CN115386364A - Preparation method of blue-light perovskite quantum dots - Google Patents
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Abstract
The invention belongs to the technical field of photoelectric material preparation, and particularly relates to a preparation method of blue-light perovskite quantum dots. The invention provides a preparation method of a blue-light perovskite quantum dot, which comprises the following steps: mixing water-soluble cesium salt, water-soluble rubidium salt, a lead-containing compound, a stabilizer and a non-polar organic solvent in a first stage, and carrying out liquid phase reaction to obtain a first-stage mixture; mixing the primary mixture and the phenylphosphonic dichloride in a secondary mode, and performing a first coordination reaction to obtain a quantum dot crystal blank; and mixing the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene in a three-stage manner, and performing a second coordination reaction to obtain the blue-light perovskite quantum dot. The blue-light perovskite quantum dot obtained by the method has the advantages of narrow peak width at half height and high color purity.
Description
Technical Field
The invention belongs to the technical field of photoelectric material preparation, and particularly relates to a preparation method of blue-light perovskite quantum dots.
Background
At present, after going through the first generation display technology (cathode ray tube) and the second generation display technology (liquid crystal display), the third generation display technology, i.e., the light emitting diode display technology, has been developed. Perovskite quantum dots are the main luminescent materials of the display technology of light-emitting diodes due to the excellent optical properties of the perovskite quantum dots.
The perovskite quantum dots mainly comprise red perovskite quantum dots, green perovskite quantum dots and blue perovskite quantum dots. The luminous performance of the traditional blue light perovskite quantum dot is far behind that of red light and green light perovskite quantum dots, and the commercial application of the blue light perovskite quantum dot is hindered.
In recent years, the luminescent performance of the blue perovskite quantum dots can be further improved by optimizing the preparation method of the blue perovskite quantum dots; however, the obtained blue perovskite quantum dot still has the defect of wide half-height peak width, so that the color purity of the blue perovskite quantum dot is low, and the application of the blue perovskite quantum dot in high-color-gamut display is limited.
Disclosure of Invention
The invention aims to provide a preparation method of a blue perovskite quantum dot, and the blue perovskite quantum dot obtained by the method provided by the invention is narrow in half-height peak width and high in color purity.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a blue-light perovskite quantum dot, which comprises the following steps:
mixing water-soluble cesium salt, water-soluble rubidium salt, a lead-containing compound, a stabilizer and a non-polar organic solvent in a first stage, and carrying out liquid phase reaction to obtain a first-stage mixture;
mixing the primary mixture and the phenylphosphonic dichloride, and performing a first coordination reaction to obtain a quantum dot crystal blank;
and mixing the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene in a three-stage manner, and performing a second coordination reaction to obtain the blue-light perovskite quantum dot.
Preferably, the water-soluble cesium salt comprises one or more of cesium carbonate, cesium acetate and cesium nitrate;
the water-soluble rubidium salt comprises one or more of rubidium carbonate, rubidium acetate and rubidium nitrate;
the lead-containing compound comprises lead oxide and/or lead acetate;
the stabilizer comprises oleylamine and oleic acid;
the non-polar organic solvent includes octadecene and/or diphenyl ether.
Preferably, the molar ratio of the oleic acid to the oleylamine is (5-10): (10-30);
the molar ratio of the water-soluble cesium salt to the water-soluble rubidium salt to the lead-containing compound to oleic acid to oleylamine is 0.175:0.075:1: (5-10): (10 to 30).
The dosage ratio of the lead-containing compound to the nonpolar organic solvent is 1mmol:20 to 30mL.
Preferably, the liquid phase reaction comprises sequentially performing a first liquid phase reaction and a second liquid phase reaction.
Preferably, the first liquid phase reaction process is as follows: heating to 100-120 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring, and preserving heat for 30-60 min; the first liquid phase reaction is carried out under vacuum conditions;
the second liquid phase reaction process comprises the following steps: heating to 260 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring to obtain the first-stage mixture; the second liquid phase reaction is carried out under a protective atmosphere.
Preferably, the molar ratio of the lead-containing compound to the phenylphosphonic dichloride is 1:2 to 4.
Preferably, the first coordination reaction is carried out under a protective atmosphere;
the temperature of the first coordination reaction is 260 ℃ and the time is 15-20 s.
