CN105542749A - Crust growing method of mixed crust origin precursor at low temperature and quantum dot - Google Patents
Crust growing method of mixed crust origin precursor at low temperature and quantum dot Download PDFInfo
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- CN105542749A CN105542749A CN201510994624.4A CN201510994624A CN105542749A CN 105542749 A CN105542749 A CN 105542749A CN 201510994624 A CN201510994624 A CN 201510994624A CN 105542749 A CN105542749 A CN 105542749A
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
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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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- C09K11/00—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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- 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
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/89—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing mercury
- C09K11/892—Chalcogenides
Abstract
The invention discloses a crust growing method of a mixed crust origin precursor at low temperature and a quantum dot. The method comprises the following steps of fully mixing a cation precursor and an anion precursor under the condition of inert gas, wherein the temperature of mixture liquor can make sure no reaction between the cation precursor and the anion precursor occurs and no precipitation; during the mixing process or after mixing, dropwise adding the mixture liquor into a core of the quantum dot for crust growing. According to the crust growing method adopted by the invention, the anion precursor and the cation precursor are mixed under the condition of low temperature without reaction, and the thickness of crust growing is further controlled through controlling different mixing proportions and dropwise adding speeds, so that the method is simple to operate, easy to control and high in repeatability.
Description
Technical field
The present invention relates to quantum dot synthesis field, particularly relate to a kind of method that encrusts and the quantum dot that mix shell source precursor at low temperatures.
Background technology
The technology that encrusts has investigation and application widely in quantum dot synthesis field, especially obtains in luminescent quantum dot field and studies widely.Since CdSe luminescent quantum dot is come out, promote the research boom of luminescent quantum dot, equally also the fields such as photodiode, following novel display, biomarker have been provided to the basis of large-scale application.
Based on the research of the size of CdSe quantum dots, fluorescence intensity (PL), emission wavelength and peak width at half height (FWHM), people have done a large amount of work improving fluorescence intensity and the peak width at half height of quantum dot, the quantum yield of quantum dot decides the luminous intensity of quantum dot, fluorescence intensity luminescent quantum dot that is high and half-peak width is the target that researchist pursues always, the luminescent quantum dot of high fluorescent and half-peak width has the advantage of the good aspect of colour purity, therefore has broad application prospects in the display field in future.
The important method improving quantum dot fluorescence intensity is exactly luminous with the defect state reducing quantum dot surface at the semiconductor material of outer layer growing one deck broad-band gap of quantum dot, also has the different methods that encrusts: epitaxy, cationic exchange and continuous ionic layer deposition (SILAR) etc. for the different quantum dots technology that encrusts.Wherein continuous ionic layer deposition techniques to be applied as CdSe/ZnS, Zn in a lot of quantum dot system encrusts
xcd
1-Xs/ZnS, Zn
xcd
1-Xse/ZnS etc. are not limited thereto.To run into some lattice mismatch rate comparatively highs as different band gap material utilizing continuous ionic layer deposition techniques to encrust, also have the speed speed of shell deposition wayward to the problem such as encrusting, the source of these reasons, except the reactive behavior difference of the raw material that encrusts, is exactly add shell source mode unreasonable.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of method that encrusts and the quantum dot that mix shell source precursor at low temperatures, be intended to solve that the existing method that encrusts is unreasonable causes the problems such as lattice mismatch rate is higher, shell sedimentation rate is wayward.
Technical scheme of the present invention is as follows:
Mix the method that encrusts of shell source precursor at low temperatures, wherein, comprise step:
Fully mixed under inert gas conditions with negatively charged ion precursor by positively charged ion precursor, the temperature of mixed solution can make the two not react and not separate out;
In mixing process or when having mixed, mixed solution is dripped in quantum dot core, for encrusting.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, the temperature of described mixed solution is 80 ~ 100 DEG C.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, in dropping process, utilizes and springs up speed and the time that pump controls dropping.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, mixes positively charged ion precursor with negatively charged ion precursor in the mode dripped, or once adds mixing in certain proportion.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, positively charged ion precursor is Cd (OA)
2, Zn (OA)
2or Pb (OA)
2in one or more.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, negatively charged ion precursor is one or more in S-ODE, S-TOP, S-OA, Se-TOP, S-OLA, S-TBP or Se-TBP.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, the diameter of quantum dot core is 1 ~ 10nm.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, quantum dot core is Binary-phase or ternary phase, and the quantum dot core of Binary-phase is one or more in CdS, CdSe, CdTe, PbS, PbSe or HgS; The quantum dot core of ternary phase is Zn
xcd
1-Xs, Zn
xcd
1-Xse, Zn
xcd
1-Xte or PbSe
xs
1-Xin one or more.
