CN108998002A - The preparation method of quantum dot - Google Patents

The preparation method of quantum dot Download PDF

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CN108998002A
CN108998002A CN201810763212.3A CN201810763212A CN108998002A CN 108998002 A CN108998002 A CN 108998002A CN 201810763212 A CN201810763212 A CN 201810763212A CN 108998002 A CN108998002 A CN 108998002A
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quantum dot
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core
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CN108998002B (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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    • 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 kind of preparation method of quantum dot, comprising: step S1 prepares the core of quantum dot in the first solvent；Step S2 extracts the core of quantum dot from the first solvent；The core of quantum dot in S2 is dispersed in the second solvent by step S3, and coats shell on the core of quantum dot, obtains quantum dot；Wherein, polarity of the polarity of the second solvent less than the first solvent.The application is respectively formed the core and shell of quantum dot in the first solvent and the second solvent, can to avoid the first solvent to formed shell process interference, to help to coat shell on the core of quantum dot, better covered effect is realized, thus to obtain the high quantum dot of fluorescence quantum yield.

Description

The preparation method of quantum dot
Technical field
The application belongs to technical field of nanometer material preparation more particularly to a kind of preparation method of quantum dot.
Background technique
In recent years, quantum dot is wide due to the features such as its emission wavelength is adjustable, luminous efficiency is high, photochemical stability is strong It is general be applied to FPD, the fields such as thin film flexible is shown, LED illumination, fluorescent marker and biomedical imaging, become most Have one of potentiality and the nano material of development prospect.
The prior art is when synthesizing quantum dot, it will usually shell is coated on the core of quantum dot, to improve the hair of quantum dot Optical property.However, covered effect and bad, the fluorescence quantum yield of obtained quantum dot of the existing method to the core of quantum dot It is lower, it has a adverse impact to the luminescent properties of quantum dot.
Summary of the invention
In view of the above technical problems, the application provides a kind of preparation method of quantum dot, to solve existing common method pair The problem of the covered effect difference of the core of quantum dot.
According to the one aspect of the application, a kind of preparation method of quantum dot is provided, the preparation method includes:
Step S1 prepares the core of quantum dot in the first solvent；
Step S2 extracts the core of quantum dot from the first solvent；
The core of quantum dot in S2 is dispersed in the second solvent by step S3, and coats shell on the core of quantum dot, is obtained To quantum dot；
Wherein, polarity of the polarity of the second solvent less than the first solvent.
In this application, it inventors have found that the first solvent contributes to form the core of quantum dot, but is detrimental to form shell Layer.By the preparation method of the application, suitable first solvent and the second solvent is selected to be respectively formed the core and shell of quantum dot, Can to avoid the first solvent to formed shell interference, to help to coat shell on the core of quantum dot.And invention people's will Outer discovery, the quantum dot with shell cladding obtained in this way, fluorescence quantum yield with higher.
In some preferred embodiments of the invention, the core of quantum dot is indium sulphur, and shell is zinc sulphide.In this application, The shell of quantum dot can be the zinc sulphide shell of one layer or multilayer.Inventors have found that can by continuous ionic absorption method The multilayer zinc sulphide shell of choosing is grown in the surface of the core of indium sulphur quantum dot, and it is preferably steady to be conducive to the acquisition of indium sulphur quantum dot Qualitative and more excellent optical property.
In some preferred embodiments of the invention, step S1 includes: to mix indium source, copper source, sulphur source with the first solvent, The core of indium sulphur quantum dot is prepared at a temperature of first.Wherein, the mode that indium source, copper source, sulphur source are mixed with the first solvent include but It is not limited to the means such as stirring, ultrasound, heating.
In this application, the selection of the first temperature is within the scope of 180-220 DEG C.Due to synthesizing the selected indium of core of quantum dot Source, copper source, sulphur source and the first solvent are different, therefore required synthesis condition is also had nothing in common with each other.Inventors have found that can be with According to the partial size and wavelength of the target product of the boiling point and desired acquisition of selected raw material type and the first solvent, choosing It selects and is reacted at a suitable temperature, thus indium sulphur quantum dot required for obtaining.
