CN111647403B - Preparation method of perovskite quantum dot and perovskite quantum dot - Google Patents
Preparation method of perovskite quantum dot and perovskite quantum dot Download PDFInfo
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- CN111647403B CN111647403B CN202010639613.5A CN202010639613A CN111647403B CN 111647403 B CN111647403 B CN 111647403B CN 202010639613 A CN202010639613 A CN 202010639613A CN 111647403 B CN111647403 B CN 111647403B
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Abstract
The invention discloses a preparation method of perovskite quantum dots and perovskite quantum dots, and relates to the technical field of display.
Description
Technical Field
The invention relates to the technical field of display, in particular to a preparation method of a perovskite quantum dot and the perovskite quantum dot.
Background
All-inorganic perovskite quantum dot CsPbCl 3 /CsPbCl x Br 3-x /CsPbBr 3 /CsPbBr x I 3-x /CsPbI 3 Has higher stability and fluorescence quantum efficiency, and has wide application prospect in future display. However, the quantum dots have a large specific surface area, resulting in a high density of surface defect states, which leads to a decrease in fluorescence quantum efficiency and a decrease in stability. Affecting and limiting practical applications, which are situations that need to be avoided to the utmost.
Disclosure of Invention
The invention aims to provide a preparation method of a perovskite quantum dot and the perovskite quantum dot, which can improve the fluorescence quantum efficiency and stability of the corresponding perovskite quantum dot.
The invention is realized in the following way:
in a first aspect, the invention provides a preparation method of perovskite quantum dots, which comprises the following steps:
stirring a mixture of a lead halide-based precursor, a cesium-based precursor and a metal salt containing gallium ions to form gallium ion-doped perovskite quantum dots;
wherein the doping proportion of gallium ions in the perovskite quantum dots is less than or equal to 5%.
In an alternative embodiment, before the step of stirring the mixture of the lead halide-based precursor, the cesium-based precursor, and the metal salt containing gallium ions, the method further includes the following steps:
preparing the cesium-based precursor;
preparing a lead halide precursor containing gallium ions;
and injecting the cesium-based precursor into the lead halide precursor containing gallium ions according to an equimolar ratio.
In an alternative embodiment, the step of preparing the cesium-based precursor comprises:
adding cesium carbonate to a first solvent contained in a first container;
vacuumizing the first container and heating to a first preset temperature to discharge oxygen and water vapor;
adding oleic acid to the first solvent;
after the oxygen and the water vapor in the first container are discharged, introducing protective gas into the first container;
and heating the first container to a second preset temperature to form the cesium oleate precursor.
In an alternative embodiment, the step of preparing a lead halide precursor containing gallium ions comprises:
adding lead halide, gallium nitrate and/or gallium halide to a second solvent contained in a second container;
vacuumizing the second container and heating to a third preset temperature to discharge oxygen and water vapor;
adding oleic acid and/or oleylamine to the second solvent;
when the oxygen and the water vapor in the second container are discharged, introducing protective gas into the second container;
and raising the temperature of the second container to a fourth preset temperature to form the lead halide precursor containing the gallium ions.
In an alternative embodiment, the first predetermined temperature and the third predetermined temperature are both 100 ℃ to 120 ℃; the second preset temperature and the fourth preset temperature are both 150-160 ℃.
In an alternative embodiment, the first solvent and the second solvent are both octadecene.
In an alternative embodiment, before the step of stirring the mixture of the lead halide-based precursor, the cesium-based precursor, and the metal salt containing gallium ions, the method further includes:
injecting cesium halide and lead halide into a third solvent according to an equimolar ratio;
injecting gallium nitrate or gallium halide into the third solvent, and forming a mixed precursor;
and injecting the mixed precursor into a fourth solvent to form a mixed solution.
In an alternative embodiment, the step of stirring a mixture of a lead halide-based precursor, a cesium-based precursor, and a metal salt containing gallium ions comprises:
stirring the mixed solution;
centrifuging and precipitating the mixed solution;
and separating out the supernatant and obtaining the perovskite quantum dots doped with the gallium ions.
In alternative embodiments, the third solvent is dimethylformamide or dimethylsulfoxide; the fourth solvent is toluene, a mixed solution of toluene and n-hexane, a mixed solution of toluene and n-heptane or a mixed solution of toluene and n-octane.
In another aspect, the present invention provides a perovskite quantum dot obtained by the preparation method according to any one of the preceding embodiments, wherein the doping ratio of gallium ions in the perovskite quantum dot is less than or equal to 5%.
