CN106566529A - Passivated quantum dot and preparation method thereof - Google Patents
Passivated quantum dot and preparation method thereof Download PDFInfo
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- CN106566529A CN106566529A CN201610988388.XA CN201610988388A CN106566529A CN 106566529 A CN106566529 A CN 106566529A CN 201610988388 A CN201610988388 A CN 201610988388A CN 106566529 A CN106566529 A CN 106566529A
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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Abstract
The invention provides a passivated quantum dot. The passivated quantum dot comprises a quantum dot body and a passivation layer covering the surface of the quantum dot body, wherein the passivation layer is an inorganic compound membrane layer formed by carrying out chemical reaction on halide ions and positive ions on the surface of the quantum dot body. A preparation method of the passivated quantum dot includes the steps of providing a positive ion precursor and a negative ion precursor and preparing the quantum dot body; preparing halogen gas, dissolving the halogen gas into an organic solvent protected by vacuum or inert gas and preparing a halogen stock solution; and dissolving the quantum dot body to form a quantum dot body solution, adding the halogen stock solution into the quantum dot body solution to form a reaction system, stirring the mixed solutions for generating reaction, and purifying the mixed solutions to obtain the passivated quantum dot.
Description
Technical field
The invention belongs to quantum dot synthesis technical field, more particularly to a kind of passivation quantum dot and preparation method thereof.
Background technology
Quantum dot leads scientific and technological trend as most potential nano material.Either synthetic method or its is corresponding
Application on, the development of quantum dot synthetic technology be unable to do without all the time a purpose, i.e., improve the excellent of quantum dot to greatest extent
Performance, such as：Fluorescence intensity, half-peak breadth, stability of quantum dot etc..
The stability of quantum dot is one of important parameter of evaluation quantum dot system, and the stability difference of quantum dot can serious shadow
Ring the range of application of quantum dot.Therefore, technical staff is lifted in the optimizing stability of quantum dot and has done many research work,
Such as prepare the quantum dot of nucleocapsid structure；The surface defect of quantum dot is passivated using the coating material of correspondence zwitterion；
Improve the stability of quantum dot using means such as silicon dioxide-coated quantum dots.But these passivation means all can not be longer
Improve the fluorescence intensity and stability of quantum dot.Particularly when quantum dot be used for extreme condition special dimension when (quantum dot
Heat stability, light stability, electrical stability require all very high), the quantum dot that these conventional passivating methods are obtained is remote not
Can meet and require.Additionally, quantum dot prepared by conventional passivation means, or remaining luminous, affects the performance of quantum dot (as adopted
Method of the coating material of correspondence zwitterion to be passivated quantum dot)；There is band gap, the performance of quantum dot kernel is had
Affect.
The content of the invention
It is an object of the invention to provide a kind of passivation quantum dot and preparation method thereof, it is intended to solve existing method preparation
Passivation quantum dot long-acting can not maintain the problem of the fluorescence intensity and stability of quantum dot, especially can not meet for extreme condition
Quantum dot performance requirement problem.
The present invention is achieved in that a kind of passivation quantum dot, including quantum dot and is wrapped in the quantum dot surface
Passivation layer, and the passivation layer is the inorganic chemical that halide ion is formed with the cation Jing chemical reaction of the quantum dot surface
Thing thin layer.
And, a kind of preparation method of passivation quantum dot is comprised the following steps：
Cation presoma, anion presoma are provided, quantum dot is prepared；
Halogen gas is prepared, the halogen gas is dissolved in the organic solvent of vacuum or inert gas shielding, prepared
Halogen storing solution；
The quantum dot is dissolved to form quantum dot solution, the halogen storing solution shape is added in the quantum dot solution
Into reaction system, stirring reaction, obtain being passivated quantum dot after purification process.
The preparation method of the passivation quantum dot that the present invention is provided, using halogenic molecule the anion of quantum dot surface is exchanged,
The inorganic compound shell containing halogen is formed, method is simple, and the passivation quantum dot for obtaining not only can be improved long-term effectively
The stability of quantum dot, non-oxidizability, while can long-term effectively improve the optical property of quantum dot and reduce optical charge turning
Move.Additionally, the preparation method for being passivated quantum dot that the present invention is provided, can be passivated to quantum dot solution, can extensively answer
It is prepared by the quantum dot for other systems.
