CN108893118B - Preparation method of quantum dot and quantum dot - Google Patents

Preparation method of quantum dot and quantum dot Download PDF

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CN108893118B
CN108893118B CN201810755194.4A CN201810755194A CN108893118B CN 108893118 B CN108893118 B CN 108893118B CN 201810755194 A CN201810755194 A CN 201810755194A CN 108893118 B CN108893118 B CN 108893118B
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CN108893118A (en
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王允军
李鑫
厉芙伶
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Suzhou Xingshuo Nanotech Co Ltd
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Abstract

The invention relates to a preparation method of quantum dots, which comprises the following steps: s1, adding a selenium source and a sulfur source into a mixed precursor of a cadmium source and a zinc source to prepare a CdZnSeS core, wherein the feeding amount of the selenium source is larger than that of the sulfur source by the amount of a substance; s2, adding a sulfur source and a cadmium source into the reaction system of S1 to form a CdS transition layer on the surface of the CdZnSeS core; s3, adding a sulfur source and a zinc source into the reaction system of S2 to further form a ZnS shell layer on the surface of the CdS transition layer, and reacting to obtain the quantum dots. The method can obtain the quantum dots with the fluorescence emission wavelength of more than 650 nm.

Description

Preparation method of quantum dot and quantum dot
Technical Field
The application belongs to the field of nanotechnology, and particularly relates to a preparation method of quantum dots and the quantum dots.
Background
The quantum dots have excellent optical characteristics such as high fluorescence quantum efficiency, adjustable emission peak position, narrow half-peak width, spectral purity and the like, and show good application prospects in the technical field of display. By using quantum dots on the LED, the color gamut value can be effectively improved, and better color expression is provided for terminal customers.
In the prior art, the emission wavelength of cadmium quantum dots is generally 450-630 nm, which limits the application of cadmium quantum dots in the wavelength range above 630 nm.
Disclosure of Invention
In view of the above technical problems, the present application provides a preparation method of a large-wavelength quantum dot and a quantum dot.
The application firstly provides a preparation method of quantum dots, which comprises the following steps:
s1, adding a selenium source and a sulfur source into a mixed precursor of a cadmium source and a zinc source to prepare a CdZnSeS core, wherein the dosage of the selenium source is larger than that of the sulfur source by the mass;
s2, adding a sulfur source and a cadmium source into the reaction system of S1 to form a CdS transition layer on the surface of the CdZnSeS core;
s3, adding a sulfur source and a zinc source into the reaction system of S2 to further form a ZnS shell layer on the surface of the CdS transition layer, and reacting to obtain the CdZnSeS/CdS/ZnS quantum dot.
In some preferred embodiments of the present invention, the cadmium source comprises at least one of cadmium oxide, cadmium chloride, cadmium oxalate, cadmium acetate, cadmium carbonate, cadmium stearate, cadmium acetylacetonate, cadmium diethyl, cadmium tetradecanoate, cadmium oleate; the zinc source comprises at least one of zinc oxide, zinc chloride, zinc oxalate, zinc acetate, zinc carbonate, zinc stearate, zinc acetylacetonate, diethyl zinc, zinc undecylenate, zinc myristate, and zinc oleate; the selenium source comprises at least one of selenium simple substance, selenium dioxide, organic phosphine complex of selenium, fatty amine compound of selenium, organic selenium compound and organic selenol compound; the sulfur source includes at least one of elemental sulfur, an organophosphine complex of sulfur, a fatty amine compound of sulfur, an organic sulfur compound, and an organic thiol compound.
In some preferred embodiments of the present invention, the selenium source comprises at least one of selenium powder, selenium dioxide, trioctylphosphine selenium, tributylphosphine selenium, tetradecene solution of selenium, pentadecene solution of selenium, hexadecene solution of selenium, heptadecene solution of selenium, octadecene solution of selenium, selenol, diselenide, selenoether, selenoate, selenoamide, selenophene, and selenazole; the sulfur source comprises at least one of sulfur powder, a tetradecene solution of sulfur, a pentadecene solution of sulfur, a hexadecene solution of sulfur, a heptadecene solution of sulfur, an octadecene solution of sulfur, a n-octylamine solution of sulfur, a tri-n-octylamine solution of sulfur, trioctylphosphine sulfur, tributylphosphine sulfur, 1-octylthiol, 1-dodecanethiol, a mixture of 1-octylthiol and tri-n-octylamine, and a mixture of 1-octylthiol and tributylphosphine.
In some preferred embodiments of the present invention, in step S1, first, a cadmium source, a zinc source, a ligand, and an organic solvent are mixed to prepare a mixed precursor of the cadmium source and the zinc source, and then, a selenium source and a sulfur source are added to prepare a CdZnSeS nucleus.