In some more preferred embodiments of the present invention, indium source includes indium acetate, carbonic acid indium, indium nitrate, inidum chloride, iodate At least one of indium, indium bromide, perchloric acid indium, stearic acid indium, tetradecylic acid indium；Copper source includes stannous chloride, cuprous bromide, iodine Change at least one of cuprous；Sulphur source includes elemental sulfur, the Amine Solutions of elemental sulfur, alkyl hydrosulfide, vulcanization trialkyl phosphine, sulphur Change at least one of trialkenyl phosphine, alkyl amino sulfide, alkenyl amino sulfide.
In some more preferred embodiments of the present invention, the first solvent is the saturation or unsaturated amine of carbon atom number >=6 At least one of, it is further preferred that include hexylamine, heptyl amice, octylame, trioctylamine, nonyl amine, ten amine, ten enamines, undecylamine, Hendecene amine, lauryl amine, laurylene amine, tridecyl amine, tridecylene amine, tetradecy lamine, pentadecyl amine, 15 enamines, cetylamine, 17 Amine, octadecylamine, octadecenyl amine, oleyl amine, ten enamines, hendecene amine, laurylene amine, tridecylene amine, tetradecene amine, 15 enamines, At least one of hexadecylene amine, 17 enamines, octadecenyl amine.Inventors have found that first solvent contributes to form indium sulphur The core of quantum dot helps to obtain the quantum dot with compared with high-fluorescence quantum yield.
In some preferred embodiments of the invention, step S2 includes extracting the core of quantum dot from the first solvent Process.Inventors have found that used first solvent is unfavorable for the formation of shell when the core of synthesis quantum dot.Therefore, it will measure Son point core extracted from the first solvent, can to avoid the first solvent to later formed shell process interference.
In some more preferred embodiments of the present invention, solvent used in extraction process is extracted amount in the prior art Used Conventional solvents when son point.Preferably, Extraction solvent includes at least one in the saturated alkane of 6≤carbon atom number≤9 At least one of the saturated monohydroxy alcohol of kind and 1≤carbon atom number≤6.It is further preferred that Extraction solvent includes n-hexane, just Heptane, normal octane, ethyl alcohol, isopropanol and its mixture.
In some preferred embodiments of the invention, step S3 includes: that the core of quantum dot in S2 is dispersed in the second solvent, Precursor substance required for the shell of synthesis quantum dot is added at the second temperature, coats shell on the core of quantum dot, obtains Quantum dot.Wherein, the core of quantum dot in S2 the mode in the second solvent is dispersed in equally also to include but is not limited to stirring, surpass The means such as sound, heating.
In some more preferred embodiments of the present invention, synthesizes precursor substance required for the shell of quantum dot and include at least Zinc source.Preferably, zinc source includes zinc fluoride, zinc chloride, zinc bromide, zinc iodide, zinc carbonate, zinc sulfate, zinc nitrate, perchloric acid Zinc, zinc acetate, zinc polycarboxylate, zinc methide, diethyl zinc, zinc acetylacetonate, zinc stearate, zinc oleate, ten sour zinc, undecenoic acid At least one of zinc, tetradecylic acid zinc, hexadecylic acid zinc and diethyldithio-carbamate zinc.
In some more preferred embodiments of the present invention, synthesizing precursor substance required for the shell of quantum dot further includes sulphur Source.Preferably, sulphur source includes elemental sulfur, the Amine Solutions of elemental sulfur, alkyl hydrosulfide, vulcanization trialkyl phosphine, vulcanization trialkenyl At least one of phosphine, alkyl amino sulfide, alkenyl amino sulfide.Wherein, when sulphur source is selected as the organic amine of elemental sulfur When solution, the volume ratio with the second solvent is 1:(1~10).
In this application, second temperature selection is within the scope of 180-260 DEG C.In some more preferred embodiments of the present invention In, zinc source and optional sulphur source, this step of selective repetition, cladding are added into the second solvent of the core for being dispersed with quantum dot One layer or multilayer zinc sulphide shell.Inventors have found that the shell cladding of quantum dot is the case where clad temperature is gradually increased Lower progress.Since quantum dot becomes larger in constantly growth, in the step of coating shell, needs to improve reaction temperature and help shell Layer is formed, so that obtaining the uniformity preferably has the quantum dot of shell cladding.