The passivation quantum dot that the present invention is provided, with preferably light stability, heat stability, electrical stability, antioxidation
Property and optical property, and effect remains permanent, can be applied to the use demand of special dimension extreme condition.
Description of the drawings
Fig. 1 is the preparation method schematic flow sheet of passivation quantum dot provided in an embodiment of the present invention；
Fig. 2 is the design sketch of the preparation passivation quantum dot that the embodiment of the present invention provides 1.
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only to explain
The present invention, is not intended to limit the present invention.
Embodiments provide a kind of passivation quantum dot, including quantum dot and be wrapped in the blunt of the quantum dot surface
Change layer, and the passivation layer is the inorganic compound that halide ion is formed with the cation Jing chemical reaction of the quantum dot surface
Thin layer.
Specifically, the quantum dot can be conventional quantum dot, including Binary-phase quantum dot, ternary phase quantum dot, quaternary
Phase quantum dot.Wherein, the Binary-phase quantum dot includes but is not limited to CdS, CdSe, CdTe, InP, AgS, PbS, PbSe, HgS；
The ternary phase quantum dot includes but is not limited to ZnXCd1-XS、CuXIn1-XS、ZnXCd1-XSe、ZnXSe1-XS、ZnXCd1-XTe、
PbSeXS1-X；The quaternary phase quantum dot includes but is not limited to ZnXCd1-XS/ZnSe、CuXIn1-XS/ZnS、ZnXCd1-XSe/ZnS、
CuInSeS、ZnXCd1-XTe/ZnS、PbSeXS1-X/ZnS。
In the embodiment of the present invention, in quantum dot surface one layer of passivation layer, and the passivation layer halide ion and institute are enclosed with
State the inorganic compound thin film layer that the cation Jing chemical reaction of quantum dot surface is formed.Specifically, the halide ion is fluorine
At least one in ion, chloride ion, bromide ion, iodide ion.
Passivation quantum dot provided in an embodiment of the present invention, with preferably light stability, heat stability, electrical stability,
Non-oxidizability and optical property, and effect remains permanent, can be applied to the use demand of special dimension extreme condition.
Quantum dot is passivated described in the embodiment of the present invention can be prepared by following methods.
And, with reference to Fig. 1, the embodiment of the present invention additionally provides a kind of preparation method of passivation quantum dot, including following step
Suddenly：
S01., cation presoma, anion presoma are provided, quantum dot is prepared；
S02. halogen gas is prepared, the halogen gas is dissolved in the organic solvent of vacuum or inert gas shielding,
Prepare halogen storing solution；
S03. the quantum dot is dissolved to form quantum dot solution, the halogen deposit is added in the quantum dot solution
Liquid forms reaction system, and stirring reaction obtains being passivated quantum dot after purification process.
Specifically, in above-mentioned steps S01, the cation presoma, the anion presoma are not clearly limited, this
Field conventional cation presoma, anion presoma are all in the embodiment of the present invention range of choice.Specifically, it is described sun from
Sub- presoma includes but is not limited to zinc oleate, cadmium oleate, plumbi oleas, Oleic acid indium.The anion presoma is included but is not limited to
S-ODE、S-TOP、S-OA、Se-TOP、S-OLA、 S-TBP、Se-TBP、Te-ODE、Te-OA、Te-TOP、Te-TBP、(TMS)2S。
Thus cation presoma described in the embodiment of the present invention can be prepared not in any combination with the anion presoma
The Binary-phase quantum dot of same type.The quantum dot can be conventional quantum dot, including Binary-phase quantum dot, ternary phase quantum
Point, quaternary phase quantum dot.Wherein, the Binary-phase quantum dot include but is not limited to CdS, CdSe, CdTe, InP, AgS, PbS,
PbSe、HgS；The ternary phase quantum dot includes but is not limited to ZnXCd1-XS、CuXIn1-XS、ZnXCd1-XSe、ZnXSe1-XS、
ZnXCd1-XTe、PbSeXS1-X；The quaternary phase quantum dot includes but is not limited to ZnXCd1-XS/ZnSe、CuXIn1-XS/ZnS、
ZnXCd1-XSe/ZnS、CuInSeS、ZnXCd1-XTe/ZnS、PbSeXS1-X/ZnS。
Quantum dot described in the embodiment of the present invention can be prepared using this area conventional method.Below with red CdSe amounts
As a example by son point, its preparation method is illustrated.It should be appreciated that the preparation method of red CdSe quantum dots herein, as just a reality
Example, not with the species and preparation method for limiting quantum dot of the present invention.