Preferably, the first coordination reaction is terminated by a cooling treatment; the cooling rate of the cooling treatment is 50-60 ℃/s.
Preferably, the mass ratio of the quantum dot crystal blank to the tetraoctyl ammonium fluoride to the benzoyl bromide is 1:2:2 to 3;
the dosage ratio of the quantum dot crystal blank to the toluene is 5-10 mg:1mL.
Preferably, the temperature of the second coordination reaction is 25-30 ℃ and the time is 40-45 min.
The invention provides a preparation method of a blue-light perovskite quantum dot, which comprises the following steps: mixing water-soluble cesium salt, water-soluble rubidium salt, a lead-containing compound, a stabilizer and a non-polar organic solvent in a first stage, and carrying out liquid phase reaction to obtain a first-stage mixture; mixing the primary mixture and the phenylphosphonic dichloride in a secondary mode, and performing a first coordination reaction to obtain a quantum dot crystal blank; and mixing the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene in a three-stage manner, and performing a second coordination reaction to obtain the blue-light perovskite quantum dot. In the present invention, benzoyl bromide provides anion-exchanged Br ions for the quantum dots; the tetraoctyl ammonium fluoride can be used as a high-efficiency stable replacement ligand to replace a ligand easy to desorb on the surface of the quantum dot, so that the stability of the quantum dot is enhanced; meanwhile, after a crystal blank is prepared by high-temperature shock cooling, the quantum dots are gradually grown into crystals with uniform particle size through a slow and stable regrowth environment, and finally the obtained blue-light perovskite quantum dots are narrow in half-height peak width and high in color purity.
Drawings
FIG. 1 is an absorption spectrogram, a fluorescence spectrogram and a fluorescence real image of the blue-light perovskite quantum dot obtained in example 1;
FIG. 2 is a fluorescence quantum yield test chart of the blue perovskite quantum dots obtained in example 1;
fig. 3 is a graph showing the change of the fluorescence quantum yield with time of the perovskite quantum dots obtained in example 1 and comparative example 1.
Detailed Description
The invention provides a preparation method of a blue-light perovskite quantum dot, which comprises the following steps:
mixing water-soluble cesium salt, water-soluble rubidium salt, a lead-containing compound, a stabilizer and a non-polar organic solvent in a first stage, and carrying out liquid phase reaction to obtain a first-stage mixture;
mixing the primary mixture and the phenylphosphonic dichloride in a secondary mode, and performing a first coordination reaction to obtain a quantum dot crystal blank;
and mixing the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene in a three-stage manner, and performing a second coordination reaction to obtain the blue-light perovskite quantum dot.
In the present invention, all the starting materials for the preparation are commercially available products well known to those skilled in the art, unless otherwise specified.
According to the invention, water-soluble cesium salt, water-soluble rubidium salt, lead-containing compound, stabilizer and nonpolar organic solvent are mixed at first grade, and a first-grade mixture is obtained through liquid phase reaction.
In the present invention, the water-soluble cesium salt preferably includes one or more of cesium carbonate, cesium acetate, and cesium nitrate. In the present invention, the water-soluble rubidium salt preferably includes one or more of rubidium carbonate, rubidium acetate, and rubidium nitrate. In the present invention, the lead-containing compound preferably comprises lead oxide and/or lead acetate. In the present invention, the non-polar organic solvent preferably includes octadecene and/or diphenyl ether.
In the present invention, the stabilizer preferably includes oleylamine and oleic acid; the mol ratio of the oleic acid to the oleylamine is (5-10): (10 to 30), more preferably (6 to 9): (12 to 28), more preferably (7 to 8): (15 to 25).
In the present invention, the molar ratio of the water-soluble cesium salt, the water-soluble rubidium salt, the lead-containing compound, the oleic acid, and the oleylamine is preferably 0.175:0.075:1: (5-10): (10 to 30), more preferably 0.175:0.075:1: (6-9): (12 to 28), more preferably 0.175:0.075: (7-8): (15 to 25).
In the present invention, the ratio of the amount of the lead-containing compound to the nonpolar organic solvent is preferably 1mmol:20 to 30mL, more preferably 1mmol:12 to 28mL, more preferably 1mmol: 15-25 mL.
