CN106367068A - Quantum dot and high pressure preparation method thereof - Google Patents
Quantum dot and high pressure preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a quantum dot. The preparation method comprises a, mixing a cation precursor, a first ligand and a first organic solvent to obtain a cation-ligand solution, and b, mixing an anion precursor and the cation-ligand solution in an enclosed high pressure environment and in an inert gas atmosphere, and heating the mixed solution to the first temperature so that the cation-ligand and the anion precursor undergo a chemical reaction to produce the quantum dot. The high pressure preparation method can increase a selectable organic solvent scope, utilizes the organic solvent with a low boiling point and low recovery difficulty to realize quantum dot preparation and production, reduces a production cost and is environmentally friendly.
Description
Technical field
The present invention relates to a kind of preparation method of quantum dot and the quantum dot being obtained by this preparation method.
Background technology
Quantum dot, is also called semiconductor nanocrystal, is that particle diameter is usually 1-20 nanometer and has the material of crystal structure
Material.Quantum dot can send fluorescence under suitable light source or voltage excite, in display, biomarker, illumination and solar energy neck
Domain all has very big application potential.
At present, before the preparation method of quantum dot is mainly passed through to make cation precursor and anion in high temperature organic solvent
Body occurs chemical reaction to generate nanocrystal.The method the selection of organic solvent is required higher it is desirable to be able to before to reaction
Body has preferable solvability, has the boiling point higher than chemical reaction temperature, simultaneously the high temperature ring when chemical reaction occurs
Keep in border being stably not involved in reacting.From the point of view of being easy to the demand of preparation manipulation and industrialization production, organic solvent also needs to
Have following property: environment friendly, stable in the air in order to deposit, hypotoxicity, low melting point is (less than 25 DEG C, preferably lower than
20 DEG C) to be processed at room temperature.Additionally, the process problem of a large amount of organic solvents also can be faced in industrialization production.
In order to reach above-mentioned requirements, the organic solvent range of choice that current high temperature organic faciess are prepared used in quantum dot is extremely limited,
And typically there is longer carbochain, larger molecular weight, boiling point higher it is difficult to reclaim.These problems are in industrialization production
More amplify, become a difficult problem hindering quantum dot to prepare industrialization.
Content of the invention
The organic solvent range of choice present in incorporating quantum point industrialization preparation process of the present invention is little it is difficult to that reclaims asks
Topic is it is proposed that a kind of new quantum dot preparation method is it is intended to the cost of reduction quantum dot industrialization production and environmental pollution are asked
Topic.
The present invention proposes a kind of preparation method of quantum dot, comprises the following steps: a) by cation precursor, first join
Body, the first organic solvent are mixed to form cationic ligand solution；B) under airtight environment under high pressure and atmosphere of inert gases
In, anionic pre-cursors are mixed with described cationic ligand solution, and is heated to the first temperature and cause described cationic ligand
There is chemical reaction with described anionic pre-cursors, generate quantum dot.
Preferably, described high pressure range is 0.2mpa 5mpa.
Preferably, described cation precursor includes the compound of i-th race's metallic element, the chemical combination of the i-th i race metallic element
Thing, the compound of the i-th ii race metallic element, the compound of the i-th v race metallic element or transition metal element compound.
Preferably, described cation precursor include at least one in following metallic element: cd, zn, hg, cu, ag, ni,
co、fe、mn、ti、zr、in、pb.
Preferably, described cation precursor includes at least one in following compound: metal-oxide, metal carbonate
Salt, metal halide, metal alkoxide, metal mercaptide salt, metal acid imide, metal alkyl, metal aryl salt, metal complex,
Metal solvent compound.
Preferably, described cation precursor includes at least one in following compound: zinc chloride, zinc acetate, stearic acid
Zinc, zinc carbonate, zinc oxide, Aska-Rid., cadmium acetate, cadmium stearate, cadmium carbonate, Caddy (Cleary), Indium sesquioxide., indium acetate, carbonic acid indium, chlorine
Change indium.