Used as a specific embodiment, red CdSe quantum dots preparation method is comprised the following steps：
S011. cadmium oleate { Cd (OA)2Presoma preparation：Aska-Rid. (CdO) 2mmol, oil are added in there-necked flask
Acid (OA) 3ml, octadecylene (ODE) 10ml elder generation room temperature evacuation 30mins, is then being heated to 180 DEG C of row argon 60mins, so
180 DEG C of evacuation 30mins are maintained afterwards, are cooled to room temperature standby.
S012. the preparation of selenium (Se) presoma：The Se for claiming 4mmol is added in trioctylphosphine oxygen phosphorus (TOP) of 4ml, is heated
To 170 DEG C of maintenance 30min, 140 DEG C are then cooled to.
S013. the preparation of red CdSe quantum dots：By the cadmium oleate { Cd (OA) in step S0112Presoma is heated to
280 DEG C, the fast speed heat of selenium (Se) presoma for then extracting 2ml is injected into cadmium oleate { Cd (OA)2The interior reaction 2min of precursor, profit
With psychrolusia mixed liquor is cooled down rapidly, using methanol, toluene the CdSe that dried obtains redness is centrifuged
Quantum dot.
In above-mentioned steps S02, there is provided halogen gas, the halogen gas can form halide ion in subsequent step, with
The anion exchange cationoid reaction of the quantum dot surface (halide ion with) of the quantum dot surface, forms and covers
In the inorganic passivation shell of the quantum dot surface.Specifically, the halogen gas be fluorine gas, chlorine, bromine gas, iodine gas in extremely
Few one kind, corresponding, the halide ion is at least one in fluorion, chloride ion, bromide ion, iodide ion.The halogen
The reactivity of ion is strong, once but combined with the cation in embodiment of the present invention quantum dot, the compound stability of formation
It is very strong, external environment impact is not easily susceptible to, being capable of long sustaining its performance.And the passivation layer being consequently formed, it is not involved in lighting,
Improve the luminescent properties of quantum dot；And without band gap, do not affect kernel quantum dot.
In the embodiment of the present invention, the preparation of the halogen gas can be realized using conventional method.It is with chlorine below
Example, illustrates its preparation method.
As a specific embodiment, the chlorine (Cl2) preparation method be：Take the dilute hydrochloric acid (HCl) of 20ml with
The weight percentage of 50ml is placed in the there-necked flask of 100ml for the liquor natrii hypochloritises of 6wt%, and room temperature is mixed,
The gas that bubbling is produced in flask is the chlorine containing moisture.
Further, moisture is contained in the halogen gas based on preparation, and the fluorescent emission of quantum dot is sensitive to water oxygen, if
It is aqueous in reaction system, the fluorescent effect of quantum dot can be affected.It is therefore preferable that being dried process to the halogen gas.Tool
Body is preferred, the halogen gas is passed through in desiccant such as anhydrous calcium chloride and is dried.Herein, the selection of desiccant does not have
Clearly limit, conventional desiccant is used equally to the embodiment of the present invention.
