CN107573924A - A kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots - Google Patents
A kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of more shell CdZnS/CdSe/ZnS core/shell structure quantum dots, using high warm injection method, alternately continuous ionic layer Absorption Growth method and bi precursor method synthesis CdZnS/CdSe/ZnS quantum dots, wherein thering are four kinds of feasible schemes to synthesize this quantum dot again.The present invention by continuously coat different-thickness, the different numbers of plies CdSe and ZnS shells, obtain the wide spectral range of continuously adjustable, have the characteristics that monochromaticjty is good, monodispersity is good and there is narrow and symmetrical fluorescence emission peak, luminous stability can be also effectively improved, possesses more more preferable optical characteristics than single CdZnS quantum dots and CdSe quantum dot or CdZnS/CdSe quantum dots.It is also, continuous to wrap up ZnS shells, thus it is possible to vary the distribution of the electron hole of quantum dot, thus can to prepare a variety of materials of different nature, further apply various aspects by changing the thickness of CdSe shells.
Description
Technical field
The present invention relates to the preparation of nanocrystalline material and application, for a kind of more shell mould CdZnS/CdSe/ZnS core shell knots
The preparation method of structure quantum dot.
Background technology
Nanoscale structures material abbreviation nano material, refer to a kind of powdery being made up of basic granules or lumps it is natural or
Artificial material, one or more three-dimensional dimensions of this basic granules are between 1 nanometer to 100 nanometers, and this basic
The total quantity of grain accounts for more than 50% in all total number of particles of whole material.When the size of particle reaches nanometer scale, Fermi
Electron energy level near energy level splits into discrete energy levels by continuous state.When energy level spacing is more than heat energy, magnetic energy, electrostatic energy, magnetostatic
Can, the cohesion energy of photon energy or superconducting state when, it may appear that the quantum effect of nano material so that its magnetic, light, sound, heat, electricity,
Superconduct performance change.The present invention is to make use of the optics of nano material.
Quantum dot (QDs) is a kind of zero-dimensional semiconductor nanocrystal, approximate ball-type, the nm of diameter 1 ~ 12, can be divided
Dissipate and form colloid in water or organic solvent.Swashing for even less than corresponding semiconductor body phase material is closely sized to due to quantum dot
Son (electronics-hole to) Bohr radiuses, be stimulated caused by electronics and hole be limited in narrow and small three dimensions,
Quantum limitation effect thus is shown, there is unique optical property.Quantum dot is generally by II-VI race or III-group Ⅴ element group
Into.It is quantized to cause emission spectrum discrete, dependent on quantum dot size with energy, can be accurate so as to obtain one kind
The emitter of fluorescence emission wavelengths is adjusted, so size and component by changing quantum dot, can accurately regulate and control quantum dot
Glow color and quantum dot luminous efficiency.At present, quantum dot be probably find since the dawn of human civilization it is classic luminous
Material, huge application potential is shown in medical biotechnology and photoelectric device etc..
The luminous efficiency and light, the approach of chemical stability for increasing quantum dot mainly have two kinds：First, quantum dot surface is modified
Organic ligand；2nd, quantum dot surface coated inorganic shell.Typically, organic ligand can not be passivated the electronics of quantum dot surface simultaneously
With hole trap state, and Yi Shoushui, oxygen attack and light degradation, it is impossible to quantum dot is kept long-term effectively luminous and stability.
In order to further enhance the reliability and stability of quantum dot light emitting, people have developed core/shell structure quantum dot, the present invention
CdZnS/CdSe/ZnS quantum dots belong to core/shell structure quantum dot, can use respectively with high warm injection method, alternately continuous ionic layer
Absorption Growth method and bi precursor method synthesis CdZnS/CdSe/ZnS quantum dots, wherein thering are four kinds of feasible schemes to synthesize again
This quantum dot.
