjected to a heat treatment at a temperature of 120 to 150 ℃; preferably 120 to 130 ℃; more preferably, the time of the heat treatment is 0.3 to 1 hour.
In some embodiments of the invention, csPbX is included 3 In the preparation method of the solution of the quantum dots, the reaction temperature is 220-260 ℃; preferably, the reaction temperature is 220-250 ℃; more preferably, the reaction time is 1 to 10min.
In some embodiments of the invention, a method of preparing an oleylamine halide precursor includes: heating and vacuumizing the mixture of oleylamine and halogen acid to obtain the product; preferably, the temperature of the heat treatment is 100 to 150 ℃.
According to the preparation method of the perovskite quantum dot, the perovskite quantum dot is processed by adopting a surface ligand post-processing process, so that the repeatability is high, the process is simple, the operation is easy, the cost is low, and the amplification is easy; and the fluorescence efficiency, the blue light stability and the thermal stability of the perovskite quantum dots are greatly improved.
The invention also provides a perovskite quantum dot which is prepared by the preparation method of the perovskite quantum dot.
In some embodiments of the invention, the perovskite quantum dots have a luminous efficiency of 99% or more.
Also provided in some embodiments of the present invention is an optical film, made primarily from the perovskite quantum dots described above.
In some embodiments of the invention, the optical film is prepared from perovskite quantum dots, UV glue and initiator. Preferably, the mass ratio of the UV glue to the initiator is 50-100: 1.
this is further illustrated below with reference to specific examples.
Example 1
Referring to fig. 1, the preparation method of the perovskite quantum dot provided in this embodiment includes the following steps:
(A) And (3) putting 10mL of oleylamine and 1.28mL of hydrobromic acid into a three-neck flask, then putting the three-neck flask into a heating jacket, heating, stirring, vacuumizing, heating to 120 ℃, and vacuumizing until no bubbles are generated in the three-neck flask, thereby obtaining the oleylamine bromine precursor.
(B) Adding cesium carbonate (0.0326 g and 0.1 mmoL), lead oxide (0.0446g and 0.2 mmoL), 1-octadecene (10 mL) and oleic acid (1 mL) into a three-neck flask, then putting the three-neck flask into a heating jacket, heating, stirring and vacuumizing at the stirring speed of 700rpm, heating to 120 ℃, keeping the temperature at 120 ℃ for 30min, heating to 240 ℃, quickly injecting 0.8mL of oleylamine bromide precursor by using a syringe when the temperature of a reaction solution in the three-neck flask is stabilized to 240 ℃, reacting for 5min, and cooling to obtain a solution containing cesium-lead bromide quantum dots.
(C) Adding 75 mu L n-dodecyl mercaptan into 5mL of solution containing cesium lead bromine quantum dots, stirring for 30min at 25 ℃ to obtain a reaction solution, wherein the volume ratio of the reaction solution to n-hexane is 1:2, then centrifuging at the rotating speed of 6000rpm for 5min, discarding the supernatant obtained by centrifugation, dispersing the precipitate in 3mL of n-hexane, finally centrifuging at the rotating speed of 5000rpm for 5min, and collecting the supernatant to obtain the perovskite quantum dot dispersion liquid.
Example 2
The perovskite quantum dot preparation method provided in this example refers to example 1, except that n-dodecyl mercaptan is replaced with hexadecyl mercaptan.
Example 3
The preparation method of the perovskite quantum dot provided by the embodiment is referred to as embodiment 1, and is different from embodiment 1 in that n-dodecyl mercaptan is replaced by hexanethiol.
Example 4
The perovskite quantum dot preparation method provided in this example refers to example 1, except that n-dodecyl mercaptan is replaced with octadecyl mercaptan.
Example 5
The perovskite quantum dot preparation method provided in this example refers to example 1, except that n-dodecanethiol was replaced with 1, 6-hexanedithiol.
Example 6
The preparation method of the perovskite quantum dot provided in this example refers to example 1, except that n-dodecyl mercaptan is replaced with 1, 9-nonanedithiol.
