CN107400507A - A kind of nearly mid and far infrared alloy quantum dot and preparation method thereof - Google Patents
A kind of nearly mid and far infrared alloy quantum dot and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of nearly mid and far infrared alloy quantum dot and preparation method thereof.The preparation method of nearly mid and far infrared alloy quantum dot provided by the invention, including：The first cation, the second cation, fatty acid part, amine part, phosphoric acid class part and non-coordinating solvent are mixed first, heating obtains cation precursor；First cationic source includes lead source；Second cation includes zinc ion or cadmium ion.Stratum nucleare anion is injected into resulting cation presoma again, nuclear reaction is carried out into and obtains quantum dot presoma；Shell anion is added, shelling is carried out and reacts to obtain nearly mid and far infrared alloy quantum dot；Stratum nucleare anion and shell anion are independently selected from for selenium, sulphur or tellurium.The present invention prepares core shell structure alloy infrared quantum point using one pot of hot injection method of organic solvent of high temperature, and the nuclear shell structure quantum point launch wavelength being prepared is adjustable, and particle monodispersity is good and yield is high.
Description
Technical field
The present invention relates to nano-functional material technical field, more particularly to a kind of nearly mid and far infrared alloy quantum dot and its system
Preparation Method.
Background technology
Developing rapidly and improving with human sciences's civilization, various infrared application device such as detectors, solar-electricity
The life to the mankind such as pond, biomarker imaging produces subtle influence.Infrared quantum point, was widely used in spy in the last few years
Survey device, solar cell and biomarker field.But due to material category, structure and the method limitation synthesized, cause to synthesize
Infrared quantum point there is fluorescence adjustability difference or fluorescence efficiency it is low the problem of, always can not efficiently be applied to detection
Device, solar cell point and bio-imaging etc..
Graded alloy quantum dot XPbY@XY (Y=S, Se or Te, X=Zn, Cd) due to quantum dot core XPbY (Y=S, Se or
Te, X=Zn, Cd) band-gap tuning act on cause quantum dot fluorescence reach near-infrared, in infrared or even far infrared transmission ripple
Section, can be widely used in various infrared device applications.
The preparation method of graded alloy quantum dot mainly has at present：Colloid chemistry methods, i.e., have in organic solvent with metal
Machine thing is presoma, and at 350 DEG C prepared by back flow reaction；Hydro-thermal method, refer in special closed reactor, by the way that water is heated
The method that alloy quantum dot is made to supercritical temperature or close to supercritical temperature；Microporous medium method refers to that quantum dot will be synthesized
Ion be incorporated into the duct of mesoporous material and prepare alloy quantum dot；Reverse micro emulsion self-assemble mould board method, that is, pass through gas-liquid
Phase reaction prepares the quantum dot with well-crystallized performance.
But there is the problem of quantum dot bad dispersibility and low yield for above-mentioned synthetic method.
The content of the invention
It is an object of the invention to provide a kind of nearly mid and far infrared alloy quantum dot and preparation method thereof.It is provided by the invention
Preparation method is simple to operate, the quantum dot favorable dispersibility being prepared and quantum dot yield height.
The invention provides a kind of preparation method of nearly mid and far infrared alloy quantum dot, comprise the following steps：
(1) by the first cationic source, the second cationic source, fatty acid part, amine part, phosphoric acid class part and non-match somebody with somebody
Position solvent mixing, heating obtain cation precursor；First cation includes lead source；Second cationic source includes zinc
Source or cadmium source；
(2) stratum nucleare negative ion source is injected in the cation presoma obtained to the step (1), nuclear reaction is carried out into, obtains
To quantum dot presoma；
(3) shell negative ion source is added in the quantum dot presoma obtained to the step (2), shelling reaction is carried out, obtains
To the nearly mid and far infrared alloy quantum dot with core shell structure；
Selenium, sulphur or tellurium is selected independently in the stratum nucleare negative ion source and shell negative ion source.
Preferably, the mol ratio of the first cationic source and the second cationic source is (0.0001~1) in the step (1)：
(1~100000).
Preferably, the temperature of heating is 100 DEG C in the step (1)；The time of the heating is 40min.