Preferably, described first part include one of fatty acid, alkylamine, alkylphosphines, alkyl phosphine oxide, phosphonic acids or
Person is multiple.
Preferably, described fatty acid includes capric acid, Oleic acid, lauric acid/dodecanoic acid, tetradecylic acid, hexadecylic acid or stearic acid.
Preferably, the fusing point of described first organic solvent is less than 25 DEG C, and boiling point is higher than 150 DEG C.
Preferably, described first organic solvent includes at least one in following compound: 1 heptane, 1 octane, 1 nonyl
Alkane, 1 decane, 1 hendecane, 1 dodecane, 1 tridecane, 1 tetradecane, 1 heptene, 1 octene, 1 nonene, 1 decene, 1
Hendecene, 1 laurylene, 1 tridecylene, 1 tetradecene, 1 hexylamine, 1 heptyl amice, 1 octylame, 1 nonyl amine, 1 decyl amine, 10 one
Amine, 1 lauryl amine, 1 cetylamine, 1,12 diamino dodecane, 1,18 diaminourea octadecanes, 1,16 diaminourea hexadecanes, 1,
The 14 diaminourea tetradecanes, 1 enanthol, 1 capryl alcohol, 1 nonyl alcohol, 1 decanol, 1 hexadecanol, 1 lauryl alcohol, 1 tridecanol, 10 four
Alcohol, acetic acid dodecyl ester, 1 valeric acid, 1 caproic acid, 1 enanthic acid, 1 octanoic acid, 1 n-nonanoic acid, 1 capric acid, undecanoic acid, lauric acid/dodecanoic acid, ten
Three acid, tetradecylic acid, 1 decyl mercaptan, 1 undecyl mercaptan, 1 lauryl mercaptan, 1 tetradecanylthioalcohol.
Preferably, described anionic pre-cursors are selected from simple substance, covalent compound or ionic compound.
Preferably, described anionic pre-cursors include at least one following element: element sulphur, selenium element, P elements, tellurium unit
Element.
Preferably, before mixing with described cationic ligand solution, described anionic pre-cursors and Ligands, second
Organic solvent is mixed to form anionic pre-cursors solution, described anionic pre-cursors in the way of described anionic pre-cursors solution with described
Cationic ligand solution mixes.
Preferably, described first temperature range is 150 350 DEG C.
Preferably, described first temperature range is 200 350 DEG C.
Preferably, described quantum dot be selected from one of compound: cdse, cds, cdte, znse, zns, inp,
inas、cdznse、cdzns、cdznte、inznp、inznas.
Preferably, described preparation method also includes step c) reactant in step b) is further heated to second temperature
And keep a period of time.
Preferably, described second temperature scope is 250 350 DEG C.
The invention allows for a kind of quantum dot, it is obtained by preparation method as above.
Preferably, the half-peak breadth of described quantum dot is less than 30nm, and quantum efficiency is higher than 80%.
Compared with prior art, the method have the advantages that by the preparation method of the present invention, selectable have
Machine solvent scope increases, and can realize preparation and the life of quantum dot using the organic solvent that the relatively low recovery of boiling point is more prone to
Produce.The preparation method of the present invention reduces production cost, to more environment-friendly.The quantum dot that the preparation method of the present invention obtains
Can be widely applied in the fields such as display.
Brief description
Fig. 1 is the Absorption and emission spectra figure of the quantum dot of embodiment 2 in the present invention；
Fig. 2 is the Absorption and emission spectra figure of the quantum dot of embodiment 5 in the present invention；
Fig. 3 is the Absorption and emission spectra figure of the quantum dot of embodiment 6 in the present invention.
Specific embodiment
Below in conjunction with embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail, shows
So, described embodiment is only a part of embodiment of the present invention, rather than whole embodiment.Based in the present invention
Embodiment, the every other enforcement that those of ordinary skill in the art are obtained on the premise of not making creative work
Mode, broadly falls into the scope of the present invention.
