CN108998002B - Preparation method of quantum dot - Google Patents

Preparation method of quantum dot Download PDF

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CN108998002B
CN108998002B CN201810763212.3A CN201810763212A CN108998002B CN 108998002 B CN108998002 B CN 108998002B CN 201810763212 A CN201810763212 A CN 201810763212A CN 108998002 B CN108998002 B CN 108998002B
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quantum dots
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CN108998002A (en
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王允军
张永乐
张龙珠
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Suzhou Xingshuo Nanotech Co Ltd
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
    • C09K11/621—Chalcogenides
    • C09K11/623—Chalcogenides with zinc or cadmium

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Abstract

The application provides a preparation method of quantum dots, which comprises the following steps: step S1, preparing a core of quantum dots in a first solvent; step S2, extracting cores of the quantum dots from a first solvent; s3, dispersing the cores of the quantum dots in the S2 in a second solvent, and coating a shell layer on the cores of the quantum dots to obtain the quantum dots; wherein the polarity of the second solvent is less than the polarity of the first solvent. According to the method, the core and the shell of the quantum dot are formed in the first solvent and the second solvent respectively, interference of the first solvent to the process of forming the shell can be avoided, so that the shell is coated on the core of the quantum dot, a better coating effect is achieved, and the quantum dot with high fluorescence quantum yield is obtained.