The content of the invention
It is an object of the invention to provide a kind of preparation side of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots
Method, CdZnS/CdSe/ZnS quantum dots are using high warm injection method, alternately continuous ionic layer Absorption Growth method and bi precursor side
Prepared by method, the quantum dot of preparation has an obvious core shell structure, and the distribution of ZnS shells can be widened to several layers by 1 layer, each layer
The cladding of ZnS shells all can effectively eliminate monokaryon quantum dot surface anions and canons defect, reduce nonradiative transition, improve luminous
Performance；Prepared CdZnS/CdSe/ZnS quantum dots have that half-peak width i.e. monochromaticjty is good, the symmetrical i.e. monodispersity of PL spectrum
The features such as excellent luminance performance and continuously adjustabe wide spectrum for waiting well, and single CdZnS and CdSe amounts under identical size
Son point and CdZnS/CdSe quantum dots can not show the characteristic that is showed of CdZnS/CdSe/ZnS quantum dots after combination, after combination
CdZnS/CdSe/ZnS quantum dots have the optical characteristics abundanter than three above quantum dot.
The present invention is achieved like this, a kind of preparation side of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots
Method, it is characterised in that comprise the following steps：
（1）CdZnS quantum dots are synthesized by high warm injection method；
（2）Pass through（1）Obtained CdZnS quantum dots precipitation mixes with corresponding ligand solvent, by the way that zwitterion is directly added dropwise
It is incubated after mixed liquor to prepare CdZnS/CdSe；
（3）Pass through（2）Obtained CdZnS/CdSe quantum dots precipitation mixes with corresponding ligand solvent, can be by the way that negative and positive are directly added dropwise
Be incubated after the mixed liquor of ion and prepare CdZnS/CdSe/ZnS quantum dots, also can by first injection respectively, it is rear be added dropwise negative and positive from
It is incubated after son to prepare CdZnS/CdSe/ZnS quantum dots.
The step（1）In be that air is excluded by degassing method at 100 DEG C, and judge be incubated end be to pass through company
The whether constant method of continuous sampling contrast absorption spectrum.
The step（1）In be to add acetic anhydride zinc, cadmium oxide, oleic acid and 1-ODE octadecylenes simultaneously, at 305 DEG C
Inject S-ODE.
The step（2）In be that zwitterion is added dropwise simultaneously into main reaction, be incubated to the constant end of absorption spectrum.
The step（2）In used cadmium oleate can be prepared with two methods, and using being preceding heated to 60 DEG C.
The step（2）In be that air is excluded by degassing method at 80 DEG C, and heat up in an inert atmosphere.
The step（2）In Se powder elder generation ultrasonic dissolution used in tributyl phosphorus（TBP）In, then add appropriate 1-ODE ten
The cadmium oleate of the amount of eight alkene and grade material, and heating and thermal insulation.
The step（2）The CdZnS/CdSe quantum dots of middle preparation need to be purified to obtain CdZnS/CdSe powder, carry
Pure procedure includes：Gained CdZnS/CdSe quantum dots stoste extract repeatedly, then stoste centrifuges, and removes unnecessary Cd members
Element.Solution after centrifugation promotees precipitation with ethanol is added, then obtains CdZnS/CdSe powder by centrifugation, is finally dried in vacuo
30min。
The step（3）In have four kinds of schemes parcel shell ZnS, both can directly be added dropwise zwitterion mixed liquor and also can
To be incubated after first injection respectively, rear dropwise addition zwitterion to prepare CdZnS/CdSe/ZnS quantum dots.
The step（3）Middle CdZnS/CdSe powder is dissolved with appropriate toluene, and vacuumizes 50min at 120 DEG C.
The step（3）In be to start the mixed solution of the element containing Zn and Cd to be added dropwise with 2mL/h speed at 240 DEG C
Into main reaction, in 300 DEG C of insulations.
Embodiment
1st, the preparation method of CdZnS/CdSe/ZnS quantum dots：
（1）Synthesize CdZnS nuclear materials.Use cadmium oxide CdO and acetic anhydride zinc Zn (Ac)2As raw material, wherein anhydrous vinegar
Sour zinc Zn (Ac)2It is excessive.By 0.5mmolCdO and 5mmol Zn (Ac)2Add in 50ml there-necked flasks, then add 6ml oleic acid OA
With 10mL octadecylenes, air is excluded by blasting the min of inert gas 15 when temperature reaches 100 DEG C, then in inert gas ring
315 DEG C are heated under border, injects 1mmolS sources when temperature reaches 305 DEG C（High purity sulphur is dissolved in octadecylene）, candidate agent
After injection, a sample is taken at regular intervals, surveys absorption spectrum, when the absorption spectrum sampled twice in succession does not change,
Insulation terminates, and is cooled to 60 DEG C, that is, forms CdZnS nuclear materials, and stoste shows purple under ultraviolet light.