The invention has the following beneficial effects:
according to the preparation method of the perovskite quantum dot and the perovskite quantum dot, provided by the invention, the metal salt containing gallium ions, the lead halide-based precursor and the cesium-based precursor are mixed and stirred to form the perovskite quantum dot doped with the gallium ions, wherein the doping proportion of the gallium ions in the perovskite quantum dot is less than or equal to 5%, and through the doping of high-valence gallium ions, the free carrier concentration in the perovskite quantum dot can be improved, the surface defects are passivated, and the fluorescence quantum efficiency and stability are improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a comparison graph of the effect of the perovskite quantum dots provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 conventional products which are not indicated by manufacturers and are commercially available.
The features and properties of the present invention are described in further detail below with reference to examples.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The embodiment of the invention provides a preparation method of perovskite quantum dots, which comprises the following steps:
a) And stirring a mixture of a lead halide-based precursor, a cesium-based precursor and a metal salt containing gallium ions to form the gallium ion doped perovskite quantum dot, wherein the doping proportion of the gallium ions in the perovskite quantum dot is less than or equal to 5%.
In the process of preparing the perovskite quantum dot, metal salt (such as gallium nitrate, gallium chloride, gallium bromide, gallium iodide and the like) containing gallium ions is mixed with a corresponding lead halide precursor, and then the lead halide precursor reacts with a cesium-based precursor to prepare the perovskite quantum dot (CsPbCl) with the surface doped with the gallium ions and the effective doping proportion of which is less than or equal to 5 percent 3 /CsPbCl x Br 3-x /CsPbBr 3 /CsPbBr x I 3-x /CsPbI 3 ) The N-type doping brought by trivalent metal gallium ions can improve the free carrier concentration of the perovskite quantum dots and passivate defects on the surfaces of the perovskites, so that the fluorescence quantum efficiency and stability of the corresponding perovskite quantum dots are improved.
In this embodiment, before step a, a precursor needs to be prepared, and in this embodiment, the perovskite quantum dots can be prepared by a thermal injection method or a ligand exchange method.
When the hot injection method is adopted, the method comprises the following pre-steps before the step A:
a01 Preparing a cesium-based precursor;
a02 Preparing a lead halide precursor containing gallium ions;
a03 Cesium-based precursor is injected into a lead halide precursor containing gallium ions in equimolar proportions.
Specifically, the step of preparing the cesium-based precursor in this embodiment includes:
a011 Cesium carbonate is added to a first solvent contained in a first container;
a012 Evacuating the first container and raising the temperature to a first preset temperature to discharge oxygen and water vapor;
a013 Adding oleic acid to the first solvent;
a014 Introducing a shielding gas into the first container after the oxygen and the water vapor in the first container are discharged;
a015 Heating the first container to a second predetermined temperature to form the cesium oleate precursor.
Here, the protective gas is an inert or rare gas such as nitrogen, argon, helium, or the like.
Specifically, the step of preparing the lead halide precursor containing gallium ions in this embodiment includes:
a021 Adding lead halide, gallium nitrate and/or gallium halide to a second solvent contained in a second container;
a022 Evacuating the second container and raising the temperature to a third predetermined temperature to vent oxygen and water vapor;
a023 Adding oleic acid and/or oleylamine to the second solvent;
a024 When oxygen and water vapor in the second container are discharged, introducing protective gas into the second container;
a025 Raising the temperature of the second container to a fourth preset temperature to form a lead halide precursor containing gallium ions.
It should be noted that, here, step a 021) includes the following combinations: lead halides and gallium nitrates; lead halides and gallium halides; lead halides, gallium nitrates, and gallium halides.
In the embodiment, the first preset temperature and the third preset temperature are both 100-120 ℃; the second preset temperature and the fourth preset temperature are both 150-160 ℃.
In this example, both the first solvent and the second solvent are octadecene. Of course, the first solvent may be any other organic solvent capable of dissolving cesium carbonate, and the second solvent may be any other organic solvent capable of dissolving lead halide, gallium nitrate and gallium halide, which are not listed here.
Specifically, the process for preparing the perovskite quantum dot by adopting the thermal injection method comprises the following steps:
firstly, preparing a precursor of cesium oleate, adding cesium carbonate into octadecene, vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, adding oleic acid, stopping vacuumizing when no bubbles exist, introducing nitrogen for protection, heating to 150-160 ℃ to form the cesium oleate precursor, and heating and stirring at constant temperature.