Description

Preparation method of quantum dot
Technical Field
The application belongs to the technical field of nano material preparation, and particularly relates to a preparation method of quantum dots.
Background
In recent years, due to the characteristics of adjustable luminescence wavelength, high luminescence efficiency, strong photochemical stability and the like, the quantum dot is widely applied to the fields of flat panel display, thin film flexible display, LED illumination, fluorescent markers, biomedical imaging and the like, and becomes one of the nano materials with the most potential and development prospect.
In the prior art, when synthesizing the quantum dot, a shell layer is generally coated on the core of the quantum dot so as to improve the luminous performance of the quantum dot. However, the existing method has poor coating effect on the cores of the quantum dots, and the obtained quantum dots have low fluorescence quantum yield and have bad influence on the luminous performance of the quantum dots.
Disclosure of Invention
Aiming at the technical problems, the application provides a preparation method of quantum dots, which aims to solve the problem that the existing common method has poor coating effect on cores of the quantum dots.
According to one aspect of the present application, there is provided a method of preparing a quantum dot, the method comprising:
step S1, preparing a core of quantum dots in a first solvent;
step S2, extracting cores of the quantum dots from a first solvent;
s3, dispersing the cores of the quantum dots in the S2 in a second solvent, and coating a shell layer on the cores of the quantum dots to obtain the quantum dots;
wherein the polarity of the second solvent is less than the polarity of the first solvent.
In this application, the inventors have found that the first solvent aids in forming the core of the quantum dot, but does not facilitate forming the shell layer. According to the preparation method, the core and the shell of the quantum dot are formed by selecting the proper first solvent and the proper second solvent respectively, so that the interference of the first solvent on the formation of the shell can be avoided, and the coating of the shell on the core of the quantum dot is facilitated. And the inventors have unexpectedly found that quantum dots with shell coating obtained in this way have a higher fluorescence quantum yield.
In some preferred embodiments of the invention, the core of the quantum dot is copper indium sulfide and the shell is zinc sulfide. In the present application, the shell layer of the quantum dot may be one or more zinc sulfide shells. The inventor finds that the optional multilayer zinc sulfide shell layer is grown on the surface of the core of the copper indium sulfide quantum dot by a continuous ion adsorption method, thereby being beneficial to the copper indium sulfide quantum dot to obtain better stability and better optical property.
In some preferred embodiments of the present invention, step S1 comprises: and mixing an indium source, a copper source and a sulfur source with a first solvent, and preparing the cores of the copper-indium-sulfur quantum dots at a first temperature. The means for mixing the indium source, the copper source and the sulfur source with the first solvent includes, but is not limited to, stirring, ultrasonic treatment, heating and the like.
In this application, the first temperature is selected to be in the range of 180-220 ℃. Since the indium source, copper source, sulfur source, and first solvent selected for synthesizing the cores of the quantum dots are different, the required synthesis conditions are also different. The inventors found that the reaction can be performed at a proper temperature according to the kind of the raw material selected and the boiling point of the first solvent, and the particle size and wavelength of the desired target product to be obtained, thereby obtaining the desired copper indium sulfide quantum dot.
In some preferred embodiments of the present invention, the indium source comprises at least one of indium acetate, indium carbonate, indium nitrate, indium chloride, indium iodide, indium bromide, indium perchlorate, indium stearate, indium tetradecanoate; the copper source comprises at least one of cuprous chloride, cuprous bromide and cuprous iodide; the sulfur source comprises at least one of elemental sulfur, an organic amine solution of elemental sulfur, an alkyl mercaptan, a trialkylphosphine sulfide, a trialkenylphosphine sulfide, an alkylamino sulfide, and an alkenyl amino sulfide.
In some preferred embodiments of the present invention, the first solvent is at least one of saturated or unsaturated amines having 6 or more carbon atoms, and more preferably at least one of hexylamine, heptylamine, octylamine, trioctylamine, nonylamine, dodecylamine, undecylamine, dodecylamine, tridecylamine, tetramine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, oleylamine, decadecylamine, undecylenamine, dodecenamine, tridecylamine, tetradecylenamine, pentadecylenamine, hexadecylenamine, heptadecylenamine, octadecylamine. The inventors have found that this first solvent helps to form a core of copper indium sulfide quantum dots, helping to obtain quantum dots with higher fluorescence quantum yields.
In some preferred embodiments of the present invention, step S2 includes a process of extracting cores of quantum dots from the first solvent. The inventors found that the first solvent used in synthesizing the core of the quantum dot is not conducive to the formation of the shell layer. Therefore, the core of the quantum dot is extracted from the first solvent, and the interference of the first solvent on the process of forming the shell layer afterwards can be avoided.
In some preferred embodiments of the present invention, the solvents used in the extraction process are all conventional solvents used in the prior art for extracting quantum dots. Preferably, the extraction solvent includes at least one of saturated alkanes having 6.ltoreq.carbon atoms.ltoreq.9 and at least one of saturated monohydric alcohols having 1.ltoreq.carbon atoms.ltoreq.6. Further preferably, the extraction solvent comprises n-hexane, n-heptane, n-octane, ethanol, isopropanol, and mixtures thereof.