Example 7
The preparation method of the perovskite quantum dot provided by the embodiment comprises the following steps:
(A) And (3) putting 10mL of oleylamine and 1.5mL of hydroiodic acid into a three-neck flask, putting the three-neck flask into a heating jacket, heating, stirring, vacuumizing, heating to 120 ℃, and vacuumizing until no bubbles are generated in the three-neck flask, thereby obtaining the oleylamine-iodine precursor.
(B) Cesium carbonate (0.0326 g and 0.1 mmoL), lead oxide (0.0446g and 0.2 mmoL), 1-octadecene (10 mL) and oleic acid (1 mL) are added into a three-neck flask, then the three-neck flask is placed into a heating jacket to be heated, stirred and vacuumized, the stirring speed is 700rpm, the heating is carried out to 140 ℃, the temperature is kept at 140 ℃ for 30min, then the temperature is raised to 230 ℃, when the temperature of the reaction liquid in the three-neck flask is stabilized to 230 ℃, 0.8mL of oleylamine iodine precursor is rapidly injected by using a syringe, the reaction liquid is reacted for 5min, and then the cooling is carried out, thus obtaining the solution containing the cesium-lead-iodine quantum dots.
(C) Adding 100 mu L n-dodecyl mercaptan into 5mL of solution containing cesium lead iodine quantum dots, stirring for 30min at 25 ℃ to obtain a reaction solution, wherein the volume ratio of the reaction solution to n-hexane is 1:2, then centrifuging at the rotating speed of 6000rpm for 5min, discarding the supernatant obtained by centrifugation, dispersing the precipitate in 3mL of n-hexane, finally centrifuging at the rotating speed of 5000rpm for 5min, and collecting the supernatant to obtain the perovskite quantum dot dispersion liquid.
Example 8
The preparation method of the perovskite quantum dot provided by the embodiment refers to embodiment 1, except that in the step (C), 125 μ L of n-dodecyl mercaptan is added into 5mL of the solution containing the cesium lead bromide quantum dot.
Comparative example 1
The preparation method of the perovskite quantum dot provided by the comparative example is as in example 1, except that in the step (C), the solution containing the cesium lead bromide quantum dot and n-hexane are mixed according to a volume ratio of 1:2, then centrifuging at the rotating speed of 6000rpm for 5min, discarding the supernatant obtained by centrifugation, dispersing the precipitate in 3mL of n-hexane, finally centrifuging at the rotating speed of 5000rpm for 5min, and collecting the supernatant to obtain the perovskite quantum dot dispersion liquid.
Test example 1
The dispersion liquid of perovskite quantum dots prepared in example 1 and comparative example 1 was subjected to a luminescence property test, and the result of the luminescence efficiency (PLQY) test is shown in fig. 2. In fig. 2, the dispersion of the perovskite quantum dots of example 1 is after ligand exchange; the dispersion of perovskite quantum dots of comparative example 1 was prepared before ligand exchange.
As can be seen from FIG. 2, the luminous efficiency of the perovskite quantum dot dispersion before ligand exchange is 89%, the luminous peak position is 516nm, and the half-peak width is 15.35nm; the luminous efficiency of the perovskite quantum dot dispersion liquid after ligand exchange is 99%, the luminous peak position is also 516nm, and the half-peak width is 14.89nm; after ligand exchange, the luminous efficiency of the perovskite quantum dots is improved to be close to 100%, but the luminous peak position and the half-peak width are not obviously changed, which shows that the crystal structure of the quantum dots is not greatly influenced in the ligand exchange process.
Test example 2
Optical films were prepared using the dispersions of perovskite quantum dots prepared in example 1 and comparative example 1, respectively, and their stability was tested.
The preparation method of the optical film comprises the following steps:
pumping out the dispersion liquid of the perovskite quantum dots to obtain a precipitate, and dispersing the precipitate in a small amount of isobornyl acrylate dispersing agent to obtain a solution of the perovskite quantum dots; then 2.0g of UV glue and 0.02g of 1173 initiator are added and mixed evenly.
After uniform mixing, placing the mixture in a vacuum defoaming machine for defoaming treatment, wherein the time of the defoaming treatment is 5min, and the rotating speed of the defoaming treatment is set as follows in sequence: 550rpm (60 s), 800rpm (60 s), 1200rpm (60 s), 600rpm (60 s), 200rpm (60 s).
