CN112375567B - Method for preparing cesium-lead-bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation - Google Patents
Method for preparing cesium-lead-bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation Download PDFInfo
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Abstract
The invention discloses a method for preparing cesium lead bromoperovskite quantum dots based on in-situ aminosilane and bromide ion passivation. The quantum dot fluorescence quantum efficiency obtained by the invention can reach 99%, and the quantum dot fluorescence quantum efficiency has higher stability in high-temperature environment and polar organic solvent, and is suitable for preparing high-performance luminescent devices in air by adopting a solution method.
Description
Technical Field
The invention relates to a preparation method of cesium-lead-bromine perovskite quantum dots suitable for a solution method device process, and belongs to the field of novel nano material preparation.
Background
Light emitting diodes based on inorganic semiconductor materials are a highly efficient light emitting device. The luminescent layer material and the device prepared by epitaxial growth of the single crystal substrate usually need to obtain a light emitting body in a point light source form through the procedures of laser cutting, surface mounting, packaging and the like so as to be applied to illumination, backlight and the like, and have the disadvantages of complex process and higher manufacturing cost. And if applied to micro-scale displays, also requires the use of more complex and massive transfer techniques. The inorganic perovskite nano crystal in the quantum dot form has excellent luminescence property, the fluorescence quantum efficiency is up to more than 90%, the full peak width at half height of an emission spectrum can be as low as 20nm, and the inorganic perovskite nano crystal can be prepared by a simpler solution method and is a more ideal luminescent material. In the aspect of device application, the quantum dot material can be prepared into a thin film light-emitting layer with the thickness of dozens of nanometers by using an organic solvent and a solution process. For electroluminescent devices, a carrier transport layer also needs to be prepared above the light emitting layer. The carrier transport layer prepared by the solution method can further reduce the manufacturing cost of the device, for example, a zinc oxide nano-crystalline film prepared by taking ethanol as a solvent is a good electron transport layer material. Ethanol is used as a common polar organic solvent, has good solution processability, but has a great destructive effect on a perovskite quantum dot light-emitting layer at the bottom layer. Therefore, the development of the perovskite quantum dot material with high tolerance to ethanol is of great significance for the development of quantum dot electroluminescent devices.
Disclosure of Invention
In order to avoid the defects in the prior art, the invention provides a method for preparing cesium-lead-bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation, aiming at obtaining CsPbBr with high fluorescence quantum efficiency (PLQY) and high tolerance to solvents such as ethanol and the like 3 And (4) quantum dots.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the method for preparing the cesium-lead-bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation is characterized by comprising the following steps of: firstly, respectively preparing a cesium oleate precursor solution and a lead bromide precursor solution containing zinc bromide, then adding aminosilane into the lead bromide precursor solution, and then injecting the cesium oleate precursor solution into the lead bromide precursor solution by a thermal injection method for reaction, thereby obtaining the cesium lead bromoperovskite quantum dot with a passivation layer formed on the surface. The method specifically comprises the following steps:
Adding cesium carbonate, oleic acid and octadecene into a three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 100-120 ℃, introducing nitrogen to a positive pressure, keeping the temperature for 5 minutes, continuing heating to 150 ℃, stirring at a constant temperature until the cesium carbonate is dissolved to obtain a cesium oleate precursor solution, and heating to 120 ℃ before use;
Adding lead bromide, zinc bromide and octadecene into another three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 100-120 ℃, introducing nitrogen to a positive pressure, stirring at a constant temperature for 0.5-1 h, adding oleic acid and aminosilane, heating to 150 ℃, and continuously stirring until the lead bromide and the zinc bromide are completely dissolved; then the temperature is increased to 165-170 ℃, and injection is carried outReacting the cesium oleate precursor solution synthesized in the step 1 for 5-10 s, and then cooling the cesium oleate precursor solution to room temperature in an ice water bath to obtain CsPbBr with a passivation layer formed on the surface 3 A quantum dot mother liquor;
And (3) mixing the quantum dot mother liquor obtained in the step (2) with ethyl acetate, carrying out centrifugal cleaning, and dispersing the obtained precipitate in a solvent to obtain a purified quantum dot dispersion liquid.