The process of the first mixing is not particularly limited, and may be performed by a process known to those skilled in the art.
In the present invention, the liquid phase reaction preferably includes sequentially performing a first liquid phase reaction and a second liquid phase reaction. In the present invention, the first liquid phase reaction is preferably carried out by: heating to 100-120 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring, and preserving heat for 30-60 min; the first liquid phase reaction is carried out under vacuum conditions. In the present invention, the stirring speed is preferably 400 to 500rpm. In the present invention, the raw material can be dissolved by carrying out the first liquid phase.
In the present invention, the process of the second liquid phase reaction is preferably: heating to 260 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring to obtain the first-stage mixture; the second liquid phase reaction is carried out under a protective atmosphere. In the present invention, the rotation speed of the stirring is preferably 400 to 500rpm. In the present invention, the protective atmosphere is preferably argon.
After the primary mixture is obtained, the primary mixture and the phenylphosphonic dichloride are mixed in a secondary mode, and the quantum dot crystal blank is obtained through a first coordination reaction.
In the present invention, the molar ratio of the lead-containing compound to the phenylphosphonic dichloride is preferably 1:2 to 4, more preferably 1:3. in the present invention, the first coordination reaction is preferably carried out under a protective atmosphere; the protective atmosphere is preferably argon. In the present invention, the temperature of the first coordination reaction is preferably 260 ℃ and the time is preferably 15 to 20 seconds. In the present invention, the first coordination reaction is preferably terminated by a cooling treatment. In the present invention, the cooling rate of the cooling treatment is preferably 50 to 60 ℃/s. In the embodiment of the present invention, the cooling treatment is preferably performed by placing the reaction solution in an ice-water bath. In the invention, the reaction is rapidly stopped by utilizing cooling treatment with larger temperature difference, and the crystal can be rapidly precipitated, thereby obtaining a large number of quantum dot crystal blanks.
After the first coordination reaction is terminated, the present invention preferably further comprises subjecting the obtained reaction solution to post-treatment; the post-treatment preferably comprises the steps of:
standing the obtained reaction solution to restore the temperature of the reaction solution to room temperature, and performing first separation to obtain a first precipitate;
mixing the first precipitate and n-hexane for the first time, and performing second separation to obtain a first supernatant;
mixing the supernatant with methyl acetate for the second time, and performing third separation to obtain a second precipitate;
and thirdly, mixing the second precipitate and toluene to obtain a toluene solution containing the quantum dot crystal embryo.
In the present invention, the first separation mode is preferably centrifugal separation; the rotation speed of the centrifugal separation is preferably 10000rpm, and the time is preferably 5min.
In the present invention, the ratio of the amount of the first precipitate to n-hexane is preferably 10mg:1mL.
The first mixing process is not particularly limited, and may be performed by a process known to those skilled in the art.
In the present invention, the second separation mode is preferably centrifugal separation; the rotational speed of the centrifugal separation is preferably 4000rpm, and the time is preferably 1min.
In the present invention, the volume ratio of the first supernatant to methyl acetate is preferably 1:3. the process of the second mixing is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art. In the present invention, the third separation mode is preferably centrifugal separation; the rotation speed of the centrifugal separation is preferably 10000rpm, and the time is preferably 5min.
In the invention, the quantum dot crystal blank is cleaned by adopting methyl acetate, and excessive ligand on the surface of the quantum dot can be removed.
The third mixing method is not particularly limited, and may be performed by a process known to those skilled in the art. In the invention, the concentration of the quantum dot crystal embryo in the toluene solution containing the quantum dot crystal embryo is preferably 10mg/mL.
In the invention, cesium ions and lead ions in the solution and chloride ions provided by the injected phenylphosphonic dichloride are subjected to crystal growth through a rapid crystallization reaction at high temperature; and simultaneously, rapidly cooling through an ice water bath and stopping a crystallization reaction under the action of a surface ligand to finally obtain the quantum dot crystal blank with smaller particle size.
After the quantum dot crystal blank is obtained, the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene are mixed in a three-level mode, and the deep blue light perovskite quantum dot is obtained through a second coordination reaction.
