CN110423616A - Core-shell quanta dots preparation method, quantum dot optoelectronic devices - Google Patents
Core-shell quanta dots preparation method, quantum dot optoelectronic devices Download PDFInfo
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 230000005693 optoelectronics Effects 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 239000003446 ligand Substances 0.000 claims abstract description 20
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- 239000002904 solvent Substances 0.000 claims description 6
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- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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Abstract
The invention discloses core-shell quanta dots preparation method and quantum dot optoelectronic devices.Wherein, core-shell quanta dots preparation method, comprising the following steps: provide the first quantum dot, the second quantum dot, ligand and the first solution comprising fatty amine, wherein average grain diameter of the average grain diameter of the second quantum dot less than the first quantum dot；It mixes the first quantum dot, the second quantum dot, ligand and the first solution and forms reaction system, in the reaction system, the second quantum dot gradually dissolves, and the lysate of the second quantum dot forms shell in the first quantum dot outgrowth, so that core-shell quanta dots be made.The synthesis step of core-shell quanta dots of the present invention is simple, and the reaction time is short, reproducible, is conducive to that core-shell quanta dots are mass produced, while being also beneficial to obtain the good core-shell quanta dots of monodispersity.
Description
Technical field
The present invention relates to quanta point material technical field more particularly to core-shell quanta dots preparation methods, quantum dot light electric appliance
Part.
Background technique
In nano material, solution semiconductor of the size within the scope of quantum confinement nanocrystalline (solution quantum dot) is excellent with its
Different optical property, such as fluorescence quantum yield height, Absorber Bandwidth, emission peak is narrow, optical stability is good, causes scientific circles and work
The extensive concern of industry.In the fields such as biomarker and imaging, light emitting diode, laser, quantum dot photovoltaic device, quantum dot is ground
Study carefully one of the hot spot for having become respective field.People's daily life is influenced in display (quantum dot backlight TV), illumination etc.
Field, practical application has been obtained in quantum dot.Especially in display field, compared to organic fluorescence materials and inorganic fluorescent
Powder, quantum dot can more truly restore image color, realize full gamut covering, and then promote the texture and solid of picture
Sense.
As it is a kind of it is emerging shine and photoelectric material, the synthesis chemistry of solution quantum dot be so far its develop it is decisive because
Element.For the nuclear quantum dot of one-component, core-shell quanta dots have higher optics and chemical stability.Prepare nucleocapsid
When quantum dot, especially in shell growth course, it is crucial to need to solve the problems, such as two, first is that being avoided as much as shell precursor
Spontaneous nucleation, the other is guarantee shell precursor uniformly grown in nuclear quantum dot.
2003, researcher in this field proposed alternating ion layer adsorption growth method (SILAR) in CdSe quantum dot
The controllable CdS shell of upper growth thickness, namely: the concentration of CdSe quantum dot is measured first, is obtained needed for coating each layer of CdS
The amount of anion presoma, cationic presoma, and anion presoma, cationic presoma are alternately added, forerunner's physical efficiency
It is enough particularly well adsorbed in the surface of quantum dot, to be conducive to inhibit the spontaneous nucleation of anion presoma and cationic presoma existing
As.After SILAR method, core-shell quanta dots morphology and size is distributed all relatively good, fluorescence half-peak width.But SILAR method is only
Suitable for the cladding of thin layer core-shell quanta dots, with the increase of shell, the amount of presoma required for each layer will be corresponding
Increase, in this way during cladding, anion presoma and cationic presoma are easy spontaneous nucleation.In addition, precursor concentration
Increase can change the pattern of quantum dot, the pattern of core-shell quanta dots can be to aspherical transformation.Then, researcher in this field
Thermal cycle alternating ion layer adsorption growth method (TC-SILAR) is further developed in 2007, i.e. low temperature injects presoma, drop
The reactivity of low presoma, makes it well, uniformly be adsorbed on the surface of quantum dot, then increases temperature and is reacted.
In this way, with the increase of shell thickness, core-shell structure still keeps spherical morphology.In addition, 2013, another group is ground
Study carefully a kind of method for synthesizing core-shell quanta dots of employee development, i.e., at 300 DEG C, using cadmium oleate and spicy thioalcohol as being formed
The presoma of CdS shell has synthesized the very narrow CdSe/CdS core-shell structure of transmitting half-peak breadth, and it is glimmering that fluorescence half-peak breadth is in individual particle
Most narrow to have reached 65.3meV in the range of light, fluorescence quantum yield is close to 100%.