Further, the aminosilane is 3-aminopropyltrimethoxysilane.
Further, in step 1, the mass to volume ratio of cesium carbonate, oleic acid and octadecene was 0.8g: 2-3 mL:35 to 50mL.
Further, in the step 2, the mass-to-volume ratio of the lead bromide, zinc bromide, octadecene, oleic acid, aminosilane and cesium oleate precursor solution is 0.15g:0.45g: 10-15 mL: 1-1.2 mL: 1-1.2 mL: 1.5-2 mL.
Further, in the step 3, the volume ratio of the ethyl acetate to the quantum dot mother liquor is 2-3: 1.
further, in step 3, the solvent is heptane, hexane or toluene, and the concentration of the obtained quantum dot dispersion is 5-10 mg/mL.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention is in CsPbBr 3 In the synthesis of the quantum dots, zinc bromide and aminosilane are introduced in sequence, so that the silane passivation on the surface of the quantum dots with high quality is realized, the fluorescence quantum efficiency of the obtained quantum dots exceeds 99%, and the quantum dots have high tolerance to high-temperature heat treatment, ethanol solvent and the like after film formation, and can meet the requirement of a solution method for preparing quantum dot light-emitting devices.
2. According to the synthesis method, zinc bromide and lead bromide are added into octadecene at the same time to form a bromine-rich environment, so that CsPbBr is effectively inhibited 3 The generation of defect state in the nanocrystalline and the formation of bromine-rich surface, thereby improving the fluorescence quantum efficiency of the material, and simultaneously, 3-aminopropyl trimethoxy silane is adopted to replace oil ammonia in the prior method, and through the amino group and the halogen ion between the amino group and the halogen ionStrong chemical action in CsPbBr 3 A high-quality silane passivation layer is formed on the surface, so that the stability of the material is improved. The PLQY of the obtained nanocrystal can be increased to 99%, and the thermal stability and the ethanol tolerance of the nanocrystal reach the level of commercial application.
3. The nanocrystalline prepared by the method has obvious difference from the nanocrystalline prepared based on the mercaptosilane ligand in the aspects of ligand materials, preparation process, surface chemical properties and the like, and has different performances on solvent tolerance.
4. The preparation method has the advantages of simple preparation process, short time and good repeatability.
Drawings
FIG. 1, FIG. 2, and FIG. 3 show CsPbBr obtained in the examples 3 、InAP-CsPbBr 3 、BrInAP-CsPbBr 3 Absorption (solid line) versus PL (dashed line) plots for quantum dots.
FIG. 4, FIG. 5, and FIG. 6 are CsPbBr obtained in the examples, respectively 3 、InAP-CsPbBr 3 、BrInAP-CsPbBr 3 PL intensity change of the quantum dot dispersion after 3 hours of addition to absolute ethanol at a volume ratio of 2.
FIG. 7 and FIG. 8 show CsPbBr obtained in example 3 And BrInAP-CsPbBr 3 The PL intensity of quantum dots was changed after heating at 120 ℃ for 24 minutes by spin coating on quartz glass at 2000rpm for 30 s.
FIG. 9 shows BrInAP-CsPbBr obtained in example 1 3 Fourier infrared spectra of quantum dots.
Detailed Description
In order to make the above objects, features and advantages of the present invention more comprehensible, specific embodiments thereof will be described in detail with reference to the following examples. The following is merely exemplary and illustrative of the principles of the present invention, and various modifications, additions and substitutions of similar structures to the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims.
Comparative example 1
The cesium lead bromoperovskite quantum dot is prepared by the following steps:
Adding 0.8g of cesium carbonate, 2.5mL of oleic acid and 40mL of octadecene into a three-necked flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 120 ℃, introducing nitrogen to a positive pressure, keeping the temperature for 5 minutes, continuing heating to 150 ℃, stirring at a constant temperature until the cesium oleate precursor solution is dissolved, and heating to 120 ℃ before use.