Under conditions of vacuum or inert gas shielding, the halogen gas is dissolved in organic solvent, prepare halogen
Storing solution.The vacuum or inert gas shielding, can avoid halogenic molecule that other miscellaneous side reactions occur, miscellaneous so as to introduce other
Matter, disturbs the embodiment of the present invention to be passivated the preparation of quantum dot.Specifically, the noble gases include but is not limited to argon.Wherein,
Used as dispersant or disperse medium, for dissolving halogen gas and quantum dot, its selection is not clearly limited the organic solvent,
It will be appreciated, however, that the organic solvent can not produce reaction with the halogen gas and/or quantum dot.Preferably, it is described
Organic solvent may be selected the carbon tetrachloride of asepsis environment-protecting, certainly, not limited to this.
Preferably, the concentration of halogen gas molecule is 0.1-0.2mol/L in the halogen storing solution.The halogen gas
The concentration of molecule is too low, then reaction efficiency is relatively slow or is difficult to reaction fully.
In above-mentioned steps S03, the quantum dot is dissolved to form quantum dot solution, it is preferred that the quantum dot solution
Concentration is 10-40mg/mL.The concentration of suitable quantum dot solution is conducive to fully exchanging for surface anion and halogen.
Further, the halogen storing solution is added to form reaction system in the quantum dot solution, halogen forms halogen
Plain ion, the anion exchange with quantum dot surface, prepares passivation layer.Wherein, in the reaction system, halogen gas and quantum
The content of point is than meeting (0.1-0.2) mol：(10-40)mg.In the proportion, the moon that quantum dot shows both had been can ensure that
Ion is fully exchanged with halide ion, and waste is not resulted in again, can be with cost-effective.Further, the embodiment of the present invention is stirred
The response time is mixed for 20-180min.
The embodiment of the present invention carries out purification process by the quantum dot after passivation layer is prepared.The method of the purification process can be with
For：Add methanol, acetone in mixed liquor after the reaction to be centrifuged, surface is obtained after dried shape is passivated by halogen
Into the quantum dot of inorganic compound shell.Certainly, the method not limited to this of purification process.
Specifically, by taking red quantum point CdSe, halogen gas chlorine as an example, it forms the design sketch of passivation quantum dot as schemed
Described in 2.
The preparation method of passivation quantum dot provided in an embodiment of the present invention, using halogenic molecule the moon of quantum dot surface is exchanged
Ion, forms the inorganic compound shell containing halogen, and method is simple, and the passivation quantum dot for obtaining not only can be long-term effectively
Stability, the non-oxidizability of quantum dot are improved, while can long-term effectively improve the optical property of quantum dot and reduce photoelectricity
Lotus shifts.Additionally, the preparation method of passivation quantum dot provided in an embodiment of the present invention, not only can be carried out blunt to quantum dot solution
Change, it is also possible to which quantum dot solid film is passivated, prepared by the quantum dot that can be widely applied for other systems.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of passivation quantum dot, it is characterised in that including quantum dot and the passivation layer for being wrapped in the quantum dot surface, and institute
State the inorganic compound thin film layer that passivation layer is that halide ion is formed with the cation Jing chemical reaction of the quantum dot surface.
2. passivation quantum dot as claimed in claim 1, it is characterised in that the halide ion be fluorion, chloride ion, bromine from
At least one in son, iodide ion.
3. passivation quantum dot as claimed in claim 1 or 2, it is characterised in that the quantum dot include Binary-phase quantum dot, three
First phase quantum dot, quaternary phase quantum dot.
4. passivation quantum dot as claimed in claim 3, it is characterised in that the Binary-phase quantum dot include CdS, CdSe,
CdTe、InP、AgS、PbS、PbSe、HgS；The ternary phase quantum dot includes ZnXCd1-XS、CuXIn1-XS、ZnXCd1-XSe、
ZnXSe1-XS、ZnXCd1-XTe、PbSeXS1-X；The quaternary phase quantum dot includes ZnXCd1-XS/ZnSe、CuXIn1-XS/ZnS、
ZnXCd1-XSe/ZnS、CuInSeS、ZnXCd1-XTe/ZnS、PbSeXS1-X/ZnS。
5. a kind of preparation method that quantum dot is passivated as described in claim 1-4 is arbitrary, comprises the following steps：
Cation presoma, anion presoma are provided, quantum dot is prepared；
Halogen gas is prepared, the halogen gas is dissolved in the organic solvent of vacuum or inert gas shielding, prepare halogen
Storing solution；
The quantum dot is dissolved to form quantum dot solution, adds the halogen storing solution to be formed instead in the quantum dot solution
System, stirring reaction is answered to obtain being passivated quantum dot after purification process.