The present invention proposes a kind of preparation method of quantum dot, comprises the following steps: a) by cation precursor, first join
Body, the first organic solvent are mixed to form cationic ligand solution；B) under airtight environment under high pressure and atmosphere of inert gases
In, anionic pre-cursors are mixed with cationic ligand solution, and is heated to the first temperature and cause cationic ligand and anion
There is chemical reaction in precursor, generate quantum dot.
With respect to traditional quantum dot high temperature organic faciess preparation method, the present invention can be using more lower boiling organic under normal pressure
The preparation of quantum dot realized by solvent so that organic solvent is more convenient for reclaiming, and not only reduces cost, and more friendly to environment
Good.It should be noted that the preparation of quantum dot is a kind of nano level micromanagement reaction, extremely quick to each reaction condition
Sense, reaction condition variation slightly will cause large effect to quantum dot product.The present invention is not simple by quantum
The pressure of point preparation reaction improves, but the multiple other reaction conditions in quantum dot preparation process are groped accordingly
With adjustment it was demonstrated that preparation and the probability producing high-quality quantum dot under high pressure.
High pressure makes the elevation of boiling point of the first organic solvent.The corresponding high pressure range of different organic solvents is different.
In a preferred embodiment, high pressure range is 0.2mpa 5mpa.
There is complexation reaction in cation precursor and part in the first organic solvent, form cationic ligand compound, and
It is dissolved in the first organic solvent.
Cation precursor includes one or more cation precursor compounds.In one preferred embodiment, sun
Ion precursor includes at least one in following compound: the compound of i-th race's metallic element, the chemical combination of the i-th i race metallic element
Thing, the compound of the i-th ii race metallic element, the compound of the i-th v race metallic element, transition metal element compound.Excellent at one
Select in embodiment, cation precursor include at least one in following metallic element: cd, zn, hg, cu, ag, ni, co, fe,
mn、ti、zr、in、pb.In one preferred embodiment, cation precursor includes at least one in following compound: gold
Belong to oxide, metal carbonate, metal halide, metal alkoxide, metal mercaptide salt, metal acid imide, metal alkyl, metal virtue
Base salt, metal complex, metal solvent compound.In a detailed embodiment, cation precursor is included in following compound
At least one: zinc chloride, zinc acetate, zinc stearate, zinc carbonate, zinc oxide, Aska-Rid., cadmium acetate, cadmium stearate, carbonic acid
Cadmium, Caddy (Cleary), Indium sesquioxide., indium acetate, carbonic acid indium, indium chloride.
In one preferred embodiment, the first part includes but is not limited to fatty acid, alkylamine, alkylphosphines, alkyl
One of phosphine oxide, phosphonic acids or multiple.Preferably, fatty acid include capric acid, Oleic acid (oleic acid, abbreviation oa), ten
Diacid, tetradecylic acid, hexadecylic acid or stearic acid.
First organic solvent is used for dissolving cation precursor compound or anion pre-cursor compounds and various part
Compound, it is desirable to have stronger solvability, and keep stably being not involved in chemical reaction.For meeting the needs of pyroreaction, the
One organic solvent need to have high boiling point.Additionally due to using in a large number as solvent, use cost problem and environmental pollution need to be considered
Problem.With respect to the organic solvent in the preparation of existing quantum dot, first organic solvent of the present invention has shorter carbochain, more
It is easy to recycle, by great reduces cost, it is to avoid environmental pollution.
In one preferred embodiment, the first organic solvent include alkane, alkene that carbon atom number range is 6 18,
At least one in alkanol, alkylamine, Arrcostab, fatty acid, alkyl hydrosulfide.Preferably, the carbon number of the first organic solvent
Scope is 8 12.Preferably, the fusing point of the first organic solvent is less than 25 DEG C, and boiling point is higher than 100 DEG C.Preferably, first is organic molten
The fusing point of agent is less than 20 DEG C, and boiling point is higher than 100 DEG C.