Adding 0.2g of lead bromide and 20mL of octadecene into another three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, introducing nitrogen to positive pressure, stirring at constant temperature for 40min, adding 2mL of oleic acid and 2mL of oily ammonia, and continuously stirring until the lead bromide is completely dissolved; heating to 165 ℃ again, injecting 2mL of the cesium oleate precursor solution synthesized in the step 1, reacting for 8s, and cooling to room temperature in an ice-water bath to obtain CsPbBr 3 And (4) quantum dot mother liquor.
And (3) mixing the quantum dot mother liquor obtained in the step (2) with ethyl acetate according to the volume ratio of 1 3 The concentration of the dispersion of quantum dots was 5mg/mL.
Comparative example 2
This example prepares cesium lead bromoperovskite quantum dots as follows:
Same as in comparative example 1.
Adding 0.15g of lead bromide and 10mL of octadecene into another three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 120 ℃, introducing nitrogen to a positive pressure, stirring at a constant temperature for 40min, adding 1mL of oleic acid and 1mL of 3-aminopropyltrimethoxysilane, heating to 150 ℃, and continuously stirring until the lead bromide is completely dissolved; raising the temperature to 165 ℃ again, injecting 1.5mL of the cesium oleate precursor solution synthesized in the step 1, reacting for 8s,then cooling to room temperature in ice-water bath to obtain InAP-CsPbBr 3 And (4) quantum dot mother liquor.
And (3) mixing the quantum dot mother liquor obtained in the step (2) with ethyl acetate according to the volume ratio of 1 3 The concentration of the dispersion of quantum dots was 5mg/mL.
Example 1
The cesium lead bromoperovskite quantum dot is prepared by the following steps:
Same as in comparative example 1.
Adding 0.15g of lead bromide, 0.45g of zinc bromide and 10mL of octadecene into another three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 120 ℃, introducing nitrogen to a positive pressure, stirring at a constant temperature for 40min, adding 1mL of oleic acid and 1mL of 3-aminopropyltrimethoxysilane, heating to 150 ℃, and continuously stirring until the lead bromide and the zinc bromide are completely dissolved; heating to 165 ℃ again, injecting 1.5mL of the cesium oleate precursor solution synthesized in the step 1, reacting for 8s, cooling in an ice water bath to room temperature to obtain BrInAP-CsPbBr 3 And (4) quantum dot mother liquor.
And (3) mixing the quantum dot mother liquor obtained in the step (2) with ethyl acetate according to the volume ratio of 1 3 The concentration of the dispersion liquid of the quantum dots is 5mg/mL;
FIG. 1 shows CsPbBr obtained in comparative example 1 3 The absorption (solid line) and PL (dashed line) curves of the quantum dots, from which CsPbBr can be seen 3 The luminescence peak position of the quantum dot is 511nm.
FIG. 2 is the InAP-CsPbBr obtained in comparative example 2 3 The absorption (solid line) and PL (dotted line) curves of the quantum dots can be seen, and InAP-CsPbBr can be seen from the graph 3 The luminescence peak position of the quantum dot is 511nm.
FIG. 3 shows BrInAP-CsPbBr obtained in example 1 3 The absorption (solid line) and PL (dotted line) curves of the quantum dots can be seen from the graph, and BrInAP-CsPbBr can be seen 3 The luminescence peak position of the quantum dot is 513nm.
By integrating sphere method (the main testing equipment is a Horiba FluoroMax-4 high-sensitivity integrated fluorescence spectrometer, and the configured integrating sphere is Horiba
) CsPbBr was measured at an excitation wavelength of 365nm 3 、InAP-CsPbBr 3 、BrInAP-CsPbBr 3 The PLQY of the quantum dots is 64.71%, 80.11% and 99.34%, respectively.
FIG. 4, FIG. 5, and FIG. 6 are CsPbBr 3 、InAP-CsPbBr 3 、BrInAP-CsPbBr 3 PL change of the quantum dot dispersion after 3 hours of addition to absolute ethanol at a volume ratio of 2. CsPbBr can be seen from the figure 3 The PL intensity of the quantum dots is reduced to 40 percent, and the InAP-CsPbBr 3 And BrInAP-CsPbBr 3 The quantum dot PL intensity hardly changes.