Preferably, the amount of the total material of shell anion is in stratum nucleare anion and the step (3) in the step (2)
1.5~100000 times of the amount of the material for the cation precursor that the step (2) is injected to stratum nucleare negative ion source.
Preferably, the temperature in the step (2) into nuclear reaction is 300 DEG C, and the time into nuclear reaction is 10min.
Preferably, stratum nucleare negative ion source is injected in the form of stratum nucleare negative ion source solution in the step (2)；The stratum nucleare
The solvent of negative ion source solution is positive tributylphosphine and/or tri-n-octyl phosphine.
Preferably, the temperature that shelling is reacted in the step (3) is 310 DEG C, and the time of the shelling reaction is 60min.
Preferably, shell negative ion source is added in the form of shell negative ion source solution in the step (3)；The shell
The solvent of negative ion source solution is positive tributylphosphine and/or tri-n-octyl phosphine.
Preferably, also include after step (3) the shelling reaction：Obtained shelling reaction product is cooled down successively,
Extraction, centrifuge and dry, obtain nearly mid and far infrared alloy quantum dot.
Present invention also offers nearly mid and far infrared alloy quantum dot prepared by the preparation method described in above-mentioned technical proposal, tool
There is core shell structure, including chemical composition is XPbY1Nucleome and chemical composition be XY2Shell；The X is Zn or Cd；The Y1
And Y2Independently selected from S, Se or Te.
The preparation method of nearly mid and far infrared alloy quantum dot provided by the invention, comprises the following steps：First by the first sun
Ion gun, the second cationic source, fatty acid part, amine part, phosphoric acid class part and non-coordinating solvent mixing, heating obtain
Cation precursor；Wherein the first cationic source includes lead source；Second cationic source includes zinc source or cadmium source.Again to resulting
Stratum nucleare anion is injected in cation presoma, nuclear reaction is carried out into and obtains quantum dot presoma；After add shell anion
Source, carry out shelling and react to obtain nearly mid and far infrared alloy quantum dot；Wherein, stratum nucleare negative ion source and shell negative ion source be independently
Selected from for selenium, sulphur or tellurium.The present invention prepares core shell structure alloy infrared quantum point using one pot of hot injection method of organic solvent of high temperature,
Inexpensive, simple to operate and short preparation period, reappearance are high；The nuclear shell structure quantum point launch wavelength being prepared
Adjustable, particle monodispersity is good and yield is high.
Embodiment
The invention provides a kind of preparation method of nearly mid and far infrared alloy quantum dot, comprise the following steps：
(1) by the first cationic source, the second cationic source, fatty acid part, amine part, phosphoric acid class part and non-match somebody with somebody
Position solvent mixing, heating obtain cation precursor；First cationic source includes lead source；Second cationic source includes
Zinc source or cadmium source；
(2) stratum nucleare negative ion source is injected in the cation presoma obtained to the step (1), nuclear reaction is carried out into and obtains
Quantum dot presoma；
(3) shell negative ion source is added in the quantum dot presoma obtained to the step (2), shelling reaction is carried out, obtains
To the nearly mid and far infrared alloy quantum dot with core shell structure；
The stratum nucleare negative ion source and shell negative ion source are independently selected as selenium, sulphur or tellurium.
The present invention by the first cationic source, the second cationic source, fatty acid part, amine part, phosphoric acid class part and
Non-coordinating solvent mixes, and heating obtains cation precursor.In the present invention, the temperature of the heating is preferably 100 DEG C, described
The time of heating is preferably 40min.In the present invention, the heating is preferably carried out under vacuum.The present invention adds to described
The embodiment of heat does not have particular/special requirement, using mode of heating well-known to those skilled in the art.
In the present invention, first cationic source includes lead source；The lead source preferably includes lead acetate, lead oxide, chlorine
Change the one or more in lead, lauric acid/dodecanoic acid lead, tetradecylic acid lead, hexadecylic acid lead, lead stearate and plumbi oleas.The present invention is to the lead
The specific source in source does not have particular/special requirement, using commercial goods well-known to those skilled in the art.