In some more preferred embodiments of the present invention, the second solvent be alkane, alkene, halogenated hydrocarbons, aromatic hydrocarbon, ethers, At least one of amine, ketone, esters, it is further preferred that including normal heptane, 1- octadecane, 1- heptadecane, 1- 16 Alkane, 1- octadecene, 1- heptadecene, cetene, tetradecene, 1- dodecylene, isotriacontane, in paraffin oil It is at least one.Inventors have found that being more conducive to forming the shell of quantum dot for the second solvent is compared with the first solvent.Pass through this The preparation method of application will be distributed in the second solvent from the core of the quantum dot extracted in the first solvent, and molten second The cladding process that shell is completed in agent, can obtain the good quantum dot of covered effect.
In this application, in order to avoid moisture or oxygen are to the adverse effect of reaction, indium source used in the present invention, zinc Source, phosphorus source and the first solvent, the second solvent are all removed water and have been dried before participating in reaction.In addition, of the invention Preparation method it is identical as required reaction environment when preparing quantum dot in the prior art.Before reactions, using inertia Gas atmosphere, or moisture and oxygen in the air atmosphere removal reaction vessel of moisture and oxygen have been removed, and make in experiment Each reaction process all carried out under the protection of inert gas atmosphere.Wherein, inert gas atmosphere include nitrogen, argon gas or At least one of rare gas.
In some preferred embodiments of the invention, in order to further increase the optical property of prepared quantum dot, To after above-mentioned quantum dot, further includes the steps that removing unreacted raw material and other impurities, specifically include separation and purification.Invention People's discovery, the end reaction liquid obtained by the above method is cooled to room temperature, addition extractant, isolated extract liquor, then Acetone precipitation, the available higher quantum dot of purity is added.
According to further aspect of the application, a kind of quantum dot is provided, the core of the core including quantum dot, the quantum dot is Indium sulphur, and the shell being coated on the core of quantum dot, the shell are zinc sulphide, and the quantum dot is by above-mentioned preparation method system ?.
Compared with prior art, it is essentially consisted in the advantages of the application:
It is molten to avoid first by being respectively formed the core and shell of quantum dot in the first solvent and the second solvent by the application Agent realizes preferable covered effect to help to coat shell on the core of quantum dot to the interference for forming shell process.It is logical Cross the quantum dot that this method is prepared, fluorescence quantum yield with higher.
Detailed description of the invention
Fig. 1 is UV absorption-fluorescence emission spectrogram of compound of quantum dot in the embodiment of the present application 1；
Fig. 2 is UV absorption-fluorescence emission spectrogram of compound of quantum dot in the embodiment of the present application 2；
Fig. 3 is UV absorption-fluorescence emission spectrogram of compound of quantum dot in the embodiment of the present application 3.
Specific embodiment
Below in conjunction with the application embodiment, technical solutions in the embodiments of the present application is described in detail.It answers It is noted that described embodiment is only a part of embodiment of the application, rather than whole embodiments.
Embodiment 1
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 150mg InCl3, 30mg CuCl, 100mg sulphur powder mixed with 10mL oleyl amine, The core of CuInS quantum dot is prepared at 200 DEG C；
2) core of CuInS quantum dot is extracted from reaction system 1), extracting mode is well known；
3) 2) core of CuInS quantum dot is dispersed in 10mL cetene, is warming up to 240 DEG C, zinc oleate is added (0.5M, 2mL) and 1mL lauryl mercaptan forms ZnS shell on the core of CuInS quantum dot, obtains CuInS/ZnS quantum dot.
Fig. 1 is the UV absorption-fluorescence emission spectrogram of compound for the CuInS/ZnS quantum dot that embodiment 1 is prepared.