In the invention, the mass ratio of the quantum dot crystal blank to the tetraoctylammonium fluoride to the benzoyl bromide is preferably 1:2:2 to 3. In the invention, the dosage ratio of the quantum dot crystal blank to the toluene is preferably 5-10 mg:1mL.
In the invention, the quantum dot crystal embryo is preferably subjected to three-stage mixing in the form of a toluene solution of the quantum dot crystal embryo. In the present invention, the quantum dot crystal embryo toluene solution is preferably the toluene solution containing quantum dot crystal embryos described in the above technical solution.
In the present invention, the tetraoctylammonium fluoride is preferably three-stage mixed in the form of a toluene solution of tetraoctylammonium fluoride. In the present invention, the concentration of tetraoctylammonium fluoride in the toluene solution of tetraoctylammonium fluoride is preferably 150mg/mL. The preparation method of the tetraoctyl ammonium fluoride toluene solution is not particularly limited, and the tetraoctyl ammonium fluoride and the toluene are directly mixed and intensively stirred until the solution is clear.
In the invention, the three-stage mixing process is as follows: and adding the tetraoctyl ammonium fluoride toluene solution and benzoyl bromide into the quantum dot crystal embryo toluene solution under the condition of stirring.
In the present invention, the rotation speed of the stirring is preferably 400 to 600rpm, and more preferably 450 to 550rpm.
In the present invention, the temperature of the second coordination reaction is preferably 25 to 30 ℃ and the time is preferably 40 to 45min.
In the invention, the quantum dot crystal blank is subjected to curing and regrowth treatment by adopting tetraoctyl ammonium fluoride and benzoyl bromide, so that excessive halogen ions can be introduced into the quantum dots to construct a halogen ion-rich environment, and further, lattice defects and surface defects caused by halogen vacancies are reduced; on the other hand, the tetraoctyl ammonium fluoride is introduced, the coordination capacity of tetraoctyl ammonium radicals and halogen ions on the surface of the quantum dots is increased by utilizing the larger electronegativity of fluorine ions, and the stability and the optical performance of the quantum dots are improved by utilizing the stronger coordination capacity of the tetraoctyl ammonium radicals relative to protonated alkylamine groups and the halogen ions.
After the second coordination reaction is completed, the invention also preferably comprises post-treatment of the reaction solution; the post-treatment is preferably: fourthly, mixing the reaction liquid with methyl acetate, and carrying out fourth separation to obtain a third precipitate;
and mixing the third precipitate and n-hexane for the fifth time, and separating for the fifth time to obtain a second supernatant.
In the present invention, the volume ratio of the reaction liquid to methyl acetate is preferably 1:2 to 3. In the present invention, the fourth separation mode is preferably centrifugal separation; the rotation speed of the centrifugal separation is preferably 10000rpm, and the time is preferably 5min.
In the present invention, the ratio of the amount of the third precipitate to n-hexane is preferably 10mg:1mL. In the present invention, the fifth separation mode is preferably centrifugal separation; the rotational speed of the centrifugal separation is preferably 6000rpm, and the time is preferably 1min.
In the present invention, the second supernatant preferably includes blue perovskite quantum dots and n-hexane. In the present invention, the blue perovskite quantum dot is preferably present in the form of a blue perovskite quantum dot n-hexane solution.
In the invention, the structural formula of the blue perovskite quantum dot is preferably Cs x Rb 1-x PbCl 3 Br 3-y (ii) a The value range of x is preferably more than 0 and less than or equal to 1; the value range of y is preferably more than or equal to 0 and less than or equal to 3.