In one preferred embodiment, the first organic solvent includes one of following compound: 1 heptane, 1 pungent
Alkane, 1 nonane, 1 decane, 1 hendecane, 1 dodecane, 1 tridecane, 1 tetradecane, 1 heptene, 1 octene, 1 nonene, 1
Decene, 1 hendecene, 1 laurylene, 1 tridecylene, 1 tetradecene, 1 hexylamine, 1 heptyl amice, 1 octylame, 1 nonyl amine, 1 decyl amine,
1 undecylamine, 1 lauryl amine, 1 cetylamine, 1,12 diamino dodecane, 1,18 diaminourea octadecanes, 1,16 diaminourea ten
Six alkane, the 1,14 diaminourea tetradecanes, 1 enanthol, 1 capryl alcohol, 1 nonyl alcohol, 1 decanol, 1 hexadecanol, 1 lauryl alcohol, 10 three
Alcohol, 1 tetradecyl alchohol, acetic acid dodecyl ester, 1 valeric acid, 1 caproic acid, 1 enanthic acid, 1 octanoic acid, 1 n-nonanoic acid, 1 capric acid, undecanoic acid,
Lauric acid/dodecanoic acid, tridecanoic acid, tetradecylic acid, 1 decyl mercaptan, 1 undecyl mercaptan, 1 lauryl mercaptan, 1 tetradecanylthioalcohol.
In one preferred embodiment, except low boiling high temperature organic solvent in the first organic solvent, also include with
One of lower compound: 1 hexadecylene, 10 seven alkene, 1 octadecylene, 1 18-amine., oleyl amine, Oleic acid.In present embodiment
In, the ratio shared by above-claimed cpd is not higher than 10%.
In the present invention, anionic pre-cursors are selected from simple substance, covalent compound or ionic compound.Preferably implement at one
In mode, anionic pre-cursors include at least one following element: element sulphur, selenium element, P elements, tellurium element, arsenic element.One
In individual specific embodiment, anionic pre-cursors include at least one in following material: sulphur simple substance, hydrogen sulfide, selenium simple substance, oxygen
Change selenium, zinc phosphide, hydrogen phosphide, zinc arsenide.
In one preferred embodiment, anionic pre-cursors in the way of anionic pre-cursors solution with described cation
Ligand solution mixes.In a detailed embodiment, before mixing with cationic ligand solution, anionic pre-cursors and
Two parts, the second organic solvent are mixed to form anionic pre-cursors solution.In a detailed embodiment, joining with cation
Before liquid solution mixing, anionic pre-cursors and Ligands are mixed to form anionic pre-cursors solution.Ligands are organic with second
The range of choice of solvent is with the first part as above and the first organic solvent.In one preferred embodiment, second
Organic solvent is selected from tributyl phosphate (tributyl phosphate, abbreviation tbp).
First temperature is used for causing the chemical reaction generating quantum dot.The chemistry that in the present invention, the first temperature is caused is anti-
Should, refer to the reaction of reaction, cationic ligand and anionic pre-cursors of cation precursor and anionic pre-cursors, cationic ligand with
The reaction of anion ligand or the reaction of cation precursor and anion ligand.First temperature range of the present invention is 150
350℃.Preferably, the first temperature range is 200 350 DEG C.Different cation precursor, anionic pre-cursors and different pressures
Under power, reaction temperature is different.
Pressure in reactor in the present invention is higher, and the first required temperature is lower.In one preferred embodiment,
First temperature range is 150 250 DEG C.
In one preferred embodiment, preparation method also includes step c): the product in step b) is added further
Heat to second temperature and keeps a period of time.Preferably, second temperature scope is 200 350 DEG C.It is highly preferred that second temperature model
Enclose for 250 300 DEG C.Pressure in reactor is higher, and required second temperature is also lower.
In one preferred embodiment, the pressure range in reactor is 0.2mpa 0.5mpa, the first reaction temperature
Scope is 200 250 DEG C.In one preferred embodiment, the first range of reaction temperature is 200 250 DEG C, the second reaction temperature
Degree scope is 250 300 DEG C.