Embodiment 2
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 150mg InCl3, 40mg CuBr, 10mL lauryl mercaptan and 10mL hexadecylene amine Mixing, prepares the core of CuInS quantum dot at 220 DEG C；
2) core of CuInS quantum dot is extracted from reaction system 1), extracting mode is well known；
3) 2) core of CuInS quantum dot is dispersed in 10mL cetene, zinc stearate is added at 220 DEG C The 1- octadecene solution (4mL) of (1g).Then, 240 DEG C are warming up to, the 1- octadecene solution (4mL) of zinc stearate (1g) is added With the tri octyl phosphine solution (1mL) of sulphur powder (50mg), two layers of ZnS shell is formed on the core of CuInS quantum dot, obtains CuInS/ ZnS quantum dot.
Fig. 2 is the UV absorption-fluorescence emission spectrogram of compound for the CuInS/ZnS quantum dot that embodiment 2 is prepared.
Embodiment 3
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 280mg In (OAc)3, 30mg CuI, 4mL sulphur oleyl amine solution (0.4M) with The mixing of 20mL octadecylamine, prepares the core of CuInS quantum dot at 180 DEG C；
2) core of CuInS quantum dot is extracted from reaction system 1), extracting mode is well known；
3) 2) core of CuInS quantum dot is dispersed in 20mL cetene, is warming up to 240 DEG C, stearic acid is added The 1- octadecene solution (4mL) of zinc (1g) and the oleyl amine solution (0.4M) of 4mL sulphur form ZnS shell on the core of CuInS quantum dot Layer, obtains CuInS/ZnS quantum dot.
Fig. 3 is the UV absorption-fluorescence emission spectrogram of compound for the CuInS/ZnS quantum dot that embodiment 3 is prepared.
Comparative example 1
Identical in the preparation process with embodiment 1 of CuInS quantum dot core in comparative example 1, different is encasement The process of layer.
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 150mg InCl3, 30mg CuCl, 100mg sulphur powder mixed with 10mL oleyl amine, The core of CuInS quantum dot is prepared at 200 DEG C；
2) at 240 DEG C, zinc oleate (0.5M, 2mL) and 1mL lauryl mercaptan are added into reaction system 1), ZnS shell is formed on the core of CuInS quantum dot, obtains CuInS/ZnS quantum dot.
Comparative example 2
Identical in the preparation process with embodiment 2 of CuInS quantum dot core in comparative example 2, different is encasement The process of layer.
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 150mg InCl3, 40mg CuBr, 10mL lauryl mercaptan and 10mL hexadecylene amine Mixing, prepares the core of CuInS quantum dot at 220 DEG C；
2) the 1- octadecene solution (4mL) of zinc stearate (1g) is added into reaction system 1).Then, 240 are warming up to DEG C, the 1- octadecene solution (4mL) of zinc stearate (1g) and the tri octyl phosphine solution (1mL) of sulphur powder (50mg) is added, in CuInS Two layers of ZnS shell is formed on the core of quantum dot, obtains CuInS/ZnS quantum dot.
Comparative example 3
Identical in the preparation process with embodiment 3 of CuInS quantum dot core in comparative example 3, different is encasement The process of layer.
The preparation of CuInS/ZnS quantum dot
1) under inert gas protection, by 280mg In (OAc)3, 30mg CuI, 4mL sulphur oleyl amine solution (0.4M) with The mixing of 20mL octadecylamine, prepares the core of CuInS quantum dot at 180 DEG C；
2) at 240 DEG C, the 1- octadecene solution (4mL) and 4mL of zinc stearate (1g) are added into reaction system 1) The oleyl amine solution (0.4M) of sulphur forms ZnS shell on the core of CuInS quantum dot, obtains CuInS/ZnS quantum dot.
Step 2) in the quantum dot, comparative example 1-3 of step 3) acquisition in embodiment 1-3 is obtained respectively using conventional method Quantum dot purified, the photoluminescent property of test each sample after purification.
Test result such as table 1.
Table 1
The fluorescence quantum yield that can be seen that the quantum dot that the present processes obtain from above-mentioned test data is higher.It is logical Cross and extract the core of quantum dot from the first solvent, can to avoid the first solvent to formed shell interference, to more have Help coat shell on the core of quantum dot, realizes better covered effect.
The quantum dot fluorescence quantum yield with higher with shell cladding prepared by the application method, therefore, This method is very advantageous in the luminescent properties for improving quantum dot, to meet quantum dot in multi-field application demand.