In the present invention, second cationic source includes zinc source or cadmium source；The zinc source preferably includes zinc acetate, oxidation
One or more in zinc, zinc chloride, zinc laurate, tetradecylic acid zinc, hexadecylic acid zinc, zinc stearate and zinc oleate；The cadmium source
Preferably include in cadmium acetate, cadmium oxide, caddy, lauric acid/dodecanoic acid cadmium, tetradecylic acid cadmium, hexadecylic acid cadmium, cadmium stearate and cadmium oleate
It is one or more.The present invention does not have particular/special requirement to the source in the zinc source and cadmium source, and use is well known to those skilled in the art
Zinc source and cadmium source commercial goods.
In the present invention, the mol ratio of first cationic source and the second cationic source is preferably (0.0001~1)：(1
~100000).
In the present invention, the fatty acid part preferably includes lauric acid/dodecanoic acid, tetradecylic acid, hexadecylic acid, stearic acid and oleic acid
In one or more；The amine part preferably includes one kind in lauryl amine, tetradecy lamine, cetylamine, octadecylamine and oleyl amine
It is or a variety of；The phosphoric acid class part preferably includes TOPO and/or tributylphosphine.The present invention is to the fatty acid
The specific source of part, amine part and phosphoric acid class part does not have particular/special requirement, using city well-known to those skilled in the art
Sell commodity.
In the present invention, the non-coordinating solvent preferably includes 1- octadecylenes (ODE) or trioctylamine.The present invention is to the 1-
The specific source of octadecylene does not have particular/special requirement, using commercial goods well-known to those skilled in the art.
After obtaining cation precursor, the present invention injects stratum nucleare negative ion source into the obtained cation presoma,
Carry out into nuclear reaction and obtain quantum dot presoma.In the present invention, the stratum nucleare negative ion source is selenium, sulphur or tellurium；The present invention is right
The source of the selenium, sulphur and tellurium does not have particular/special requirement, using well-known to those skilled in the art.
In the present invention, the stratum nucleare negative ion source injects preferably in the form of stratum nucleare negative ion source solution；The stratum nucleare
The solvent of negative ion source solution is preferably positive tributylphosphine and/or tri-n-octyl phosphine.The present invention is to the positive tributylphosphine and three
The source of n-octyl phosphine does not have particular/special requirement, using commercial goods well-known to those skilled in the art.The present invention to institute
When stating injection stratum nucleare negative ion source in cation precursor, the temperature of the cation precursor is preferably 300 DEG C.In the present invention
In, the charge velocity of the stratum nucleare negative ion source is preferably quick.In the present invention, the injection of the stratum nucleare negative ion source is preferred
Carried out under protective atmosphere, the protective atmosphere is preferably argon gas.
The present invention injects stratum nucleare negative ion source into the cation presoma, carries out into nuclear reaction and obtains body before quantum dot
Body, the composition of the quantum dot precursor is preferably XPbY1, wherein, the X is Zn or Cd；The Y1For S, Se or Te.In this hair
In bright, the quantum dot precursor is specially ZnPbS, ZnPbSe, ZnPbTe, CdPbS, CdPbSe or CdPbTe.In the present invention,
The temperature into nuclear reaction is preferably 300 DEG C；The time into nuclear reaction is 10min.In the present invention, the nucleation is anti-
Preferably it should be carried out under protective atmosphere, the protective atmosphere is preferably argon gas.In the present invention, the stratum nucleare negative ion source injection
During cation precursor, the stratum nucleare negative ion source preferably reacts to obtain body before quantum dot with cation precursor
Body.
After obtaining quantum dot presoma, the present invention adds shell negative ion source into the obtained quantum dot presoma,
Shelling reaction is carried out, obtains the nearly mid and far infrared alloy quantum dot with core shell structure.In the present invention, the shell anion
Source is selenium, sulphur or tellurium；The present invention does not have particular/special requirement to the source of the selenium, sulphur and tellurium, ripe using those skilled in the art institute
Know.In the present invention, the species of the shell negative ion source and the species of stratum nucleare negative ion source are preferably consistent.
In the present invention, the amount of the total material of the stratum nucleare anion and the shell anion for it is described to stratum nucleare the moon from
1.5~100000 times of the amount of the material of the cation precursor of son injection.