But the synthetic method of the various core-shell quanta dots developed at present is long there are the reaction time, reaction process is cumbersome, at
This height, the disadvantages of energy consumption is high, are unfavorable for the large-scale production of core-shell quanta dots.Formed stratum nucleare needed for presoma dosage with
The increase of shell thickness is increasing, in shell synthesis process, with being continuously added for presoma, is easy to appear spontaneous nucleation,
So that phenomena such as scale topography monodisperse of quantum dot is deteriorated, and fluorescence half-peak breadth narrows, and be difficult to carry out some complicated knots
The synthesis of structure or special construction quantum dot.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of core-shell quanta dots preparation method, solutions
The certainly self-contained nuclear phenomenon in shell growth course obtains the good core-shell quanta dots of monodispersity.
According to an aspect of the present invention, a kind of core-shell quanta dots preparation method is provided, comprising the following steps:
There is provided the first quantum dot, the second quantum dot, ligand and the first solution comprising fatty amine, wherein above-mentioned second
The average grain diameter of quantum dot is less than the average grain diameter of above-mentioned first quantum dot；
It mixes above-mentioned first quantum dot, above-mentioned second quantum dot, above-mentioned ligand and above-mentioned first solution and forms reactant
System, in above-mentioned reaction system, above-mentioned second quantum dot gradually dissolves, and the lysate of above-mentioned second quantum dot is above-mentioned first
Quantum dot outgrowth forms shell, so that core-shell quanta dots be made.
Above-mentioned first quantum dot is nuclear quantum dot or core-shell quanta dots, above-mentioned second quantum in one of the embodiments,
Point is nuclear quantum dot or core-shell quanta dots.
Above-mentioned ligand is trialkyl phosphine in one of the embodiments, it is preferable that above-mentioned trialkyl phosphine is selected from following one kind
It is or a variety of: tributylphosphine, tri octyl phosphine.
The volume fraction of the above-mentioned fatty amine in above-mentioned first solution is 25%~100% in one of the embodiments,.
Above-mentioned fatty amine is the saturation or unsaturation primary amine of carbon chain lengths 8~22 in one of the embodiments,.
The difference of the partial size of the partial size of above-mentioned first quantum dot and above-mentioned second quantum dot is not small in one of the embodiments,
In 2nm, it is preferable that the partial size of above-mentioned first quantum dot is 3nm~10nm, and the partial size of above-mentioned second quantum dot is 1nm~5nm.
In one of the embodiments, in above-mentioned reaction system, the concentration of initial above-mentioned first quantum dot is greater than initial
Above-mentioned second quantum dot concentration.
Before being mixed in one of the embodiments, with above-mentioned first solution, above-mentioned first quantum dot and above-mentioned second quantum
Point mixing is scattered in solvent formation quantum dot mixed solution, in above-mentioned quantum dot mixed solution, above-mentioned first quantum dot it is dense
Degree is greater than the concentration of above-mentioned second quantum dot, mixes above-mentioned quantum dot mixed liquor, above-mentioned ligand and above-mentioned first solution and is formed
Above-mentioned reaction system.
The temperature of above-mentioned reaction system is set to be maintained at 200 DEG C~310 DEG C in one of the embodiments, reaction 5min~
30min。
According to another aspect of the present invention, a kind of quantum dot optoelectronic devices, including preceding method of the present invention preparation are provided
Obtained core-shell quanta dots.
Compared with prior art, the beneficial effects of the present invention are: the synthesis step of core-shell quanta dots of the present invention is simple, reaction
Time is short, reproducible, is conducive to that core-shell quanta dots are mass produced；Core-shell quanta dots preparation method of the invention solves shell
Self-contained nuclear phenomenon in layer growth course, help to obtain the good core-shell quanta dots of monodispersity, therefore core-shell quanta dots is glimmering
Light half-peak breadth is relatively narrow；Core-shell quanta dots preparation method of the invention can obtain the high core-shell quanta dots of fluorescence quantum yield；
In addition, core-shell quanta dots preparation method of the invention has good universality, it can be used for the conjunction of different type core-shell quanta dots
At, can be used for synthesis labyrinth core-shell quanta dots.
Detailed description of the invention
Fig. 1 illustrates the electron microscope of CdS, CdSe and CdSe/CdS quantum dot in embodiments herein 1.