In some preferred embodiments of the present invention, step S3 includes: dispersing the core of the quantum dot in the S2 in a second solvent, adding a precursor substance required by synthesizing the shell layer of the quantum dot at a second temperature, and coating the shell layer on the core of the quantum dot to obtain the quantum dot. The manner of dispersing the cores of the quantum dots in S2 in the second solvent also includes, but is not limited to, stirring, ultrasonic treatment, heating, and the like.
In some preferred embodiments of the invention, the precursor materials required to synthesize the shell layer of the quantum dot include at least a zinc source. Preferably, the zinc source comprises at least one of zinc fluoride, zinc chloride, zinc bromide, zinc iodide, zinc carbonate, zinc sulfate, zinc nitrate, zinc perchlorate, zinc acetate, zinc carboxylate, dimethyl zinc, diethyl zinc, zinc acetylacetonate, zinc stearate, zinc oleate, zinc decanate, zinc undecylenate, zinc tetradecanoate, zinc hexadecanoate, and zinc diethyldithiocarbamate.
In some preferred embodiments of the invention, the precursor materials required to synthesize the shell layer of the quantum dot further include a sulfur source. Preferably, the sulfur source comprises at least one of elemental sulfur, an organic amine solution of elemental sulfur, an alkyl mercaptan, a trialkylphosphine sulfide, a trialkenylphosphine sulfide, an alkylamino sulfide, an alkenylamino sulfide. Wherein, when the sulfur source is selected as the organic amine solution of elemental sulfur, the volume ratio of the organic amine solution to the second solvent is 1 (1-10).
In this application, the second temperature is selected to be in the range of 180-260 ℃. In some preferred embodiments of the invention, a zinc source and optionally a sulfur source are added to the second solvent in which the quantum dot cores are dispersed, optionally repeating this step, coating one or more zinc sulfide shell layers. The inventors found that the shell coating of the quantum dots was performed with gradually increasing cladding temperature. As the quantum dots grow larger continuously, in the step of coating the shell layer, the reaction temperature needs to be increased to help the shell layer to form, so that the quantum dots with the shell layer coating with good uniformity are obtained.
In some preferred embodiments of the present invention, the second solvent is at least one of alkanes, alkenes, halogenated hydrocarbons, aromatic hydrocarbons, ethers, amines, ketones, esters, and more preferably at least one of n-heptane, 1-octadecane, 1-heptadecane, 1-hexadecane, 1-octadecene, 1-heptadecene, 1-hexadecene, 1-tetradecene, 1-dodecene, isotriacontane, and paraffinic oils. The inventors have found that the second solvent is more advantageous for forming the shell layer of the quantum dot than the first solvent. According to the preparation method, the cores of the quantum dots extracted from the first solvent are dispersed into the second solvent, and the coating process of the shell layer is completed in the second solvent, so that the quantum dots with good coating effect can be obtained.
In this application, in order to avoid adverse effects of moisture or oxygen on the reaction, the indium source, zinc source, phosphorus source, and first and second solvents used in the present invention are all subjected to water removal and drying treatment before participating in the reaction. In addition, the preparation method of the invention is the same as the reaction environment required in the preparation of quantum dots in the prior art. Before the reaction, the moisture and oxygen in the reaction vessel were removed using an inert gas atmosphere or an air atmosphere from which moisture and oxygen had been removed, and each reaction process in the experiment was carried out under the protection of the inert gas atmosphere. Wherein the inert gas atmosphere comprises at least one of nitrogen, argon, or a rare gas.
In some preferred embodiments of the present invention, in order to further improve the optical properties of the prepared quantum dots, the method further comprises a step of removing unreacted raw materials and other impurities, specifically separation and purification, after obtaining the quantum dots. The inventor finds that the quantum dot with higher purity can be obtained by cooling the final reaction liquid obtained by the method to room temperature, adding an extractant, separating to obtain an extract, and then adding acetone for precipitation.
According to another aspect of the present application, there is provided a quantum dot including a core of the quantum dot, the core of the quantum dot being copper indium sulfide, and a shell layer coated on the core of the quantum dot, the shell layer being zinc sulfide, the quantum dot being produced by the above production method.
Compared with the prior art, the advantage of this application mainly lies in:
according to the method, the core and the shell of the quantum dot are formed in the first solvent and the second solvent respectively, so that the interference of the first solvent to the process of forming the shell is avoided, the shell is coated on the core of the quantum dot, and a good coating effect is achieved. The quantum dot prepared by the method has higher fluorescence quantum yield.
Drawings
FIG. 1 is a graph of the ultraviolet absorption-fluorescence emission spectrum of a quantum dot in example 1 of the present application;
FIG. 2 is a graph of the ultraviolet absorption-fluorescence emission spectrum of the quantum dots of example 2 of the present application;
FIG. 3 is a graph of the ultraviolet absorption-fluorescence emission spectrum of the quantum dots in example 3 of the present application.
Detailed Description
The technical solutions in the examples of the present application will be described in detail below in conjunction with the implementation manners 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
Preparation of CuInS/ZnS quantum dots
1) 150mg of InCl under the protection of inert gas 3 30mg of CuCl, 100mg of sulfur powder and 10mL of oleylamine are mixed, and cores of CuInS quantum dots are prepared at 200 ℃;
2) Extracting the cores of the CuInS quantum dots from the reaction system of 1), wherein the extraction mode is known;