In the present invention, the shell negative ion source injects preferably in the form of shell negative ion source solution；The shell
The solvent of negative ion source solution is preferably positive tributylphosphine and/or tri-n-octyl phosphine.The present invention is to the positive tributylphosphine and three
The source of n-octyl phosphine does not have particular/special requirement, using commercial goods well-known to those skilled in the art.The present invention to institute
When stating injection shell negative ion source in quantum dot precursor, the temperature of the quantum dot precursor is preferably 310 DEG C.In the present invention
In, the injection of the shell negative ion source is preferably carried out under protective atmosphere, and the protective atmosphere is preferably argon gas.
The present invention injects shell negative ion source into the quantum dot precursor, carries out shelling and reacts to obtain nearly mid and far infrared
Alloy quantum dot.In the present invention, the temperature of shelling reaction is preferably 310 DEG C, and the time of the shelling reaction is preferably
60min.Using the quantum dot precursor as nucleome, shell negative ion source coats to form shell the present invention in nucleome, obtains near
Mid and far infrared alloy quantum dot.In the present invention, the nearly mid and far infrared alloy quantum dot has core shell structure, including chemical group
As XPbY1Nucleome and chemical composition be XY2Shell；The X is Zn or Cd；The Y1And Y2Independently selected from S, Se or
Te.In the present invention, the nearly mid and far infrared alloy quantum dot is with XPbY1@XY2Represent.
In the present invention, the nearly mid and far infrared alloy quantum dot is specially ZnPbS@ZnS, ZnPbSe@ZnS, ZnPbTe@
ZnS、ZnPbS@ZnSe、ZnPbSe@ZnSe、ZnPbTe@ZnSe、ZnPbS@ZnTe、ZnPbSe@ZnTe、ZnPbTe@ZnTe、
CdPbS@CdS, CdPbSe@CdS or CdPbTe@CdS.In the present invention, the shelling reaction is preferably carried out under protective atmosphere,
The protective atmosphere is preferably argon gas.In the present invention, during the shell negative ion source injection quantum dot precursor, institute
Shell negative ion source is stated preferably to react to obtain nearly mid and far infrared alloy quantum dot with quantum dot precursor.
After the shelling reaction, the present invention preferably also includes：Obtained shelling reaction product is cooled down successively, extracted
Take, centrifuge and dry, obtain nearly mid and far infrared alloy quantum dot.
In the present invention, the temperature after the cooling is preferably 50 DEG C.The present invention is not special to the mode of the cooling
It is required that using the type of cooling well-known to those skilled in the art.
The present invention is extracted after preferably the shelling reaction product after the cooling is mixed with extractant, remote in obtaining closely
Infrared alloy quantum dot solution.In the present invention, the extractant is preferably the mixture of methanol and n-hexane；The n-hexane
Volume ratio with methanol is preferably 1:2~1:10.
In the present invention, the mixing is preferably carried out under agitation, and the stirring is preferably magnetic agitation；It is described to stir
The time mixed is preferably 5~20min.
The present invention is preferably stood after the completion of the stirring, makes mixed solution split-phase.In the present invention, mixed after the split-phase
The upper strata for closing solution is nearly mid and far infrared quantum dot solution, and lower floor is impurity, remaining part and methanol.The present invention is preferably by described in
The lower floor of mixed solution removes, and obtains nearly mid and far infrared quantum dot solution；The removing method of lower floor's solution is preferably to inject
Device extracts.In the present invention, the number of the extraction is preferably 4 times.
The present invention preferably by it is described it is near in remote quantum dot solution with being centrifuged after precipitant mix.In the present invention, institute
It is preferably acetone or acetonitrile to state precipitating reagent；The precipitation of the acetone or acetonitrile remote quantum dot in can promoting closely, is easy to centrifuge
In journey it is near in remote quantum dot and solvent separation.
Preferably the solid that the centrifugation obtains is dried by the present invention, obtains nearly mid and far infrared quantum dot.In the present invention
In, the drying is preferably to be dried in vacuo；The vacuum drying time is preferably 30min.
Present invention also offers nearly mid and far infrared quantum dot prepared by above-mentioned technical proposal, has core shell structure, including change
It is XPbY to learn composition1Nucleome and chemical composition be XY2Shell；The X is Zn or Cd；The Y1And Y2Independently selected from S,
Se or Te.