6. the preparation method of quantum dot is passivated as claimed in claim 5, it is characterised in that in the reaction system, halogen gas
Body is (0.1-0.2) mol with the content ratio of quantum dot：(10-40)mg.
7. the preparation method of quantum dot is passivated as claimed in claim 5, it is characterised in that halogen gas in the halogen storing solution
The concentration of body molecule is 0.1-0.2mol/L.
8. the preparation method of passivation quantum dot as claimed in claim 5, it is characterised in that the concentration of the quantum dot solution is
10-40mg/mL。
9. as described in claim 5-7 is arbitrary passivation quantum dot preparation method, it is characterised in that the halogen gas be fluorine
At least one in gas, chlorine, bromine gas, iodine gas.
10. as described in claim 5-7 is arbitrary passivation quantum dot preparation method, it is characterised in that the cation forerunner
Body includes zinc oleate, cadmium oleate, plumbi oleas, Oleic acid indium；And/or
The anion presoma includes S-ODE, S-TOP, S-OA, Se-TOP, S-OLA, S-TBP, Se-TBP, Te-ODE, Te-
OA、Te-TOP、Te-TBP、(TMS)2S。
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| WO2019001026A1 (en) * | 2017-06-28 | 2019-01-03 | Tcl集团股份有限公司 | Preparation method for metal oxide nanoparticle film and electrical component |
| CN109233801A (en) * | 2017-07-11 | 2019-01-18 | Tcl集团股份有限公司 | Quantum dot of surface modification and preparation method thereof, using with QLED device |
| CN109988556A (en) * | 2017-12-29 | 2019-07-09 | Tcl集团股份有限公司 | Quantum dot solid film and its preparation method and application |
| CN110400886A (en) * | 2018-04-24 | 2019-11-01 | 三星电子株式会社 | Luminescent film, its manufacturing method and luminescent device and display device containing the luminescent film |
| CN110616072A (en) * | 2018-06-20 | 2019-12-27 | 深圳Tcl工业研究院有限公司 | Post-processing method of InP quantum dots |
| CN111003725A (en) * | 2019-12-20 | 2020-04-14 | 上海比英半导体科技有限公司 | Low-temperature preparation method of monodisperse lead sulfide nanocluster |
| WO2020191821A1 (en) * | 2019-03-27 | 2020-10-01 | 天津市中环量子科技有限公司 | Quantum dot material processing method, highly stable quantum dot material and application thereof |
| US11242483B2 (en) * | 2018-09-30 | 2022-02-08 | Tcl Technology Group Corporation | Quantum dot |
| CN117126669A (en) * | 2022-05-18 | 2023-11-28 | 苏州星烁纳米科技有限公司 | ZnSe (Te) quantum dot, preparation method thereof and electroluminescent device |
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| WO2019001026A1 (en) * | 2017-06-28 | 2019-01-03 | Tcl集团股份有限公司 | Preparation method for metal oxide nanoparticle film and electrical component |
| US11851343B2 (en) | 2017-06-28 | 2023-12-26 | Tcl Technology Group Corporation | Preparation method for metal oxide nanoparticle film and electrical component |
| CN109233801A (en) * | 2017-07-11 | 2019-01-18 | Tcl集团股份有限公司 | Quantum dot of surface modification and preparation method thereof, using with QLED device |
| CN109988556A (en) * | 2017-12-29 | 2019-07-09 | Tcl集团股份有限公司 | Quantum dot solid film and its preparation method and application |
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| CN111003725A (en) * | 2019-12-20 | 2020-04-14 | 上海比英半导体科技有限公司 | Low-temperature preparation method of monodisperse lead sulfide nanocluster |
| CN117126669A (en) * | 2022-05-18 | 2023-11-28 | 苏州星烁纳米科技有限公司 | ZnSe (Te) quantum dot, preparation method thereof and electroluminescent device |
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