3) Dispersing the core of the CuInS quantum dot of 2) in 10mL of 1-hexadecene, heating to 240 ℃, adding zinc oleate (0.5M, 2 mL) and 1mL of dodecyl mercaptan, and forming a ZnS shell layer on the core of the CuInS quantum dot to obtain the CuInS/ZnS quantum dot.
FIG. 1 is a graph of ultraviolet absorption-fluorescence emission spectrum of CuInS/ZnS quantum dots prepared in example 1.
Example 2
Preparation of CuInS/ZnS quantum dots
1) 150mg of InCl under the protection of inert gas 3 、40mg CuBr, 10mL of dodecyl mercaptan and 10mL of hexadecenamine are mixed, and cores of CuInS quantum dots are prepared at 220 ℃;
2) Extracting the cores of the CuInS quantum dots from the reaction system of 1), wherein the extraction mode is known;
3) The cores of the CuInS quantum dots of 2) were dispersed in 10mL 1-hexadecene, and a 1-octadecene solution (4 mL) of zinc stearate (1 g) was added at 220 ℃. Then, the temperature was raised to 240℃and a solution of zinc stearate (1 g) in 1-octadecene (4 mL) and a solution of sulfur powder (50 mg) in trioctylphosphine (1 mL) were added to form two ZnS shell layers on the cores of the CuInS quantum dots, thereby obtaining CuInS/ZnS quantum dots.
FIG. 2 is a graph of the ultraviolet absorption-fluorescence emission spectrum of the CuInS/ZnS quantum dots prepared in example 2.
Example 3
Preparation of CuInS/ZnS quantum dots
1) Under the protection of inert gas, 280mg of In (OAc) 3 30mg CuI, 4mL sulfur in oleylamine solution (0.4M) and 20mL octadecylamine were mixed to prepare cores of CuInS quantum dots at 180 ℃;
2) Extracting the cores of the CuInS quantum dots from the reaction system of 1), wherein the extraction mode is known;
3) Dispersing the core of the CuInS quantum dot of 2) in 20mL of 1-hexadecene, heating to 240 ℃, adding 1-octadecene solution (4 mL) of zinc stearate (1 g) and 4mL of oleylamine solution (0.4M) of sulfur, and forming a ZnS shell layer on the core of the CuInS quantum dot to obtain the CuInS/ZnS quantum dot.
FIG. 3 is a graph of the ultraviolet absorption-fluorescence emission spectrum of the CuInS/ZnS quantum dots prepared in example 3.
Comparative example 1
The preparation process of CuInS quantum dot core in comparative example 1 was the same as in example 1, except for the process of coating the shell layer.
Preparation of CuInS/ZnS quantum dots
1) 150mg of InCl under the protection of inert gas 3 30mg of CuCl, 100mg of sulfur powder and 10mL of oleylamine are mixed, and cores of CuInS quantum dots are prepared at 200 ℃;
2) And adding zinc oleate (0.5M, 2 mL) and 1mL of dodecyl mercaptan into the reaction system of the step 1) at 240 ℃ to form a ZnS shell layer on the core of the CuInS quantum dot, thereby obtaining the CuInS/ZnS quantum dot.
Comparative example 2
The preparation process of CuInS quantum dot core in comparative example 2 was the same as in example 2, except for the process of coating the shell layer.
Preparation of CuInS/ZnS quantum dots
1) 150mg of InCl under the protection of inert gas 3 Mixing 40mg of CuBr, 10mL of dodecyl mercaptan and 10mL of hexadecylamine, and preparing the core of the CuInS quantum dot at 220 ℃;
2) To the reaction system of 1), a 1-octadecene solution (4 mL) of zinc stearate (1 g) was added. Then, the temperature was raised to 240℃and a solution of zinc stearate (1 g) in 1-octadecene (4 mL) and a solution of sulfur powder (50 mg) in trioctylphosphine (1 mL) were added to form two ZnS shell layers on the cores of the CuInS quantum dots, thereby obtaining CuInS/ZnS quantum dots.
Comparative example 3
The preparation process of CuInS quantum dot core in comparative example 3 was the same as in example 3, except for the process of coating the shell layer.
Preparation of CuInS/ZnS quantum dots
1) Under the protection of inert gas, 280mg of In (OAc) 3 30mg CuI, 4mL sulfur in oleylamine solution (0.4M) and 20mL octadecylamine were mixed to prepare cores of CuInS quantum dots at 180 ℃;
2) Zinc stearate (1 g) 1-octadecene solution (4 mL) and 4mL sulfur oleylamine solution (0.4M) are added into the reaction system of the 1) at 240 ℃ to form ZnS shell layers on cores of the CuInS quantum dots, so as to obtain the CuInS/ZnS quantum dots.
The quantum dots obtained in step 3) in examples 1 to 3 and the quantum dots obtained in step 2) in comparative examples 1 to 3 were purified by a conventional method, respectively, and fluorescence properties of each sample after purification were tested.
The test results are shown in Table 1.
TABLE 1
From the above test data, it can be seen that the quantum dots obtained by the method of the present application have higher fluorescence quantum yields. By extracting the cores of the quantum dots from the first solvent, the interference of the first solvent on the formation of the shell layers can be avoided, so that the shell layers are coated on the cores of the quantum dots more favorably, and a better coating effect is realized.
The quantum dot with the shell coating prepared by the method has higher fluorescence quantum yield, so the method is extremely beneficial to improving the luminous performance of the quantum dot, thereby meeting the application requirements of the quantum dot in multiple fields.
While the present disclosure has been particularly shown and described with reference to the preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.

Claims (1)

1. The preparation method of the quantum dot is characterized by comprising the following steps of:
1) 150mg of InCl under the protection of inert gas 3 30mg of CuCl, 100mg of sulfur powder and 10mL of oleylamine are mixed, and cores of CuInS quantum dots are prepared at 200 ℃;
2) Extracting the cores of the CuInS quantum dots from the reaction system of 1);
3) Dispersing the core of the CuInS quantum dot of 2) in 10mL of 1-hexadecene, heating to 240 ℃, adding 2mL of 0.5M zinc oleate and 1mL of dodecyl mercaptan, and forming a ZnS shell layer on the core of the CuInS quantum dot to obtain the CuInS/ZnS quantum dot.
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CN111662703B (en) * 2020-05-09 2023-11-03 中国科学院广州能源研究所 CuInS 2 Green fluorescent quantum dot with/ZnS/ZnS multilayer core-shell structure and preparation method thereof
CN115924958A (en) * 2022-11-15 2023-04-07 华北水利水电大学 Dispersible zinc oxide or zinc sulfide nano-particles for lubricating grease and preparation method and application thereof

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