（2）The purification of CdZnS nuclear quantum dots.Appropriate n-hexane is added in stoste first, is then divided in centrifuge tube
It is interior, go to precipitate after centrifugation, in triplicate.Then according to stoste：N-hexane：Ethanol=1:0.8：2.5 ratio is divided in centrifuge tube
It is interior, remove supernatant after centrifugation, last gained precipitation is incubated in a vacuum（35℃）Dry 1h.
（3）CdZnS/CdSe preparation.0.3g is taken first（2）The CdZnS solid powders of middle gained, it is dilute molten with 4mL 18
Added after solution in 50mL there-necked flasks, then add 2ml oleyl amines（OAm）, it is heated to blasting inert gas 15min exclusions at 80 DEG C
Air, reaction temperature is then increased to 220 DEG C in an inert atmosphere.Following operating method can be divided into three kinds of schemes and say
State：Scheme one, taken at 220 DEG C appropriate（4）In the speed dripped with every 3-4 seconds one of mixed liquor be added drop-wise in reaction bulb, with
The passage in reaction time, along with being grown into for quantum dot, there is corresponding Red Shift Phenomena, reagent knot to be added dropwise in absorption spectrum
Shu Hou, a sample is taken at regular intervals, survey absorption spectrum, when the absorption spectrum sampled twice in succession does not change, protect
Temperature terminates, and is cooled to room temperature, carries out next step operation；Scheme two：Both wrapped up again on the basis of the insulation of scheme one terminates
CdSe, method is the same as scheme one.Scheme three：Wrap up CdSe again on the basis of scheme two, method is the same as scheme one.
（4）This step is to prepare the solution used in parcel CdSe shells.First, appropriate pure Se powder is taken, in tributylphosphine
Ultrasonic 5min in TBP, then add appropriate 1-ODE octadecylenes and the cadmium oleate with the amount of the material such as Se powder（Preparation method is shown in
（5））, appropriate heating, added when waiting main reaction to need.
（5）Prepare cadmium oleate.Cadmium oleate can be prepared with two schemes：Scheme one, 5mmol CdO cadmium oxides are taken to add
In 25mL there-necked flask, 5ml oleic acid and 5mL1-ODE octadecylenes are added, is heated to blasting inert gas 15min rows at 100 DEG C
Except air, reaction temperature is then increased to 230 DEG C in an inert atmosphere, waits solid to be cooled to room after all dissolving
Temperature.Scheme two, first 10mmol cadmium acetates and 40mmol oleic acid are mixed in 100ml there-necked flasks, air agitation is heated to obtaining
Stop heating after clear transparent solutions, be then cooled to 60 DEG C or so addition 70ml or so acetone, there is white precipitate, then with taking out
The method of filter is collected precipitation and eluted three times with acetone, is put into vacuum drying chamber and is dried overnight.
（6）Extraction centrifugation.The CdZnS/CdSe quantum dots of the gained of scheme one are carried out extraction centrifugation, the step is this hair
Bright unique distinction, because when preparing CdZnS/CdSe, cadmium ion has remnants, can be formed when adding sulphur in being operated below
CdS, cause solution first red shift blue shift again in encapsulation process, so as to which each side characteristic of quantum dot can be influenceed.Extraction is described below
Take the specific steps of centrifugation.Extraction：The stoste of scheme one is heated to 50 DEG C, then adds n-hexane and methanol（Volume ratio is 1:
2）Layering, removes lower clear liquid, so repeatedly 3-4 times.Centrifugation：The stoste centrifugation after extraction once, then according to stoste：Just oneself
Alkane：Ethanol=1:0.8:2.5 ratio is dispensed into centrifugal bottle, is centrifuged, and removes supernatant after the heart, and gained is precipitated into vacuum
Dry 30min.Note：（3）In scheme two and the resulting solution of scheme three it is identical with the processing method of scheme one.