In some preferred embodiments of the present invention, the ligand comprises at least one of a saturated or unsaturated amine, a saturated or unsaturated acid, and a saturated or unsaturated acid having a carbon number of from about C6 to about C18.
Specifically, the ligand is at least one of saturated or unsaturated acids C14-C18, including at least one of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, decatetraenoic acid, pentadecanoic acid, hexadecenoic acid, heptadecenoic acid, and octadecenoic acid.
In some preferred embodiments of the present invention, the organic solvent comprises at least one of alkanes, alkenes, halogenated hydrocarbons, aromatic hydrocarbons, ethers, amines, ketones, and esters of C10-C22.
Specifically, the organic solvent is C14-C22 aliphatic hydrocarbon compound, including at least one of tetradecene, pentadecene, hexadecene, heptadecene, octadecene, tetradecane, pentadecane, hexadecane, heptadecane, octadecane, nonadecane, eicosane, heneicosane, docosane, tricosane, tetracosane and paraffin oil.
In some preferred embodiments of the present invention, in step S1, the dosage of the selenium source is 1.5 to 9 times of the dosage of the sulfur source, and the total dosage of the cadmium source and the zinc source is 1 to 10 times of the total dosage of the selenium source and the sulfur source.
In some preferred embodiments of the present invention, in step S1, the feeding amount of the cadmium source is 0.2 to 1 times of the feeding amount of the zinc source, the feeding amount of the selenium source is 5 to 9 times of the feeding amount of the sulfur source, and the total feeding amount of the cadmium source and the zinc source is 5 to 10 times of the total feeding amount of the selenium source and the sulfur source.
In the process of preparing the core of the quantum dot, the activity of cadmium ions is higher than that of zinc ions, so after a selenium source and a sulfur source are added, selenium and sulfur are preferentially combined with cadmium, and when the cadmium is combined with the selenium and the sulfur to a certain degree, the concentration of the cadmium is reduced and is converted into the combination of zinc, selenium and sulfur, thereby forming the CdZnSeS core with a gradient core structure.
In some preferred embodiments of the present invention, in step S1, the selenium source and the sulfur source are mixed to prepare a mixed precursor of the selenium source and the sulfur source, and then added to the mixed precursor of the cadmium source and the zinc source to prepare the CdZnSeS nucleus.
In some preferred embodiments of the present invention, a sulfur source and a cadmium source are added simultaneously to the reaction system of S1 to form a CdS transition layer on the surface of the CdZnSeS core.
In some more preferred embodiments of the present invention, the sulfur source and the cadmium source are mixed in advance to prepare a mixed precursor of the sulfur source and the cadmium source, and then the mixed precursor is added into the reaction system of S1 to form the CdS transition layer on the surface of the CdZnSeS core.
In some more preferred embodiments of the present invention, a sulfur source and a cadmium source are added separately and simultaneously to the reaction system of S1 to form a CdS transition layer on the surface of the CdZnSeS nucleus.
In some preferred embodiments of the present invention, in step S2, the amount of sulfur source is 1-2 times the amount of cadmium source.
In some preferred embodiments of the invention, in step S1, a selenium source and a sulfur source are added into a mixed precursor of a cadmium source and a zinc source at 280-340 ℃ to prepare CdZnSeS nucleus; in step S2, adding a sulfur source and a cadmium source into the reaction system of S1 at 240-280 ℃ to form a CdS transition layer on the surface of the CdZnSeS core.
In some preferred embodiments of the present invention, the method for preparing the quantum dot further includes a step of precipitating and purifying the quantum dot prepared in step S3 with a purifying agent. These steps are well known methods in the art and will not be described further herein.
In the application, the preparation process of the quantum dots is carried out in an inert gas atmosphere. In some preferred embodiments of the present invention, the inert gas comprises at least one of nitrogen and argon.
According to the method, the 'raw material feeding sequence and the raw material feeding proportion' are organically combined, firstly, the core CdZnSeS of the quantum dot is synthesized through the step S1, then, the CdS transition layer grows on the core of the quantum dot through the step S2, the emission wavelength of the quantum dot is further regulated and controlled, and finally, the ZnS shell layer is coated, so that the quantum dot with the emission wavelength of 650-670 nm is finally prepared.
In addition, the transition layer and the shell layer are directly coated on the quantum dots by an in-situ reaction method, and the cores of the quantum dots are not required to be separated and purified, so that the solvent consumption is reduced, the experimental operation steps are simplified, and the reaction time is shortened.
The application also provides a quantum dot, which comprises a core, a transition layer and a shell layer, wherein the core is CdZnSeS, the transition layer is CdS, and the shell layer is ZnS. The quantum dot is prepared by the preparation method.