Adding octadecene into gallium nitrate or corresponding gallium halide and lead halide, vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, injecting oleic acid or oleic acid oleylamine combination, stopping vacuumizing until no bubbles exist, introducing nitrogen for protection, heating to 150-160 ℃, forming a lead halide precursor containing gallium ions, and heating and stirring at constant temperature.
And (3) quickly injecting the cesium oleate precursor solution into a lead halide precursor solution containing gallium ions, and quickly cooling in an ice-water bath to obtain the gallium ion-doped all-inorganic perovskite quantum dot. The doping ratio of the gallium ions can be controlled by the ratio of the raw materials, and specific examples can be found.
The present embodiment also provides a method for preparing a precursor by a ligand exchange method, and particularly, when the ligand exchange method is adopted, before step a, the method may further include the following pre-steps:
a02 Cesium halide, lead halide are injected into the third solvent in equimolar proportions;
a03 Injecting gallium nitrate or gallium halide into the third solvent and forming a mixed precursor;
a04 Inject the mixed precursor into a fourth solvent to form a mixed solution.
Specifically, the step of stirring a mixture of a lead halide-based precursor, a cesium-based precursor, and a metal salt containing gallium ions includes:
a11 Stirring the mixture;
a12 ) centrifuging the precipitation mixture;
a13 Separating the supernatant and obtaining the perovskite quantum dots doped with gallium ions.
In this embodiment, the third solvent is dimethylformamide or dimethylsulfoxide; the fourth solvent is toluene, a mixed solution of toluene and n-hexane, a mixed solution of toluene and n-heptane or a mixed solution of toluene and n-octane. Of course, the third solvent and the fourth solvent are not limited to the organic materials listed in the present embodiment.
Specifically, the process for preparing the perovskite quantum dots by adopting a ligand exchange method comprises the following steps:
cesium halide and lead halide are dispersed in DMSO (dimethyl sulfoxide) or DMF (dimethyl formamide) solution according to the equal molar ratio, then gallium nitrate or corresponding gallium halide is injected according to a certain molar ratio to form clear liquid, and the clear liquid is uniformly stirred to form a mixed precursor. And then rapidly injecting the mixed precursor solution into a toluene solution or a mixed solution of toluene and n-hexane/n-heptane/n-octane under the condition of vigorous stirring, carrying out centrifugal precipitation, removing quantum dot particles with larger particle sizes, and selecting supernate, namely the gallium ion doped all-inorganic perovskite quantum dot. The doping ratio of the gallium ions can be controlled by the ratio of the raw materials, and specific examples can be found.
In another aspect, this embodiment further provides a perovskite quantum dot obtained by one of the foregoing two preparation methods, wherein the doping ratio of gallium ions in the perovskite quantum dot is less than or equal to 5%.
According to the preparation method of the perovskite quantum dot and the perovskite quantum dot, provided by the embodiment, the metal salt containing gallium ions, the lead halide-based precursor and the cesium-based precursor are mixed and stirred to form the perovskite quantum dot doped with the gallium ions, wherein the doping proportion of the gallium ions in the perovskite quantum dot is less than or equal to 5%, and through the doping of high-valence gallium ions, the free carrier concentration in the perovskite quantum dot can be improved, the surface defects are passivated, and the fluorescence quantum efficiency and stability are improved.
For further understanding of the present invention, the following describes a method for preparing a perovskite quantum dot provided by the present invention with reference to an example and fig. 1, where fig. 1 is a schematic diagram of the effect of the perovskite quantum dot provided by the present invention, and the scope of the present invention is not limited by the following example.
Example 1
In this embodiment, a thermal injection method is used to prepare perovskite quantum dots, specifically as follows:
preparing a cesium oleate precursor: adding 0.1mol or A mol of cesium carbonate into more than or equal to 15ml of octadecene, vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, adding more than or equal to 1.2ml of oleic acid until no bubbles exist in the solution, taking about one hour, stopping vacuumizing, introducing nitrogen for protection, heating to 150-160 ℃, preferably 150 ℃ or 160 ℃, forming a cesium oleate precursor, wherein the concentration of the cesium oleate precursor is less than or equal to 1mol/L, and heating and stirring at constant temperature.