The nearly mid and far infrared quantum dot is preferably scattered in organic solvent by the present invention to be preserved；The organic solvent is preferred
For n-hexane, toluene or chloroform.
In order to further illustrate the present invention, with reference to embodiment to nearly mid and far infrared quantum dot provided by the invention and its
Preparation method is described in detail, but they can not be interpreted as into limiting the scope of the present invention.
Embodiment 1:
Cadmium acetate, lead acetate, oleic acid, lauryl amine and TOPO part are added into 100mL three-necked flasks, it is non-
Ligand solvent 1- octadecylenes, vacuumized under the conditions of 100 DEG C 40 minutes or so, obtain cation precursor.
Argon gas is passed through in reaction system, is heated to 300 DEG C, is rapidly injected a certain amount of selenium for being dissolved in tributylphosphine, is incubated
Form quantum dot nucleus CdPbSe within 10 minutes or so.
310 DEG C are warming up to again, a certain amount of selenium for being dissolved in tributylphosphine is added dropwise, and 1h is incubated at 310 DEG C, it is remote red in obtaining closely
Outer alloy quantum dot CdPbSe CdSe, its nucleus component are CdPbSe, and shell component is CdSe.
The nearly mid and far infrared alloy quantum dot CdPbSe@CdSe being prepared are subjected to separating-purifying：
(1) quantum dot obtained after reaction drop is cooled to 50 DEG C, it is 2 to add volume ratio:1 methanol and n-hexane it is mixed
Close extractant, 5 minutes or so rear static layerings of magnetic agitation 10 minutes.Wherein, bottom is the clear, colorless methanol dissolved with impurity
Solution；Upper strata is quantum dot solution；Methanol solution with syringe from bottom extraction dissolved with magazine, the quantum dot for collecting upper strata are molten
Liquid, complete single extraction.Extractant is added in quantum dot solution again to be extracted, and is repeated four times with this.
(2) acetone is added in the quantum dot solution after four extractions to be centrifuged, supernatant is outwelled, by solid in vacuum
Drying box dries half an hour, obtains nearly mid and far infrared alloy quantum dot；(3) obtained quantum dot is dispersed in n-hexane again
Preserve.
Embodiment 2
Zinc acetate, lead acetate, lauric acid/dodecanoic acid, tetradecy lamine and TOPO part are added into 100mL three-necked flasks,
Non-coordinating solvent trioctylamine, vacuumized under the conditions of 100 DEG C 40 minutes or so, obtain cation precursor.
Argon gas is passed through in reaction system, is heated to 300 DEG C, is rapidly injected a certain amount of sulphur for being dissolved in tributylphosphine, is incubated
Form quantum dot nucleus ZnPbS within 10 minutes or so.
310 DEG C are warming up to again, a certain amount of sulphur for being dissolved in tributylphosphine is added dropwise, and 1h is incubated at 310 DEG C, it is remote red in obtaining closely
Outer alloy quantum dot ZnPbS ZnS, its nucleus component are ZnPbS, and shell component is CdSe.
The nearly mid and far infrared alloy quantum dot ZnPbS@ZnS being prepared are subjected to separating-purifying：
(1) quantum dot obtained after reaction drop is cooled to 50 DEG C, it is 2 to add volume ratio:1 methanol and n-hexane it is mixed
Close extractant, 5 minutes or so rear static layerings of magnetic agitation 10 minutes.Wherein, bottom is the clear, colorless methanol dissolved with impurity
Solution；Upper strata is quantum dot solution；Methanol solution with syringe from bottom extraction dissolved with magazine, the quantum dot for collecting upper strata are molten
Liquid, complete single extraction.Extractant is added in quantum dot solution again to be extracted, and is repeated four times with this.
Acetone is added in quantum dot solution after four extractions to be centrifuged, and outwells supernatant, solid is done in vacuum
Dry case dries half an hour, obtains nearly mid and far infrared alloy quantum dot；
(2) obtained quantum dot is dispersed in n-hexane again and preserved.
The present invention prepares core shell structure alloy infrared quantum point using one pot of hot injection method of organic solvent of high temperature, and cost is honest and clean
Valency, simple to operate and short preparation period, reappearance are high；The nuclear shell structure quantum point launch wavelength being prepared is adjustable,
Particle monodispersity is good and yield is high.