For further illustration of the present invention, the following detailed description of the preparation method of a blue perovskite quantum dot provided by the present invention is provided with reference to the drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Adding 0.105mmol of cesium carbonate, 0.045mmol of rubidium carbonate, 0.6mmol of lead oxide, 3mmol of oleic acid, 6mmol of oleylamine and 15mL of octadecene as solvents into a two-neck flask for mixing, heating to 120 ℃ at the heating rate of 10 ℃/min under the conditions of stirring (the rotating speed is 400 rpm) and vacuum, and preserving heat for 50min; then replacing the atmosphere with argon, and heating to 260 ℃ at a heating rate of 10 ℃/min under the condition of stirring (the rotating speed is 400 rpm) to obtain a first-stage mixture;
adding 0.35g of phenylphosphonyl dichloride into the primary mixture, reacting for 15s at the temperature of 260 ℃ at the rotating speed of 400rpm under the atmosphere of argon, and cooling by using an ice water bath (the cooling rate is 50 ℃/s) to terminate the reaction;
standing the obtained reaction solution to restore the temperature to room temperature, centrifuging at 10000rpm for 5min, and collecting 100mg precipitate; dispersing the obtained precipitate in 10mL of n-hexane, centrifuging at 4000rpm for 1min, and collecting 10mL of supernatant; adding the obtained supernatant into 30mL of methyl acetate, and centrifuging at 10000rpm for 5min to obtain 100mg of precipitate; mixing the obtained precipitate with 10mL of toluene to obtain a toluene solution containing the quantum dot crystal embryo;
adding 1500 mu L of 150mg/mL tetraoctyl ammonium fluoride toluene solution and 230mg benzoyl bromide into the obtained toluene solution containing the quantum dot crystal embryo at the stirring speed of 450rpm, reacting at 25 ℃ for 40min, adding 30mL methyl acetate, centrifuging at 10000rpm for 5min, and collecting 50mg precipitate; dispersing the obtained precipitate in 5mL of n-hexane, centrifuging at 6000rpm for 1min, and removing the precipitate to obtain an n-hexane solution containing perovskite quantum dots.
Example 2
Adding 0.105mmol of cesium carbonate, 0.045mmol of rubidium carbonate, 0.6mmol of lead oxide, 3mmol of oleic acid and 6mmol of oleylamine into a two-neck flask for mixing, then adding 15ml of octadecene as a solvent, heating to 100 ℃ at the heating rate of 10 ℃/min under the conditions of stirring (the rotating speed is 450 pm) and vacuum, and preserving heat for 50min; then replacing the atmosphere with argon, and heating to 260 ℃ at a heating rate of 15 ℃/min under the condition of stirring (the rotating speed is 400 rpm) to obtain a first-stage mixture;
adding 0.4g of phenylphosphonyl dichloride into the primary mixture, reacting for 15s at the temperature of 260 ℃ at the rotating speed of 400rpm under the atmosphere of argon, and cooling by using an ice water bath (the cooling rate is 50 ℃/s) to terminate the reaction;
standing the obtained reaction solution to restore the temperature to room temperature, centrifuging at 10000rpm for 5min, and collecting 100mg precipitate; dispersing the obtained precipitate in 10mL of n-hexane, centrifuging at 4000rpm for 1min, and collecting 10mL of supernatant; adding the obtained supernatant into 30mL of methyl acetate, and centrifuging at 10000rpm for 5min to obtain 100mg of precipitate; mixing the obtained precipitate with 10mL of toluene to obtain a toluene solution containing quantum dot crystal embryos;
adding 1500 mu L of 150mg/mL tetraoctyl ammonium fluoride toluene solution and 230mg benzoyl bromide into the obtained toluene solution containing the quantum dot crystal embryo at the stirring speed of 450rpm, reacting at 25 ℃ for 40min, adding 30mL methyl acetate, centrifuging at 10000rpm for 5min, and collecting 50mg precipitate; dispersing the obtained precipitate in 5mL of n-hexane, centrifuging at 6000rpm for 1min, and removing the precipitate to obtain an n-hexane solution containing perovskite quantum dots.
Comparative example 1
Perovskite quantum dots were prepared in the manner of example 1, except that no tetraoctylammonium fluoride toluene solution was added.
Performance testing
Test example 1
An absorption spectrogram, a fluorescence spectrogram and a fluorescence real object diagram of the perovskite quantum dot obtained in the embodiment 1 are shown in fig. 1, and as can be seen from fig. 1, the maximum emission peak position of the perovskite quantum dot obtained in the invention is 459nm, the perovskite quantum dot can emit deep blue fluorescence, and the peak width at half height is 15.82nm.
Test example 2
The fluorescence quantum yield of the perovskite quantum dots obtained in example 1 was tested by using an integrating sphere under the following test conditions: the model number of the instrument HORIBA FLORAMAX-3 is that the excitation wavelength is 365nm, the scanning speed is 1nm/s, and the slit width is 2nm; the obtained test curve and the test result are shown in fig. 2, and it can be seen from fig. 2 that the highest fluorescence quantum yield of the perovskite quantum dot obtained in the present embodiment is 92.13%.