Although inventor has done more detailed elaboration to the technical solution of the application and has enumerated, it should be understood that for For those skilled in the art, above-described embodiment is modified and/or the flexible or equivalent alternative solution of use is obvious , cannot all be detached from the essence of the application spirit, the term occurred in the application be used for elaboration to technical scheme and Understand, the limitation to the application can not be constituted.

Claims (10)

1. a kind of preparation method of quantum dot, which is characterized in that the preparation method includes:
Step S1 prepares the core of quantum dot in the first solvent；
Step S2 extracts the core of the quantum dot from the first solvent；
The core of quantum dot in the S2 is dispersed in the second solvent by step S3, and coats shell on the core of quantum dot, is obtained To quantum dot；
Wherein, the polarity of second solvent is less than the polarity of first solvent.
2. preparation method according to claim 1, which is characterized in that the core of the quantum dot is indium sulphur, and shell is sulphur Change zinc.
3. preparation method according to claim 2, which is characterized in that the step S1 includes:
Indium source, copper source, sulphur source are mixed with the first solvent, prepare the core of indium sulphur quantum dot at the first temperature；
Preferably, first temperature is 180-220 DEG C；
Preferably, the indium source include indium acetate, it is carbonic acid indium, indium nitrate, inidum chloride, indium iodide, indium bromide, perchloric acid indium, hard At least one of resin acid indium, tetradecylic acid indium, copper source include stannous chloride, cuprous bromide, at least one in cuprous iodide Kind, the sulphur source include elemental sulfur, the Amine Solutions of elemental sulfur, alkyl hydrosulfide, vulcanization trialkyl phosphine, vulcanization trialkenyl phosphine, At least one of alkyl amino sulfide, alkenyl amino sulfide.
4. according to claim 1 to preparation method described in any one of 3, which is characterized in that first solvent is carbon atom At least one of the saturation of number >=6 or unsaturated amine；
Preferably, first solvent includes hexylamine, heptyl amice, octylame, trioctylamine, nonyl amine, ten amine, ten enamines, undecylamine, 11 Enamine, lauryl amine, laurylene amine, tridecyl amine, tridecylene amine, tetradecy lamine, pentadecyl amine, 15 enamines, cetylamine, heptadecyl-amine, ten Eight amine, octadecenyl amine, oleyl amine, ten enamines, hendecene amine, laurylene amine, tridecylene amine, tetradecene amine, 15 enamines, hexadecylene At least one of amine, 17 enamines, octadecenyl amine.
5. preparation method according to claim 1, which is characterized in that the step S3 includes:
The core of quantum dot in the S2 is dispersed in the second solvent, is added needed for the shell of synthesis quantum dot at the second temperature The precursor substance wanted coats shell on the core of quantum dot, obtains quantum dot；
Preferably, the second temperature is 180-260 DEG C.
6. preparation method according to claim 5, which is characterized in that precursor required for the shell of the synthesis quantum dot Substance includes zinc source.
7. preparation method according to claim 5, which is characterized in that precursor required for the shell of the synthesis quantum dot Substance includes zinc source and sulphur source.
8. preparation method according to claim 7, which is characterized in that the sulphur source is the Amine Solutions of elemental sulfur, institute The volume ratio of the Amine Solutions and the second solvent of stating elemental sulfur is 1:(1~10).
9. according to claim 1, preparation method described in any one of 5 to 8, which is characterized in that second solvent be alkane, At least one of alkene, halogenated hydrocarbons, aromatic hydrocarbon, ethers, amine, ketone, esters；
Preferably, second solvent includes normal heptane, 1- octadecane, 1- heptadecane, 1- hexadecane, 1- octadecene, 1- ten At least one of seven carbenes, cetene, tetradecene, 1- dodecylene, isotriacontane, paraffin oil.
10. a kind of quantum dot characterized by comprising
The core of quantum dot, the core of the quantum dot are indium sulphur；And
The shell being coated on the core of the quantum dot, the shell are zinc sulphide；
Quantum dot preparation method as described in any one of claims 1 to 9 is made.
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