Claims (10)
1. a kind of preparation method of nearly mid and far infrared alloy quantum dot, comprises the following steps：
(1) by the first cationic source, the second cationic source, fatty acid part, amine part, phosphoric acid class part and noncoordinating molten
Agent mixes, and heating obtains cation precursor；First cationic source includes lead source；Second cationic source includes zinc source
Or cadmium source；
(2) stratum nucleare negative ion source is injected in the cation presoma obtained to the step (1), carries out into nuclear reaction, the amount of obtaining
Son point presoma；
(3) shell negative ion source is added in the quantum dot presoma obtained to the step (2), shelling reaction is carried out, is had
There is the nearly mid and far infrared alloy quantum dot of core shell structure；
Selenium, sulphur or tellurium is selected independently in the stratum nucleare negative ion source and shell negative ion source.
2. preparation method according to claim 1, it is characterised in that the first cationic source and second in the step (1)
The mol ratio of cationic source is (0.0001~1)：(1~100000).
3. preparation method according to claim 1 or 2, it is characterised in that the temperature of heating is 100 in the step (1)
℃；The time of the heating is 40min.
4. preparation method according to claim 1, it is characterised in that stratum nucleare anion and the step in the step (2)
Suddenly the amount of the total material of shell anion is the thing for the cation precursor that the step (2) is injected to stratum nucleare anion in (3)
1.5~100000 times of the amount of matter.
5. preparation method according to claim 1, it is characterised in that the temperature in the step (2) into nuclear reaction is 300
DEG C, the time into nuclear reaction is 10min.
6. preparation method according to claim 1 or 5, it is characterised in that stratum nucleare negative ion source is with core in the step (2)
The form injection of layer negative ion source solution；The solvent of the stratum nucleare negative ion source solution is positive tributylphosphine and/or three n-octyls
Phosphine.
7. preparation method according to claim 1, it is characterised in that the temperature that shelling is reacted in the step (3) is 310
DEG C, the time of the shelling reaction is 60min.
8. the preparation method according to claim 1 or 7, it is characterised in that shell negative ion source is with shell in the step (3)
The form of layer negative ion source solution adds；The solvent of the shell negative ion source solution is positive tributylphosphine and/or three n-octyls
Phosphine.
9. preparation method according to claim 1, it is characterised in that also include after step (3) the shelling reaction：To
To shelling reaction product cooled down, extracted, centrifuged and dried successively, obtain nearly mid and far infrared alloy quantum dot.
10. nearly mid and far infrared alloy quantum dot prepared by preparation method described in claim 1~9 any one, has nucleocapsid knot
Structure, including chemical composition are XPbY1Nucleome and chemical composition be XY2Shell；The X is Zn or Cd；The Y1And Y2It is independent
Ground is selected from S, Se or Te.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219792A (en) * | 2018-02-09 | 2018-06-29 | 纳晶科技股份有限公司 | Quantum dot purification process and quantum dot, device and quantum dot composition |
| CN108659818A (en) * | 2018-06-14 | 2018-10-16 | 嘉兴纳鼎光电科技有限公司 | The synthetic method of quantum dot and the quantum dot of application synthetic method synthesis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219792A (en) * | 2018-02-09 | 2018-06-29 | 纳晶科技股份有限公司 | Quantum dot purification process and quantum dot, device and quantum dot composition |
| CN108219792B (en) * | 2018-02-09 | 2021-05-07 | 纳晶科技股份有限公司 | Quantum dot purification method, quantum dot, device and quantum dot composition |
| CN108659818A (en) * | 2018-06-14 | 2018-10-16 | 嘉兴纳鼎光电科技有限公司 | The synthetic method of quantum dot and the quantum dot of application synthetic method synthesis |
| CN108659818B (en) * | 2018-06-14 | 2021-03-26 | 宁波纳鼎新材料科技有限公司 | Quantum dot synthesis method and quantum dot synthesized by using same |
| CN115477945A (en) * | 2022-09-29 | 2022-12-16 | 岭南师范学院 | Core-shell structure quantum dot and preparation method thereof |
| CN115477945B (en) * | 2022-09-29 | 2024-05-07 | 岭南师范学院 | Core-shell structure quantum dot and preparation method thereof |
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