CN106398686A - Quantum dot and preparation method thereof - Google Patents
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- CN106398686A CN106398686A CN201610801814.4A CN201610801814A CN106398686A CN 106398686 A CN106398686 A CN 106398686A CN 201610801814 A CN201610801814 A CN 201610801814A CN 106398686 A CN106398686 A CN 106398686A
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
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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
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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
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/661—Chalcogenides
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
Abstract
The invention discloses a quantum dot and a preparation method thereof. The preparation method comprises the following steps of firstly, preparing a solid fibrous film; then, putting the prepared solid fibrous film into a cation precursor solution to crosslink; injecting an anion precursor into the crosslinked solid fibrous film to react, so as to obtain the quantum dot, wherein the size of the solid fibrous film is nanometer or micrometer level. The quantum dot has the advantages that by using the solid nanometer fiber as a micro-reactor, the reaction temperature is lower, and the quantum dot can quickly nucleate and grow at a solid-liquid interface; the size of the quantum dot can be adjusted by controlling the size of the solid fibrous film or the reaction temperature; the solid nanometer fibrous film which is used as the micro-reactor can be repeatedly used, so that the cost is greatly reduced. The preparation method has the advantages that the operation is simple, the repeating is easy, and the preparation method can be used for preparation.
Description
Technical field
The present invention relates to quantum dot synthesis field, more particularly, to a kind of quantum dot and preparation method thereof.
Background technology
In recent years, because Colloidal Quantum Dots have huge answering in bio-sensing, biomarker and LED aspect
With property, researchers extensively study the optical property of quantum dot.Due to the requirement to luminescent quantum dot structure and aspect of performance,
Their controlledly synthesis is become with a noticeable research field.
In terms of luminescent quantum dot synthesis, researchers develop multiple preparation methods, such as metal-organosilane precursor method, molten
The hot method of agent, aqueous phase synthesis method, ion beam synthesis method, ultrasonic irradiation, hot injection method, chemical bath deposition, microwave radiation technology
Chemical bath deposition and solvent growth method etc..Wherein most widely employed approach of preparing is hot injection method, and this method is
The anion presoma of Se, S, Te etc. is injected in the cation presoma of Cd, Zn, Pb etc. at high temperature, fast-growth nucleation,
Crystal growth is made to form quantum dot more at a certain temperature.But, quantum dot requirement is prepared in uniform body using said method
React in system, and at higher temperatures(Typically more than 280 DEG C)Could react.In recent years, liquid-liquid two phase process has gradually developed
To be used for quantum dot synthesis, mainly to carry out forming core and crystal growth in water-oil phase interface.It is with traditional hot injection method
Compare, can be at a lower temperature(Usually less than 200 DEG C)Reacted, synthesis obtains the quantum dot of size uniform.But liquid-liquid
Two phase process yet suffers from certain defect, and the cation presoma that this method needs is generally chain alkyl acid metal salt class,
Oil phase leads to product and adopts toluene, is toxic solvent, and during the course of the reaction in order that the quantum dot generating enters at two-phase interface
Enter in oil phase in addition it is also necessary to add long chain hydrocarbon(C6-C18)As coating agent.Although in addition, this method makes reaction exist
Carry out under lower temperature, but need high pressure as subsidiary conditions.
Therefore, prior art has yet to be improved and developed.
Content of the invention
In view of above-mentioned the deficiencies in the prior art, the present invention provides a kind of quantum dot and preparation method thereof it is intended to solution is existing
The problem of liquid-liquid two phase process Shortcomings in technology.
Technical scheme is as follows:
A kind of preparation method of quantum dot, wherein, including step:Prepare solid fabric film first, then by the solid-state preparing
Tunica fibrosa is put into and is carried out crosslinking in cation precursor solution, then by the solid fabric film after the injection crosslinking of anion presoma
In reacted, obtain quantum dot;Wherein, the size of described solid fabric film is nanoscale or micron order.
The preparation method of described quantum dot, wherein, described solid fabric film is sodium citrate tunica fibrosa, potassium citrate is fine
Dimension film, sodium alginate tunica fibrosa, potassium alginate tunica fibrosa, calcium alginate fibre film, silicon dioxide fibrous membrane, titania fiber
One of film.
The preparation method of described quantum dot, wherein, prepares solid fabric film by the method for electrostatic spinning.
The preparation method of described quantum dot, wherein, the temperature that anions and canons presoma reacts at solid-liquid interface is
120~160℃.
The preparation method of described quantum dot, wherein, described cation precursor solution is that cation presoma is dissolved in
It is formulated in solvent.
The preparation method of described quantum dot, wherein, described cation presoma is CdCl2、ZnCl2、Cd(NO3)2、Zn
(NO3)2、Pb(NO3)2、Cd(Ac)2、Zn(Ac)2、Pb(Ac)2One or more of.
The preparation method of described quantum dot, wherein, the solvent of described cation precursor solution is ethanol.
The preparation method of described quantum dot, wherein, described anion presoma is S-ODE, S-TOP, S-TOPO, S-
OA, one or more of S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP.