Test example 3
The perovskite quantum dots of the example 1 and the comparative example 1 are placed in an atmospheric environment, and the change value of the fluorescence quantum yield along with time is tested under the following test conditions: the model number of the apparatus HORIBA FLORAMAX-3 is 365nm, the scanning speed is 1nm/s, the slit width is 2nm, and the fluorescence quantum yield of the 1 st day, the 4 th day, the 10 th day and the 30 th day are respectively recorded;
the obtained fluorescence quantum yield variation curve with time is shown in FIG. 3; as can be seen from fig. 3, the quantum dot added with tetraoctylammonium fluoride as a highly efficient displacement passivation ligand in example 1 has more excellent stability, and can be stored for a longer time in an atmospheric environment.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. A preparation method of a blue-light perovskite quantum dot is characterized by comprising the following steps:
mixing water-soluble cesium salt, water-soluble rubidium salt, a lead-containing compound, a stabilizer and a non-polar organic solvent in a first stage, and carrying out liquid phase reaction to obtain a first-stage mixture;
mixing the primary mixture and the phenylphosphonic dichloride in a secondary mode, and performing a first coordination reaction to obtain a quantum dot crystal blank;
and mixing the quantum dot crystal blank, tetraoctyl ammonium fluoride, benzoyl bromide and toluene in a three-stage manner, and performing a second coordination reaction to obtain the blue-light perovskite quantum dot.
2. The preparation method according to claim 1, wherein the water-soluble cesium salt comprises one or more of cesium carbonate, cesium acetate and cesium nitrate;
the water-soluble rubidium salt comprises one or more of rubidium carbonate, rubidium acetate and rubidium nitrate;
the lead-containing compound comprises lead oxide and/or lead acetate;
the stabilizer comprises oleylamine and oleic acid;
the non-polar organic solvent includes octadecene and/or diphenyl ether.
3. The method according to claim 2, wherein the molar ratio of oleic acid to oleylamine is (5 to 10): (10 to 30);
the molar ratio of the water-soluble cesium salt to the water-soluble rubidium salt to the lead-containing compound to oleic acid to oleylamine is 0.175:0.075:1: (5-10): (10 to 30).
The dosage ratio of the lead-containing compound to the nonpolar organic solvent is 1mmol:20 to 30mL.
4. The production method according to claim 1, wherein the liquid-phase reaction comprises sequentially performing a first liquid-phase reaction and a second liquid-phase reaction.
5. The method according to claim 4, wherein the first liquid phase reaction is carried out by: heating to 100-120 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring, and preserving heat for 30-60 min; the first liquid phase reaction is carried out under vacuum conditions;
the second liquid phase reaction process comprises the following steps: heating to 260 ℃ at a heating rate of 10-15 ℃/min under the condition of stirring to obtain the first-stage mixture; the second liquid phase reaction is carried out under a protective atmosphere.
6. The production method according to claim 1, wherein the molar ratio of the lead-containing compound to the phenylphosphonic dichloride is 1:2 to 4.
7. The method according to claim 6, wherein the first coordination reaction is carried out under a protective atmosphere;
the temperature of the first coordination reaction is 260 ℃ and the time is 15-20 s.
8. The production method according to claim 7, wherein the first coordination reaction is terminated by a cooling treatment; the cooling rate of the cooling treatment is 50-60 ℃/s.
9. The preparation method of claim 1, wherein the mass ratio of the quantum dot crystal blank to the tetraoctylammonium fluoride to the benzoyl bromide is 1:2:2 to 3;
the dosage ratio of the quantum dot crystal blank to the toluene is 5-10 mg:1mL.
10. The method according to claim 9, wherein the temperature of the second coordination reaction is 25 to 30 ℃ and the time is 40 to 45min.
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| CN116004228A (en) * | 2022-12-26 | 2023-04-25 | 无锡极电光能科技有限公司 | Surface modified perovskite quantum dot, preparation method thereof and core-shell structure quantum dot |
| CN116004228B (en) * | 2022-12-26 | 2024-04-26 | 无锡极电光能科技有限公司 | Surface modified perovskite quantum dot, preparation method thereof and core-shell structure quantum dot |
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