The described method that encrusts mixing shell source precursor at low temperatures, wherein, also comprises: the speed that the different optical characteristics showed by the different shell thicknesses detecting quantum dot core and then control are dripped and time.
A kind of quantum dot, wherein, adopts the method for encrusting as above described in any one to make.
Beneficial effect: the method that encrusts of the present invention, mixed anion precursor and positively charged ion precursor under the nonreactive condition of low temperature, by controlling different blending ratios and rate of addition controls the thickness that encrusts further, simple to operate, be easy to control, repeatability is high.
Accompanying drawing explanation
Fig. 1 is a kind of schema mixing the method that encrusts of shell source precursor at low temperatures of the present invention.
Fig. 2 is the schematic diagram of method of the present invention.
Embodiment
The invention provides a kind of method that encrusts and the quantum dot that mix shell source precursor at low temperatures, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, Fig. 1 is a kind of schema mixing the method that encrusts of shell source precursor at low temperatures of the present invention, and as shown in the figure, it comprises step:
S1, fully mixed under inert gas conditions with negatively charged ion precursor by positively charged ion precursor, the temperature of mixed solution can make the two not react and not separate out;
S2, in mixing process or when having mixed, by mixed solution drip in quantum dot core, for encrusting.
Because different positively charged ion shell sources and negatively charged ion shell source can be separated out at a certain temperature, so not easy to operate when adding, and the method that encrusts of the present invention, mix under adopting the temperature making the two not react and not separate out, the problem of not easy operation control when different shell source separately adds can be solved, and be easy to regulation and control, repeatability is high.
Mixed solution is being dripped in quantum dot nuclear process, can utilize and spring up speed and the time that pump controls dropping.Equally, the hybrid mode of positively charged ion precursor and negatively charged ion precursor can be also the mode dripped, or once adds mixing in certain proportion.
The temperature of described mixed solution is 80 ~ 100 DEG C, does not also separate out to make both positively charged ion precursor and negatively charged ion precursor not react.This temperature range is applicable to most precursor, but partial crustal is as Zn (OA)
2separating out lower than time corresponding temperature (80 DEG C), so need to determine mixeding liquid temperature according to the material of reality.
As shown in Figure 2, positively charged ion precursor can mix with arbitrary proportion under the nonreactive condition of low temperature with negatively charged ion precursor, the mixed solution be mixed to get can drip with arbitrary velocity, and (or with Rapid Thermal injection mode) forms quantum dot shell in quantum dot core, can be controlled the speed encrusted by the speed and time controlling dropping.
Described positively charged ion precursor is organo-metallic precursor, as: Cd (OA)
2, Zn (OA)
2or Pb (OA)
2in one or more, but to be not limited thereto.Described negatively charged ion precursor is sulfur family element and non-co-melt and dissolved dose of formation such as ODE or TOP, TBP, OA, OLA, as: one or more in S-ODE, S-TOP, S-OA, Se-TOP, S-OLA, S-TBP or Se-TBP, but be not limited thereto.
Quantum dot core for encrusting also is be obtained by reacting by above-mentioned positively charged ion precursor and negatively charged ion precursor under suitable temperature of reaction, and diameter range is about 1-10nm.Quantum dot core is Binary-phase or ternary phase, and the quantum dot core of Binary-phase is one or more in CdS, CdSe, CdTe, PbS, PbSe or HgS; The quantum dot core of ternary phase is Zn
xcd
1-Xs, Zn
xcd
1-Xse, Zn
xcd
1-Xte or PbSe
xs
1-Xin one or more.
Quantum dot shell is that above-mentioned positively charged ion precursor and negatively charged ion precursor are obtained by reacting, as: Zn (OA)
2, Cd (OA)
2obtain ZnS, CdS etc. after reacting with S-TOP, S-ODE, S-OA, Se-TOP, Se-ODE, but be not limited thereto.
Method of the present invention also comprises: the speed that the different optical characteristics showed by the different shell thicknesses detecting quantum dot core and then control are dripped and time.That is, dripping speed on quantum dot core and time for mixed solution, is go out to obtain shell thickness and determining according to its concrete manifestation.
To mix two kinds of concrete precursors, the above-mentioned method of encrusting is described in detail below.
Being prepared as follows of two kinds of precursors:
1), Zn (OA)
2the preparation of (positively charged ion precursor): the paraffin oil of the zinc acetate of 2mmol, the oleic acid of 3ml and 2ml adds in the there-necked flask of 50ml.First carry out the exhaust of 20min normal temperature, then 170 DEG C of exhaust 40min, then cool to 90 DEG C under an inert gas.