Preparing a lead halide precursor containing gallium ions: adding 0.1mmol or B mmol of lead halide, C mmol of gallium nitrate or corresponding gallium halide into 5ml or more of octadecene, wherein B =0.1-0.3, C/B =5% -80%, then vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, injecting 1ml or more of oleic acid or injecting 0.5ml or more of oleic acid and 0.5ml or more of oleylamine combination. And stopping vacuumizing until no bubbles exist, taking about one hour, introducing nitrogen for protection, heating to 150-160 ℃, preferably 150 ℃ or 160 ℃, clarifying the solution at the moment, heating at constant temperature and stirring, wherein the concentration of the lead halide precursor containing gallium ions is less than or equal to 1 mol/L. Wherein the gallium ion doping proportion of the final perovskite quantum dot can be less than or equal to 5% by controlling the molar ratio of the lead halide to the gallium nitrate or the gallium halide.
And (3) final reaction: and taking the solution containing B mol of cesium oleate from the cesium oleate precursor solution, quickly injecting the solution into the lead halide precursor solution containing gallium ions, and quickly cooling in an ice-water bath to obtain the gallium ion-doped all-inorganic perovskite quantum dot.
Example 2
In this embodiment, a ligand exchange method is used to prepare the perovskite quantum dots, specifically as follows:
preparing a precursor: dispersing cesium halide and lead halide in DMSO or DMF solution at equal molar ratio, then forming clear liquid by gallium nitrate or corresponding gallium halide at a certain molar ratio (the molar ratio of gallium nitrate or corresponding gallium halide to lead halide is 5% -80%), and stirring uniformly. Wherein the gallium ion doping proportion of the final perovskite quantum dot can be less than or equal to 5% by controlling the molar ratio of gallium nitrate or corresponding gallium halide to lead halide.
And (3) final reaction: and (2) rapidly injecting the precursor solution into a toluene solution or a mixed solution of toluene and n-hexane/n-heptane/n-octane under the condition of vigorous stirring (the volume ratio of the precursor solution to the toluene or the mixed solution is more than or equal to 10), carrying out centrifugal precipitation, removing quantum dot particles with larger particle sizes, and selecting a supernatant, namely the gallium ion doped all-inorganic perovskite quantum dots.
In summary, embodiments of the present invention provide a perovskite quantum dot and a preparation method thereof, and the perovskite quantum dot is prepared by a thermal injection method or a ligand exchange method, and the molar ratio is controlled such that the doping ratio of gallium ions of the perovskite quantum dot is less than or equal to 5%, and compared with an undoped all-inorganic perovskite quantum dot, when the doping ratio is less than or equal to 5%, the doping of high-valence metal gallium ions can improve the concentration of free carriers in the perovskite quantum dot, passivate surface defects, and thereby improve fluorescence quantum efficiency and stability.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. The preparation method of the perovskite quantum dot is characterized by comprising the following steps:
preparing a cesium oleate precursor: adding cesium carbonate into octadecene of which the volume is more than or equal to 15ml, vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, adding oleic acid of which the volume is more than or equal to 1.2ml until no bubbles exist in the solution, keeping the time for one hour, stopping vacuumizing, introducing nitrogen for protection, heating to 150-160 ℃ to form a cesium oleate precursor, wherein the concentration of the cesium oleate precursor is less than or equal to 1mol/L, and heating and stirring at constant temperature;
preparing a lead halide precursor containing gallium ions: adding B mmol of lead halide and C mmol of gallium nitrate into octadecene with the volume of more than or equal to 5ml, wherein B =0.1-0.3, C/B =5% -80%, vacuumizing, heating to 100-120 ℃, discharging oxygen and water vapor, injecting oleic acid with the volume of more than or equal to 1ml or injecting oleic acid with the volume of more than or equal to 0.5ml and oleylamine with the volume of more than or equal to 0.5ml until no bubbles exist, stopping vacuumizing for one hour, introducing nitrogen for protection, and heating to 150-160 ℃;
and (3) final reaction: quickly injecting the cesium oleate precursor into a lead halide precursor containing gallium ions, and quickly cooling in an ice-water bath to obtain perovskite quantum dots doped with the gallium ions;
the doping proportion of gallium ions in the perovskite quantum dots is less than 5%, and the surfaces of the perovskite quantum dots are doped with the gallium ions, so that the free carrier concentration of the perovskite quantum dots is improved, and defects on the surfaces of the perovskite quantum dots are passivated.
2. A perovskite quantum dot obtained by the production method according to claim 1, wherein the doping ratio of gallium ions in the perovskite quantum dot is less than 5%.
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