In one preferred embodiment, the pressure range in reactor is 0.5mpa 1mpa, the first reaction temperature model
Enclose for 150 220 DEG C.In one preferred embodiment, the first range of reaction temperature is 150 220 DEG C, the second reaction temperature
Scope is 220 260 DEG C.
In one preferred embodiment, the quantum dot of the present invention is nucleocapsid structure, and preparation method also includes step d):
Add the precursor compound needed for synthesis shell further in the reactor of step b), and keep a period of time.Concrete at one
Preferred embodiment in, synthesis shell needed for precursor compound be dissolved in the organic solvent have surfactant formed
One or more precursor compound solution, add the precursor compound needed for synthesis shell further in the reactor of step b)
Solution, and keep a period of time.Often it is repeated once step d), form one layer of shell.In the synthesis step of each layer of shell, add synthesis
Precursor compound needed for this layer of shell.
In one preferred embodiment, the preparation method of the present invention also includes the step purifying: to final reaction
Add alcohol in thing, produce precipitation, by centrifugation at least one times, washing, again centrifugation step, the quantum solid point of purification will be finally given
Body, distributes it to preserve in organic solvent.
The invention allows for a kind of quantum dot that can send fluorescence, it is obtained by preparation method as above.
In one preferred embodiment, quantum dot be selected from following compound in any one: cdse, cds,
cdte、znse、zns、inp、inas、cdznse、cdzns、cdznte、inznp、inznas.
Various structures are included by the quantum dot that preparation method of the present invention is obtained.In a preferred embodiment, quantum
Point does not have the presence of shell for single nanocrystal, outer layer except functional group.In a preferred embodiment, quantum dot bag
Include core and at least one of which shell.In a detailed embodiment, quantum dot includes core and one layer of shell, in nucleocapsid structure.Another
In individual specific embodiment, quantum dot includes core and two-layer shell, in nucleocapsid structure.
In a detailed embodiment, quantum dot is selected from any one in following compound: cdse/zns, cdse/
cds/zns、cdses/zns、cdte/zns、inp/zns、cdznse/zns、znse/zns、inas/zns、inznp/zns、
inznas/zns.
The present invention preparation quantum dot there is higher quantum efficiency and narrower half-peak breadth.Preferably implement at one
In mode, the quantum efficiency of quantum dot is higher than 80%, and half-peak breadth is less than 30nm.In one preferred embodiment, quantum dot
Quantum efficiency be higher than 90%, half-peak breadth be less than 25nm.
Embodiment 1
A kind of preparation method of cdse/znse/zns quantum dot, comprises the following steps: by 0.128g cdo, 1.83g zn
(ac)2, 15ml oa and 35ml 1 tetradecene, be placed in reactor system, reactor is airtight, be warming up to 100 DEG C, take out true
It is passed through argon after sky.After 30min, it is warming up to 300 DEG C, kettle pressure is shown as 0.2mpa, into reactor, is pressurized to 0.5mpa.
Inject, to kettle internal high pressure, the se/tbp that 3ml concentration is 2m, generate cdse core.After 30min, by 10ml/h speed into kettle
Deca 2ml concentration is the se/tbp of 1m, grows znse shell.Then Deca 4ml concentration is the s/tbp of 1m, grows zns shell.
Stopped reaction, is passed through cooling water and is down to room temperature, reactant liquor is centrifuged and uses organic solvent washing, is finally redispersed in quantum dot
In organic solvent.After tested, the quantum dot emission peak wavelength peak that the present embodiment is obtained is 625nm, a width of 27nm of half-peak.
Embodiment 2
Same as Example 1, different is, substitutes 1 tetradecene with 1 laurylene.After tested, the present embodiment is obtained
Quantum dot emission peak wavelength peak be 608nm, a width of 30nm of half-peak, as shown in Figure 1.
Embodiment 3
Same as Example 1, different is, substitutes 1 tetradecene with 1 decene, replaces oa with 1 lauric acid/dodecanoic acid.Through surveying
Examination, the quantum dot emission peak wavelength peak that the present embodiment is obtained is 615nm, a width of 29nm of half-peak.