A kind of quantum dot, wherein, the preparation method using as above arbitrary described quantum dot is prepared from.
Described quantum dot, wherein, described quantum dot is CdS, CdSe, ZnSe, ZnS, PbSe, PbS, CdTe, Cd1- xZnxS、Cd1-xZnxSe、CdSeyS1-y、Cd1-xZnxSeyS1-y、PbSeXS1-X、ZnXCd1-XOne of Te, wherein 0≤x<1,0≤
y≤1.
Beneficial effect:The present invention, using solid fabric film as microreactor, prepares oil-soluble quantum at a lower temperature
Point.Solid fabric film adopts micrometer/nanometer level solid fabric film so that anions and canons presoma can be at solid-liquid interface
It is rapidly reached in short time and is thoroughly mixed, and quickly react, generate quantum dot.In addition, the solid-state as microreactor
Nano fibrous membrane can also be utilized repeatedly, is saved greatly cost.
Brief description
Fig. 1 is the schematic diagram of the quantum dot preparation method of the embodiment of the present invention.
Specific embodiment
The present invention provides a kind of quantum dot and preparation method thereof, for making the purpose of the present invention, technical scheme and effect more
Clear, clear and definite, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein only in order to
Explain the present invention, be not intended to limit the present invention.
A kind of preparation method preferred embodiment of quantum dot of the present invention, including step:Prepare solid fabric film first, so
Afterwards the solid fabric preparing film is put into and in cation precursor solution, carry out crosslinking, then anion presoma is injected and hand over
Reacted in solid fabric film after connection, obtained quantum dot;Wherein, the size of described solid fabric film is nanoscale or micron
Level.
The present invention is using nanoscale or micron-sized solid fabric film as microreactor so that anions and canons presoma
Can react rapidly at short notice at solid-liquid interface, prepare quantum dot.This is due to micron order or nanoscale
Solid fabric film, there is the features such as reaction compartment is little, specific surface area is big, surface-active is high, quantum can be made at solid-liquid interface
The rapid forming core of point simultaneously grows.And the raw material that adopted of this method are the more commonly used metallic salts it is not necessary to specific gold
Genus-organic compound, the temperature that anions and canons presoma reacts at solid-liquid interface can be 120 ~ 160 DEG C(As 130 DEG C or
140℃), that is, react and can carry out at a lower temperature, the size of quantum dot can pass through size or the reaction of solid fabric film
Temperature is being adjusted.In addition, the solid fabric film as microreactor can also be utilized repeatedly, it is saved greatly into
This.
Preferably, solid fabric film of the present invention can be sodium citrate tunica fibrosa, potassium citrate tunica fibrosa, alginic acid
In sodium tunica fibrosa, potassium alginate tunica fibrosa, calcium alginate fibre film, silicon dioxide fibrous membrane, titanic oxide fiber film etc. one
Kind.Above-mentioned solid fabric film can be employed as microreactor, and its size is nanoscale or micron order.It is highly preferred that it is described solid
State tunica fibrosa is sodium citrate tunica fibrosa or potassium citrate tunica fibrosa.
Preferably, the present invention can prepare solid fabric film by the method for electrostatic spinning.For example, sodium citrate tunica fibrosa can
Prepared by method of electrostatic spinning.
Cation precursor solution of the present invention is that cation presoma is dissolved in solvent(As ethanol)In be formulated
's.Preferably, described cation presoma can be CdCl2、ZnCl2、Cd(NO3)2、Zn(NO3)2、Pb(NO3)2、Cd(Ac)2、
Zn(Ac)2、Pb(Ac)2One or more of Deng.It is highly preferred that cation presoma is CdCl2Or ZnCl2.
Preferably, anion presoma of the present invention is S-ODE, S-TOP, S-TOPO, S-OA, S-OLA, S-TBP, S-
One or more of DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP etc..Wherein S-ODE, S-TOP, S-TOPO, S-OA,
S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP etc. refer to be dissolved in S or Se powder organic accordingly
In thing, that is, S is dissolved in ODE, and S is dissolved in TOP, and it is medium that Se is dissolved in ODE.
Based on said method, the present invention provides a kind of quantum dot, and it adopts the preparation side of as above arbitrary described quantum dot
Method is prepared from.Quantum dot of the present invention can be CdS, CdSe, ZnSe, ZnS, PbSe, PbS, CdTe, Cd1-xZnxS、
Cd1-xZnxSe、CdSeyS1-y、Cd1-xZnxSeyS1-y、PbSeXS1-X、ZnXCd1-XOne of Te etc., wherein 0≤x<1,0≤y≤
1.
Below by embodiment, the present invention is described in detail.