（7）The preparation of CdZnS/CdSe/ZnS quantum dots.Dissolved first with appropriate toluene（6）Gained is heavy after middle centrifugation
Form sediment, and be transferred in 50mL there-necked flask, add oleyl amine and 1-ODE octadecylenes, 50min is vacuumized when being warming up to 120 DEG C, so
It is warming up to 300 DEG C in an inert atmosphere afterwards.When temperature reaches 240 DEG C, start the speed dropwise addition with 2mL/h（8）Middle system
Standby ZnS bi precursor mixed liquors, with the passage in reaction time, along with being grown into for quantum dot, there is phase in absorption spectrum
The blue-shifted phenomenon answered, wait being added dropwise after reagent terminates, a sample is taken at regular intervals, surveys absorption spectrum, when sampling twice in succession
Absorption spectrum when not changing, insulation terminates, and is cooled to 50 DEG C, finally according to（6）In extraction process 2-3 times,
Solution is preserved after extraction, carries out next step performance test and application.
（8）This step is to prepare the solution needed for parcel ZnS shells, and the method can be divided into four kinds of schemes：Scheme one, by oil
Sour zinc is dissolved in 1-ODE octadecylenes, adds 1- spicy thioalcohols, is made into certain concentration（The material such as zinc oleate and 1- spicy thioalcohols
Amount）, it is incubated after being heated to certain temperature, is added drop-wise to when waiting main reaction to need with 2mL/h speed in main reaction；Scheme two,
Weigh appropriate acetic anhydride zinc to be dissolved in oleic acid and 1-ODE octadecylenes, add n- dodecyl mereaptan, be made into certain concentration
（The amount of the material such as acetic anhydride zinc and n- dodecyl mereaptan）, it is incubated after being heated to certain temperature, with 2mL/h when main reaction needs
Speed be added drop-wise in main reaction；Scheme three, solution one is prepared first, high purity sulphur is dissolved in 1-ODE and is made into finite concentration
（Heating stirring 50min）, solution two is then prepared, is dissolved in oleic acid and 1-ODE octadecylenes and is made into necessarily with acetic anhydride zinc
Concentration, finally treat（7）Needed for middle main reaction arrival during temperature, a certain amount of solution one is first taken to inject in main reaction, after 15min
Start that solution two is added dropwise into main reaction with 2mL/h speed（The amount of the material such as acetic anhydride zinc and high purity sulphur）；Scheme four, it is first
Solution one is first prepared, a certain amount of high purity sulphur is dissolved in a small amount of TBP, 1-ODE octadecylenes is added to 2mL, then prepares
Solution two, acetic anhydride zinc is dissolved in oleic acid and 1-ODE and is made into certain concentration, is finally existed（7）In main reaction reach
During required temperature, first take a certain amount of solution one to inject in main reaction, start that solution two is added dropwise with 2mL/h speed after 15min
Into main reaction（The amount of the material such as acetic anhydride zinc and high purity sulphur）.
Claims (9)
1. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots, it is characterised in that including following step
Suddenly：
（1）CdZnS quantum dots are synthesized by high warm injection method；
（2）Pass through（1）Obtained CdZnS quantum dots precipitation mixes with corresponding ligand solvent, by the way that zwitterion is directly added dropwise
It is incubated after mixed liquor to prepare CdZnS/CdSe；
（3）Pass through（2）Obtained CdZnS/CdSe quantum dots precipitation mixes with corresponding ligand solvent, can be by the way that negative and positive are directly added dropwise
Be incubated after the mixed liquor of ion and prepare CdZnS/CdSe/ZnS quantum dots, also can by first injection respectively, it is rear be added dropwise negative and positive from
It is incubated after son to prepare CdZnS/CdSe/ZnS quantum dots.
2. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（1）In be to add acetic anhydride zinc, cadmium oxide, oleic acid and 1-ODE octadecylenes simultaneously, at 305 DEG C
Inject S-ODE.
3. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（2）In be that zwitterion is added dropwise simultaneously into main reaction, be incubated to the constant end of absorption spectrum.
4. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（2）In used cadmium oleate can be prepared with two methods, and using being preceding heated to 60 DEG C.
5. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（2）In Se powder elder generation ultrasonic dissolution used in tributyl phosphorus（TBP）In, then add appropriate 1-ODE ten
The cadmium oleate of the amount of eight alkene and grade material, and heating and thermal insulation.
6. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（2）The CdZnS/CdSe quantum dots of middle preparation need to be purified to obtain CdZnS/CdSe powder, carry
Pure procedure includes：Gained CdZnS/CdSe quantum dots stoste extract repeatedly, then stoste centrifuges, and removes unnecessary Cd members
Element；Solution after centrifugation promotees precipitation with ethanol is added, then obtains CdZnS/CdSe powder by centrifugation, is finally dried in vacuo
30min。
7. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（3）In have four kinds of schemes parcel shell ZnS, both can directly be added dropwise zwitterion mixed liquor or
Can first inject respectively, zwitterion is added dropwise afterwards after insulation prepare CdZnS/CdSe/ZnS quantum dots.
8. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（3）Middle CdZnS/CdSe powder is dissolved with appropriate toluene, and vacuumizes 50min at 120 DEG C.
9. a kind of preparation method of more shell mould CdZnS/CdSe/ZnS core/shell structure quantum dots according to claim 1, its
It is characterised by, the step（3）In be to start the mixed solution of the element containing Zn and Cd to be dripped with 2mL/h speed at 240 DEG C
It is added in main reaction, in 300 DEG C of insulations.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110028970A (en) * | 2019-04-28 | 2019-07-19 | 南昌航空大学 | CdZnSe/CdSe/ZnSe green light quantum point preparation method |
| WO2020078072A1 (en) * | 2018-10-18 | 2020-04-23 | 纳晶科技股份有限公司 | Core-shell quantum dot preparation method, core-shell quantum dot and electroluminescent device containing core-shell quantum dot |
| WO2021136002A1 (en) * | 2019-12-31 | 2021-07-08 | Tcl科技集团股份有限公司 | Quantum dot, preparation method thereof and quantum dot light-emitting diode |
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| CN101824317A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | CdxZn1-xS/ZnS ternary core-shell quantum dot and method for preparing same |
| CN103184045A (en) * | 2013-05-08 | 2013-07-03 | 河南大学 | Preparation method of semiconductor nanocrystals with II type core-shell structures |
| CN106566553A (en) * | 2016-10-20 | 2017-04-19 | 深圳天吉新创科技有限公司 | Methods for synthesizing ZnxCd1-xSe, ZnxCd1-xSe/ZnS and ZnxCd1-xSe/ZnS/ZnS alloy quantum dots |
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| CN101824317A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | CdxZn1-xS/ZnS ternary core-shell quantum dot and method for preparing same |
| CN103184045A (en) * | 2013-05-08 | 2013-07-03 | 河南大学 | Preparation method of semiconductor nanocrystals with II type core-shell structures |
| CN106566553A (en) * | 2016-10-20 | 2017-04-19 | 深圳天吉新创科技有限公司 | Methods for synthesizing ZnxCd1-xSe, ZnxCd1-xSe/ZnS and ZnxCd1-xSe/ZnS/ZnS alloy quantum dots |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020078072A1 (en) * | 2018-10-18 | 2020-04-23 | 纳晶科技股份有限公司 | Core-shell quantum dot preparation method, core-shell quantum dot and electroluminescent device containing core-shell quantum dot |
| CN110028970A (en) * | 2019-04-28 | 2019-07-19 | 南昌航空大学 | CdZnSe/CdSe/ZnSe green light quantum point preparation method |
| CN110028970B (en) * | 2019-04-28 | 2022-04-12 | 南昌航空大学 | Preparation method of CdZnSe/CdSe/ZnSe green light quantum dots |
| WO2021136002A1 (en) * | 2019-12-31 | 2021-07-08 | Tcl科技集团股份有限公司 | Quantum dot, preparation method thereof and quantum dot light-emitting diode |
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Application publication date: 20180112 |