Embodiment 4
Same as Example 1, different is, is warming up to 200 DEG C, is pressurized to 2mpa in reactor.After tested, this reality
Applying the prepared quantum dot emission peak wavelength peak of example is 610nm, a width of 32nm of half-peak.
Embodiment 5
Same as Example 1, different is, injects, to kettle internal high pressure, the se/tbp, 30s that 1ml concentration is 2m
Afterwards, by 10ml/h speed to Deca 2ml concentration in kettle be 1m se/tbp.After tested, the quantum dot that the present embodiment is obtained is sent out
Penetrating peak wavelength peak is 464nm, a width of 23nm of half-peak, as shown in Figure 2.
Embodiment 6
A kind of preparation method of inp/zns quantum dot, comprises the following steps: in reactor add 150mg indium acetate,
100mg zinc acetate, 600mg oa and 40ml 1 laurylene, evacuation is simultaneously heated to 100 DEG C, is passed through argon.It is heated to 230
DEG C, kettle pressure is shown as 0.2mpa, is pressurized to 0.5mpa into reactor.First inject 1ml phosphatization under kettle internal liquid level
Hydrogen/oleyl amine solution, reinjects 1ml tributyl phosphorus.Keep the temperature at 230 DEG C of 10min, be then down to 200 DEG C.To in three-necked bottle
Reinject 7.5ml hydrogen phosphide/laurylene solution.It is heated to 200 DEG C, adds the s/tbp that 8ml concentration is 1m, grow zns shell.
Reactant liquor is centrifuged and purifies twice with washing with acetone, in organic solvent by quantum dot redispersion finally.After tested, this enforcement
The quantum dot emission peak wavelength peak that example is obtained is 588nm, a width of 73nm of half-peak, as shown in Figure 3.
Described above, by the method for the present invention, can be high-quality using the relatively low solvent synthesis of boiling point at a lower temperature
The quantum dot of amount.
Although inventor technical scheme has been done with elaboration in greater detail and enumerate it will be appreciated that for
For those skilled in the art, above-described embodiment is modified and/or flexible or be obvious using equivalent replacement scheme
, all can not depart from the essence of spirit of the present invention, the term occurring in the present invention be used for the elaboration of technical solution of the present invention and
Understand, can not be construed as limiting the invention.
Claims (20)
1. a kind of preparation method of quantum dot is it is characterised in that comprise the following steps: a) by cation precursor, the first part,
One organic solvent is mixed to form cationic ligand solution；B) under airtight environment under high pressure and in atmosphere of inert gases, by the moon
Ion precursor is mixed with described cationic ligand solution, and is heated to the first temperature described cationic ligand of initiation and described the moon
There is chemical reaction in ion precursor, generate quantum dot.
2. preparation method according to claim 1 it is characterised in that: described high pressure range be 0.2mpa 5mpa.
3. preparation method according to claim 1 it is characterised in that: described cation precursor includes i-th race's metallic element
Compound, the compound of the i-th i race metallic element, the compound of the i-th ii race metallic element, the chemical combination of the i-th v race metallic element
Thing or transition metal element compound.
4. preparation method according to claim 3 it is characterised in that: described cation precursor is included in following metallic element
At least one: cd, zn, hg, cu, ag, ni, co, fe, mn, ti, zr, in, pb.
5. preparation method according to claim 1 it is characterised in that: described cation precursor is included in following compound
At least one: metal-oxide, metal carbonate, metal halide, metal alkoxide, metal mercaptide salt, metal acid imide, alkyl
Metal, metal aryl salt, metal complex, metal solvent compound.
6. preparation method according to claim 1 it is characterised in that: described cation precursor is included in following compound
At least one: zinc chloride, zinc acetate, zinc stearate, zinc carbonate, zinc oxide, Aska-Rid., cadmium acetate, cadmium stearate, cadmium carbonate,
Caddy (Cleary), Indium sesquioxide., indium acetate, carbonic acid indium, indium chloride.