Embodiment 1
In conjunction with shown in Fig. 1, the preparation process of quantum dot is as follows:
(1)Sodium citrate tunica fibrosa is prepared by method of electrostatic spinning
The sodium citrate of 3g is dissolved in 10mL distilled water, the dimethyl second sulfone adding 3wt%, as cosolvent, adds 2.4g
Polystyrene, then at a temperature of 60 DEG C, stirring 3h obtains uniform solution.Solution is injected in the syringe of 10mL, injection
Using internal diameter, solution ejection end made by the stainless steel syringe needle for 0.4mm to device.Collector is made using the copper mesh of 4cm × 5cm, sprays syringe needle
Distance to copper mesh is 12cm, and middle using power, the uviol lamp for 100W is irradiated.The jet velocity of solution is 1.2mL/
H, high voltage power supply is 18kV.Continue to obtain certain thickness nano level sodium citrate tunica fibrosa after 4h after whole spinning process,
Sodium citrate tunica fibrosa is taken off from copper mesh and is placed in N2After insulation 6h at 80 DEG C in atmosphere furnace, it is cooled to room temperature standby.
(2)Cation presoma and the crosslinking of sodium citrate tunica fibrosa
Zn (the NO of configuration 2mmol/mL3)2Cd (NO with 0.2mmol/mL3)2Ethanol solution, above-mentioned electrostatic spinning is obtained
Sodium citrate tunica fibrosa put into and soak 2h in ethanol solution so as to full cross-linked.Soak and fully take out sodium citrate fiber afterwards
Film ethanol purge, removes unnecessary cation presoma.Then the sodium citrate tunica fibrosa after crosslinking is placed on 60 DEG C
Drying for standby in drying box.
(3)Anions and canons presoma reacts at solid-liquid interface, then generates quantum dot
Take 2mmol Se to be dissolved in 4mL TOP and the mixed solution of 10mL ODE, dissolving is stirred at room temperature and obtains uniform Se-
TOP-ODE anion presoma.By step(2)Sodium citrate tunica fibrosa after the crosslinking obtaining is placed in the oblique there-necked flask of 50mL
In, in N2It is heated to 140 DEG C under atmosphere.Then Se-TOP-ODE anion presoma is injected in oblique there-necked flask and carry out instead
Should, after reaction 20min, solution is poured out with ethyl acetate and ethanol precipitation, then cleans centrifugation with chloroform and acetone, obtain
Cd1-xZnxS quantum dot.
In sum, a kind of quantum dot and preparation method thereof that the present invention provides, the present invention using solid nanofibers as
Microreactor, reaction temperature is relatively low, quantum dot can at solid-liquid interface rapid forming core growing, the size of quantum dot can be led to
Cross the size controlling solid fabric film or reaction temperature to be adjusted.In addition, the solid nanofibers as microreactor
Film can also be utilized repeatedly, is saved greatly cost.Additionally, the method simple to operate it is easy to repeating and can be used for making
Standby oil-soluble quantum dot.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved according to the above description or to convert, all these modifications and variations all should belong to the guarantor of claims of the present invention
Shield scope.
Claims (10)
1. a kind of preparation method of quantum dot is it is characterised in that include step:Prepare solid fabric film first, then will prepare
Good solid fabric film is put into and is carried out crosslinking in cation precursor solution, then by consolidating after the injection crosslinking of anion presoma
Reacted in state tunica fibrosa, obtained quantum dot;Wherein, the size of described solid fabric film is nanoscale or micron order.
2. the preparation method of quantum dot according to claim 1 is it is characterised in that described solid fabric film is sodium citrate
Tunica fibrosa, potassium citrate tunica fibrosa, sodium alginate tunica fibrosa, potassium alginate tunica fibrosa, calcium alginate fibre film, silica are fine
One of dimension film, titanic oxide fiber film.
3. the preparation method of quantum dot according to claim 1 it is characterised in that prepared solid by the method for electrostatic spinning
State tunica fibrosa.
4. the preparation method of quantum dot according to claim 1 is it is characterised in that anions and canons presoma is in solid-liquid circle
At face, the temperature of reaction is 120 ~ 160 DEG C.
5. the preparation method of quantum dot according to claim 1 is it is characterised in that described cation precursor solution is sun
Ion presoma is dissolved in and is formulated in solvent.
6. the preparation method of quantum dot according to claim 5 is it is characterised in that described cation presoma is CdCl2、
ZnCl2、Cd(NO3)2、Zn(NO3)2、Pb(NO3)2、Cd(Ac)2、Zn(Ac)2、Pb(Ac)2One or more of.
7. quantum dot according to claim 5 preparation method it is characterised in that described cation precursor solution molten
Agent is ethanol.
8. quantum dot according to claim 1 preparation method it is characterised in that described anion presoma be S-ODE,
S-TOP, S-TOPO, S-OA, one of S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP or many
Kind.
9. a kind of quantum dot it is characterised in that using described quantum dot as arbitrary in claim 1 ~ 8 preparation method preparation and
Become.
10. quantum dot according to claim 9 it is characterised in that described quantum dot be CdS, CdSe, ZnSe, ZnS,
PbSe、PbS、CdTe、Cd1-xZnxS、Cd1-xZnxSe、CdSeyS1-y、Cd1-xZnxSeyS1-y、PbSeXS1-X、ZnXCd1-XIn Te
One kind, wherein 0≤x<1,0≤y≤1.
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CN115568241A (en) * | 2022-11-29 | 2023-01-03 | 广东聚华新型显示研究院 | Light-emitting device, preparation method thereof and display device |
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