Compared with the prior art, the method has the advantages that:
the quantum dot with the fluorescence emission wavelength of more than 650nm is obtained by taking CdZnSeS as the core of the quantum dot and coating the CdS transition layer and the ZnS shell layer on the surface of the core, the fluorescence emission half-peak width of the quantum dot is narrow (less than or equal to 30nm), the quantum efficiency is high (more than or equal to 75 percent), and the quantum dot can be applied to multiple fields.
In addition, the preparation method is simple and convenient to operate, short in reaction time and high in efficiency, and meets the requirement of quantum dot large-scale production.
Drawings
FIG. 1 is a fluorescence emission spectrum of the quantum dot in example 1;
FIG. 2 is a fluorescence emission spectrum of the quantum dot in example 2;
fig. 3 is a fluorescence emission spectrum of the quantum dot in example 3.
Detailed Description
The technical solutions in the examples of the present application will be described in detail below with reference to the embodiments of the present application. It should be noted that the described embodiments are only some embodiments of the present application, and not all embodiments.
[ example 1 ]
Step 1:
preparation of mixed precursors of sulfur and selenium sources
Respectively taking 9mmol of selenium powder and 1mmol of sulfur powder, and fully mixing the selenium powder and the 1mmol of sulfur powder with 5mL of tributyl phosphine to obtain a mixed precursor (S/Se-TBP, 2M) of a selenium source and a sulfur source;
step 2:
preparation of quantum dots
Mixing 12mmol zinc oleate and 12mmol cadmium oleate, heating to 320 ℃, adding 4ml S/Se-TOP prepared in the step 1, and reacting for 20 min. Then, the temperature was reduced to 270 ℃ and 6mLS-TOP solution (2M, sulfur precursor solution of sulfur powder dissolved in trioctylphosphine) and 80mL of cadmium oleate (0.2M) were added dropwise to the reaction system at the same time, and the reaction was carried out for 20 min. Finally, 2mL of decadithiol and 10mL of diethyl zinc (1M) were added dropwise and reacted for 10 min. And cooling to room temperature, and precipitating and purifying the product by using a conventional method to finally obtain the CdZnSeS/CdS/ZnS quantum dot.
[ example 2 ]
Step 1:
preparation of mixed precursors of sulfur and selenium sources
Respectively taking 9mmol of selenium powder and 1mmol of sulfur powder, and fully mixing the selenium powder and the 1mmol of sulfur powder with 5mL of tributyl phosphine to obtain a mixed precursor (S/Se-TBP, 2M) of a selenium source and a sulfur source;
step 2:
preparation of quantum dots
Mixing 12mmol zinc oleate and 12mmol cadmium oleate, heating to 320 ℃, adding 4ml S/Se-TOP prepared in the step 1, and reacting for 20 min. Then, the temperature was reduced to 270 ℃ and 8mL of S-TOP solution (2M, a sulfur precursor solution of sulfur powder dissolved in trioctylphosphine) and 80mL of cadmium oleate (0.2M) were added dropwise to the reaction system at the same time, and the reaction was carried out for 20 min. Finally, 2mL of decadithiol and 10mL of diethyl zinc (1M) were added dropwise and reacted for 10 min. And cooling to room temperature, and precipitating and purifying the product by using a conventional method to finally obtain the CdZnSeS/CdS/ZnS quantum dot.
[ example 3 ]
Step 1:
preparation of mixed precursors of sulfur and selenium sources
Respectively taking 9mmol of selenium powder and 1mmol of sulfur powder, and fully mixing the selenium powder and the 1mmol of sulfur powder with 5mL of tributyl phosphine to obtain a mixed precursor (S/Se-TBP, 2M) of a selenium source and a sulfur source;
step 2:
preparation of quantum dots
Mixing 12mmol of zinc oleate and 12mmol of cadmium oleate, heating to 320 ℃, adding 8ml of S/Se-TOP prepared in the step 1, and reacting for 20 min. Then, the temperature was reduced to 270 ℃ and 4mL of S-TOP solution (2M, a sulfur precursor solution of sulfur powder dissolved in trioctylphosphine) and 80mL of cadmium oleate (0.2M) were added dropwise to the reaction system at the same time, and the reaction was carried out for 20 min. Finally, 2mL of decadithiol and 10mL of diethyl zinc (1M) were added dropwise and reacted for 10 min. And cooling to room temperature, and precipitating and purifying the product by using a conventional method to finally obtain the CdZnSeS/CdS/ZnS quantum dot.
The raw material charge and experimental test data for examples 1 to 3 are shown in table 1.
TABLE 1
Figure BDA0001726562580000061
The fluorescence emission spectrum of the quantum dot of example 1 is shown in fig. 1, the fluorescence emission spectrum of the quantum dot of example 2 is shown in fig. 2, and the fluorescence emission spectrum of the quantum dot of example 3 is shown in fig. 3. As can be seen from the figure, the fluorescence emission wavelengths of the quantum dots are all above 650nm, and the half-peak width is less than 30 nm.
Although the present disclosure has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent substitutions, will be apparent to those skilled in the art without departing from the spirit of the disclosure, and that no limitations to the present disclosure are intended or should be inferred therefrom.