7. preparation method according to claim 1 it is characterised in that: described first part includes fatty acid, alkylamine, alkane
One of base phosphine, alkyl phosphine oxide, phosphonic acids or multiple.
8. preparation method according to claim 1 it is characterised in that: described fatty acid include capric acid, Oleic acid, lauric acid/dodecanoic acid,
Tetradecylic acid, hexadecylic acid or stearic acid.
9. preparation method according to claim 1 it is characterised in that: the fusing point of described first organic solvent be less than 25 DEG C,
Boiling point is higher than 100 DEG C.
10. preparation method according to claim 1 it is characterised in that: described first organic solvent includes following compound
In at least one: 1 heptane, 1 octane, 1 nonane, 1 decane, 1 hendecane, 1 dodecane, 1 tridecane, 1 tetradecane,
1 heptene, 1 octene, 1 nonene, 1 decene, 1 hendecene, 1 laurylene, 1 tridecylene, 1 tetradecene, 1 hexylamine, 1 heptan
Amine, 1 octylame, 1 nonyl amine, 1 decyl amine, 1 undecylamine, 1 lauryl amine, 1 cetylamine, 1,12 diamino dodecane, 1,18 2
Amino octadecane, 1,16 diaminourea hexadecanes, the 1,14 diaminourea tetradecanes, 1 enanthol, 1 capryl alcohol, 1 nonyl alcohol, 1 decanol, 1
Hexadecanol, 1 lauryl alcohol, 1 tridecanol, 1 tetradecyl alchohol, acetic acid dodecyl ester, 1 valeric acid, 1 caproic acid, 1 enanthic acid, 1 octanoic acid,
1 n-nonanoic acid, 1 capric acid, undecanoic acid, lauric acid/dodecanoic acid, tridecanoic acid, tetradecylic acid, 1 decyl mercaptan, 1 undecyl mercaptan, 1 lauryl mercaptan, 10
Four mercaptan.
11. preparation methoies according to claim 1 it is characterised in that: described anionic pre-cursors be selected from simple substance, covalent combination
Thing or ionic compound.
12. preparation methoies according to claim 1 it is characterised in that: described anionic pre-cursors include below at least one
Element: sulfur, selenium, phosphorus, tellurium, arsenic.
13. preparation methoies according to claim 1 it is characterised in that: mixing it with described cationic ligand solution
Before, described anionic pre-cursors and Ligands, the second organic solvent are mixed to form anionic pre-cursors solution, described anionic pre-cursors
Mixed with described cationic ligand solution in the way of described anionic pre-cursors solution.
14. preparation methoies according to claim 1 it is characterised in that: described first temperature range be 150 300 DEG C.
15. preparation methoies according to claim 1 it is characterised in that: described first temperature range be 200 250 DEG C.
16. preparation methoies according to claim 1 it is characterised in that: described quantum dot be selected from compound one
Kind: cdse, cds, cdte, znse, zns, inp, inas, cdznse, cdzns, cdznte, inznp, inznas.
17. preparation methoies according to claim 1 it is characterised in that: described preparation method also includes step c): by step
B) reactant in is further heated to second temperature and keeps a period of time.
18. preparation methoies according to claim 18 it is characterised in that: described second temperature scope be 250 350 DEG C.
19. preparation methoies according to claim 1 it is characterised in that: described preparation method also includes step d): to step
B) add the precursor compound needed for synthesis shell in reactor further, and keep a period of time.
A kind of 20. quantum dots are it is characterised in that be obtained by described preparation method arbitrary in claim 1 19.
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| PCT/CN2016/098745 WO2018032564A1 (en) | 2016-08-17 | 2016-09-12 | High-pressure preparation method for quantum dot, and quantum dot |
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| CN107098324A (en) * | 2017-05-08 | 2017-08-29 | 苏州星烁纳米科技有限公司 | A kind of preparation method of indium phosphide quantum dot |
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| WO2018032564A1 (en) | 2018-02-22 |
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