After the defoaming is finished, parameters of a coater (coating thickness, coating distance, coating speed and the like) are adjusted, a common membrane with a certain width is cut, and then the defoaming dispersion liquid is subjected to blade coating by the coater to form a membrane. And after coating is finished, carrying out UV (ultraviolet) photocuring for 1min, and after curing, cutting to obtain the optical film.
The optical film was subjected to brightness (LV, initial value LV) 0 ) And testing, and respectively placing the test piece in a blue light irradiation environment and a high-temperature environment for stability comparison. The results are shown in fig. 3 and 4. In fig. 3 and 4, the ligand exchange is followed by a dispersion of the perovskite quantum dots of example 1; the dispersion of perovskite quantum dots of comparative example 1 was prepared before ligand exchange.
As can be seen from Table 3, the optical film prepared by adopting the perovskite quantum dots before ligand exchange has brightness rapidly reduced by 70% after 24h, the brightness is reduced by more than 80% after 72h, and the blue light stability is extremely poor; the optical film prepared by adopting the ligand-exchanged perovskite quantum dots has excellent thermal stability, and the brightness is reduced by only 27% after about 600 h.
As can be seen from Table 4, the brightness of the optical film prepared by adopting the perovskite quantum dots before ligand exchange is rapidly reduced by 84% after 24h, and the brightness is reduced by over 90% after 72h, so that the optical film is extremely unstable; the optical film prepared by adopting the ligand-exchanged perovskite quantum dots is quite stable, and the brightness is reduced by only 24% within about 600 h.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the perovskite quantum dot is characterized by comprising the following steps:
will contain CsPbX 3 Mixing the solution of the quantum dots with a thiol ligand, and carrying out ligand exchange reaction to obtain the perovskite quantum dots;
the CsPbX 3 Quantum dotsWherein X is at least one selected from Cl, br and I;
the thiol-based ligand includes an alkyl thiol.
2. The method for producing a perovskite quantum dot as claimed in claim 1, wherein the number of carbon atoms of the alkanethiol is 6 to 18.
3. The method of preparing a perovskite quantum dot as claimed in claim 1, wherein the alkyl thiol comprises at least one of hexanethiol, octanethiol, nonanethiol, n-dodecylmercaptan, tetradecylthiol, hexadecylthiol, octadecanethiol, 1, 6-hexanedithiol, 1, 8-octanethiol, 1, 9-nonanedithiol and 1, 10-decanedithiol.
4. The method for preparing a perovskite quantum dot as claimed in claim 1, wherein the CsPbX-containing material is CsPbX 3 CsPbX in solution of quantum dots 3 The molar ratio of the quantum dots to the thiol ligands is 1:1 to 6.
5. The method for preparing perovskite quantum dots according to claim 1, wherein the temperature of the ligand exchange reaction is 20-25 ℃; the time of the ligand exchange reaction is 0.5 to 2 hours.
6. The method for preparing a perovskite quantum dot as claimed in claim 1, wherein the CsPbX-containing material is CsPbX 3 The preparation method of the solution of the quantum dots comprises the following steps:
heating and vacuumizing a mixture of cesium source, lead source, 1-octadecene and oleic acid, mixing with oleylamine halide precursor, and reacting to obtain the CsPbX-containing material 3 A solution of quantum dots.
7. The method of making the perovskite quantum dot of claim 6, wherein the cesium source comprises at least one of cesium carbonate, cesium acetate, cesium chloride, cesium bromide, and cesium iodide.
8. The method of making a perovskite quantum dot as claimed in claim 6, wherein the lead source comprises at least one of lead oxide, lead acetate, lead chloride, lead bromide and lead iodide.
9. The production method of the perovskite quantum dot as claimed in claim 6, characterized by comprising at least one of the following features (1) to (2):
(1) The temperature of the heating treatment is 120-150 ℃;
(2) The reaction temperature is 220-260 ℃.
10. A perovskite quantum dot, characterized by being prepared by the method for preparing a perovskite quantum dot according to any one of claims 1 to 9.
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