FIG. 7 and FIG. 8 are CsPbBr, respectively 3 And BrInAP-CsPbBr 3 The PL intensity of quantum dots was changed after heating at 120 ℃ for 24 minutes by spin coating on quartz glass at 2000rpm for 30 s. CsPbBr 3 The PL intensity of the quantum dots is almost reduced to 0 after being heated 3 The PL intensity of the quantum dots after heating only drops to 84% of the original.
FIG. 9 shows BrInAP-CsPbBr 3 Fourier infrared spectrum of quantum dot at 908cm -1 、1082cm -1 And 1641cm -1 Nearby exhibits enhanced characteristic absorption at 1195cm -1 New characteristic absorptions appeared, indicating the formation of a large number of Si-O surface chemical structures and new structural features.
The above is merely an exemplary embodiment of the present invention and is not intended to limit the present invention, and any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The method for preparing the cesium-lead-bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation is characterized by comprising the following steps of: firstly, respectively preparing a cesium oleate precursor solution and a lead bromide precursor solution containing zinc bromide, then adding 3-aminopropyl trimethoxy silane into the lead bromide precursor solution, and then injecting the cesium oleate precursor solution into the lead bromide precursor solution by a thermal injection method for reaction, thereby obtaining the cesium lead bromoperovskite quantum dots with the surface formed with a passivation layer, wherein the cesium lead bromoperovskite quantum dots comprise the following steps:
step 1, synthesis of cesium oleate precursor solution
Adding cesium carbonate, oleic acid and octadecene into a three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 100-120 ℃, introducing nitrogen to a positive pressure, keeping the temperature for 5 minutes, continuing heating to 150 ℃, stirring at a constant temperature until the cesium carbonate, the oleic acid and the octadecene are dissolved to obtain a cesium oleate precursor solution, and heating to 120 ℃ before use;
step 2, synthesis of quantum dots
Adding lead bromide, zinc bromide and octadecene into another three-neck flask, introducing nitrogen to remove water and oxygen, vacuumizing, heating to 100-120 ℃, introducing nitrogen to a positive pressure, stirring at a constant temperature for 0.5-1h, adding oleic acid and 3-aminopropyltrimethoxysilane, heating to 150 ℃, and continuously stirring until the lead bromide and the zinc bromide are completely dissolved; heating to 165-170 ℃, injecting the cesium oleate precursor solution synthesized in the step 1, reacting for 5-10s, cooling to room temperature in an ice water bath, and obtaining CsPbBr with a passivation layer formed on the surface 3 A quantum dot mother liquor; wherein the mass volume ratio of the lead bromide, the zinc bromide, the octadecene, the oleic acid, the 3-aminopropyl trimethoxy silane and the cesium oleate precursor solution is 0.15g:0.45g:10 to 15mL:1 to 1.2mL:1 to 1.2mL:1.5 to 2mL;
step 3, purifying the quantum dots
And (3) mixing the quantum dot mother liquor obtained in the step (2) with ethyl acetate, carrying out centrifugal cleaning, and dispersing the obtained precipitate in a solvent to obtain a purified quantum dot dispersion liquid.
2. The method for preparing cesium lead bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation according to claim 1, characterized in that: in the step 1, the mass-to-volume ratio of cesium carbonate, oleic acid and octadecene is 0.8g:2 to 3mL:35 to 50mL.
3. The method for preparing cesium lead bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation according to claim 1, characterized in that: in the step 3, the volume ratio of the ethyl acetate to the quantum dot mother liquor is 2 to 3:1.
4. the method for preparing cesium lead bromine perovskite quantum dots based on in-situ aminosilane and bromide ion passivation according to claim 1, characterized in that: in the step 3, the solvent is heptane, hexane or toluene, and the concentration of the obtained quantum dot dispersion liquid is 5-10mg/mL.
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