Claims (5)

1. The preparation method of the quantum dot is characterized by comprising the following steps:
s1, adding a selenium source and a sulfur source into a mixed precursor of a cadmium source and a zinc source at 280-340 ℃ to prepare CdZnSeS nucleus, wherein the feeding amount of the selenium source is 1.5-9 times of the feeding amount of the sulfur source, and the total feeding amount of the cadmium source and the zinc source is 1-10 times of the total feeding amount of the selenium source and the sulfur source;
s2, adding a sulfur source and a cadmium source into the reaction system of S1 at 240-280 ℃ to form a CdS transition layer on the surface of a CdZnSeS core, wherein the feeding amount of the sulfur source is 1-2 times of that of the cadmium source in terms of the amount of substances;
s3, adding a sulfur source and a zinc source into the reaction system of S2 to further form a ZnS shell layer on the surface of the CdS transition layer, and reacting to obtain the CdZnSeS/CdS/ZnS quantum dots, wherein the emission wavelength of the CdZnSeS/CdS/ZnS quantum dots is above 650 nm.
2. The method for preparing a quantum dot according to claim 1, wherein: in step S1, the selenium source and the sulfur source are mixed to prepare a mixed precursor of the selenium source and the sulfur source, and then the mixed precursor is added to the mixed precursor of the cadmium source and the zinc source to prepare the CdZnSeS nucleus.
3. The method for preparing a quantum dot according to claim 1, wherein: in the step S2, a sulfur source and a cadmium source are simultaneously added to the reaction system of S1 to form a CdS transition layer on the surface of the CdZnSeS nucleus.
4. The method for preparing a quantum dot according to any one of claims 1 to 3, wherein: the cadmium source comprises at least one of cadmium oxide, cadmium chloride, cadmium oxalate, cadmium acetate, cadmium carbonate, cadmium stearate, cadmium acetylacetonate, diethyl cadmium, cadmium myristate and cadmium oleate;
the zinc source comprises at least one of zinc oxide, zinc chloride, zinc oxalate, zinc acetate, zinc carbonate, zinc stearate, zinc acetylacetonate, diethyl zinc, zinc undecylenate, zinc myristate and zinc oleate;
the selenium source comprises at least one of a selenium simple substance, selenium dioxide, an organic phosphine complex of selenium, a fatty amine compound of selenium, an organic selenium compound and an organic selenol compound;
the sulfur source comprises at least one of elemental sulfur, an organic phosphine complex of sulfur, a fatty amine compound of sulfur, an organic sulfur compound and an organic thiol compound.
5. A quantum dot, comprising: the quantum dot comprises a core, a transition layer and a shell, wherein the core is CdZnSeS, the transition layer is CdS, the shell is ZnS, the emission wavelength of the CdZnSeS/CdS/ZnS quantum dot is above 650nm, and the quantum dot is prepared by the preparation method of any one of claims 1-4.
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