2), the preparation of S-ODE (negatively charged ion precursor): the S of 2.4mmol is joined 120 DEG C of heating in the TOP of 2ml and, until form the liquid of clear, be cooled to room temperature subsequently.
3), the S-ODE to room temperature is gone to join Zn (OA) by cold
2in (with certain speed drip mixing or once add mixing in certain proportion), the speed that mixing drips can utilize and springs up pump to control, and fully mixing and mixed solution will remain in 80-100 DEG C of temperature range not react and be also unlikely to zinc oleate S-ODE and Zn (OA) under an inert gas
2separate out.
4), in step 3) complete (or carrying out) while, utilize and spring up pump and slowly drip in the middle of mixed solution to the quantum dot core mixed solution of high temperature for encrusting with certain speed.
5), finally by detecting different optical characteristics that the different shell thicknesses of quantum dot show and then controlling the speed that drips and time.
Method of the present invention is simple to operate, being easy to repetition and the blending ratio of two kinds of precursors also can arbitrarily regulate and control when encrusting, also effectively avoiding some that produce when separately dripping and being unfavorable for that the drawback of repetition is as the speed of dropping and the bad ratio held impact and add two kinds of precursors in mixed solution of consumption; And two kinds of precursors can not react after the drop wise addition in participation instantaneously.
The present invention also provides a kind of quantum dot, and it adopts the method for encrusting as above to make.
In sum, the method that encrusts of the present invention, mixed anion precursor and positively charged ion precursor under the nonreactive condition of low temperature, by controlling different blending ratios and rate of addition controls the thickness that encrusts further, simple to operate, be easy to control, repeatability is high.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (10)
1. mix the method that encrusts of shell source precursor at low temperatures, it is characterized in that, comprise step:
Fully mixed under inert gas conditions with negatively charged ion precursor by positively charged ion precursor, the temperature of mixed solution can make the two not react and not separate out;
In mixing process or when having mixed, mixed solution is dripped in quantum dot core, for encrusting.
2. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, it is characterized in that, the temperature of described mixed solution is 80 ~ 100 DEG C.
3. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, is characterized in that, in dropping process, utilizes and springs up speed and the time that pump controls dropping.
4. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, is characterized in that, mixed by positively charged ion precursor, or once add mixing in certain proportion in the mode dripped with negatively charged ion precursor.
5. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, it is characterized in that, positively charged ion precursor is Cd (OA)
2, Zn (OA)
2or Pb (OA)
2in one or more.
6. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, it is characterized in that, negatively charged ion precursor is one or more in S-ODE, S-TOP, S-OA, Se-TOP, S-OLA, S-TBP or Se-TBP.
7. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, it is characterized in that, the diameter of quantum dot core is 1 ~ 10nm.
8. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, it is characterized in that, quantum dot core is Binary-phase or ternary phase, and the quantum dot core of Binary-phase is one or more in CdS, CdSe, CdTe, PbS, PbSe or HgS; The quantum dot core of ternary phase is Zn
xcd
1-Xs, Zn
xcd
1-Xse, Zn
xcd
1-Xte or PbSe
xs
1-Xin one or more.
9. the method that encrusts mixing shell source precursor at low temperatures according to claim 1, is characterized in that, also comprise: the speed that the different optical characteristics showed by the different shell thicknesses detecting quantum dot core and then control are dripped and time.
10. a quantum dot, is characterized in that, adopts the method for encrusting as described in any one of claim 1 ~ 9 to make.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111117622A (en) * | 2020-01-07 | 2020-05-08 | 上海交通大学 | A kind of Mn: ZnSe/ZnSeS quantum dot and preparation method thereof |
| WO2020134141A1 (en) * | 2018-12-29 | 2020-07-02 | Tcl科技集团股份有限公司 | Method for preparing quantum dot |
| TWI733153B (en) * | 2019-07-31 | 2021-07-11 | 國立虎尾科技大學 | Manufacturing method of quantum dot and white light element |
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| WO2020134141A1 (en) * | 2018-12-29 | 2020-07-02 | Tcl科技集团股份有限公司 | Method for preparing quantum dot |
| TWI733153B (en) * | 2019-07-31 | 2021-07-11 | 國立虎尾科技大學 | Manufacturing method of quantum dot and white light element |
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| CN111117622B (en) * | 2020-01-07 | 2022-03-01 | 上海交通大学 | A kind of Mn: ZnSe/ZnSeS quantum dot and preparation method thereof |
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Application publication date: 20160504 |