Specific embodiment
In the following, being described further in conjunction with specific embodiment to the present invention, it should be noted that is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
It should be noted that the term " first ", " second " etc. in the description and claims of this application are to be used for
Similar object is distinguished, without being used to describe a particular order or precedence order.In addition, term " includes " and " having " and
Their any deformation, it is intended that cover it is non-exclusive include, for example, containing the process of a series of steps or units, side
Method, system, product or equipment those of are not necessarily limited to be clearly listed step or unit, but may include being not clearly listed
Or other step or units intrinsic for these process, methods, product or equipment.
The present invention provides a kind of core-shell quanta dots preparation method, comprising the following steps:
There is provided the first quantum dot, the second quantum dot, ligand and the first solution comprising fatty amine, wherein the second quantum
Average grain diameter of the average grain diameter of point less than the first quantum dot；
It mixes the first quantum dot, the second quantum dot, ligand and the first solution and forms reaction system, in the reaction system,
Second quantum dot gradually dissolves, and the lysate of the second quantum dot forms shell in the first quantum dot outgrowth, so that core be made
Shell quantum dot.
In above-mentioned technical proposal, the first quantum dot is the quantum dot of shell to be covered, and the second quantum dot is for providing shell
Material needed for growth.In the prior art, when growing shell, cationic forerunner is added usually into the solution comprising quantum dot
Body and anion presoma, during shell coating reaction, cationic presoma and anion presoma are easy spontaneous nucleation, this
And lead to the reason of core-shell quanta dots monodispersity difference made from the prior art.And in the present invention, for growing the material of shell
Material is initially formed lesser second quantum dot of size, then by lesser second quantum dot of size and larger-size first quantum dot
It is mixed in solution, under certain conditions, the second quantum dot dissolves in the solution, and the product of dissolution can be in the first amount
Son point outgrowth forms shell, and core-shell quanta dots monodispersity obtained is good, fluorescence half-peak width.
The principle class for principle and Ostwald ripening phenomenon the small size particles dissolution that second quantum dot dissolves in the solution
Seemingly.Ostwald curing refers to lesser crystallization or grain dissolution in solute and is deposited in relatively large crystallization or particle again.
The present invention artificially provides the second quantum dot and large-sized first quantum dot of small size in the solution, when meeting certain condition
When, the second quantum dot of solution small-medium size is dissolved and is deposited on large-sized first quantum dot, is equivalent in the first quantum
Shell in point outer cladding.
Fatty amine in above-mentioned reaction system can effectively dissolve the second quantum dot of small size, and etch large-sized
One quantum dot is conducive to accelerate to cure between curing and particle in particle.In addition, fatty amine is also used as stablizing matching for quantum dot
Body helps to improve the fluorescence quantum yield of core-shell quanta dots.
Ligand in above-mentioned reaction system primarily serves the effect of stable quantum dot, and the addition of ligand is conducive to improve nucleocapsid
The fluorescence quantum yield of quantum dot.
Quantum dot of first quantum dot as shell to be covered, can be nuclear quantum dot and is also possible to core-shell quanta dots.When
When first quantum dot is nuclear quantum dot, it can be the quantum dot of one-component, be also possible to alloy quantum dot.When the first quantum
When point is core-shell quanta dots, shell can be one layer and be also possible to multilayer.First quantum dot can be a kind of quantum dot, can also
To include a variety of quantum dots.
Second quantum dot can be nuclear quantum dot and be also possible to nucleocapsid quantum as the quantum dot of shell growth material is provided
Point.When the second quantum dot is nuclear quantum dot, it can be the quantum dot of one-component, be also possible to alloy quantum dot.When
When two quantum dots are core-shell quanta dots, shell can be one layer and be also possible to multilayer, in addition, in the reaction system, the second amount
The shell in son point outside is first dissolved, and the Shell Materials of dissolution are first coated on outside the first quantum dot, and the core in the second quantum dot is most
After be dissolved, the nuclear material of dissolution is finally coated on outside the first quantum dot.Second quantum dot can be a kind of quantum dot, can also be with
Including a variety of quantum dots.It is noted that the quantum dot of one-component described in the present invention refer to including it is a kind of cation and
A kind of quantum dot of anion.
First quantum dot can be the same or different with the second quantum dot, when the first quantum dot is identical as the second quantum dot
When, also that is, the growth of homostyructure.
Core-shell quanta dots preparation method provided by the invention is suitable for the synthesis of a variety of different core-shell quanta dots.In a reality
It applies in example, the first quantum dot is CdSe, and the second quantum dot is that CdS can be made using aforementioned core-shell quanta dots preparation method
CdSe/CdS core-shell quanta dots.In another embodiment, the first quantum dot is CdSe, and the second quantum dot is ZnSe, before
Core-shell quanta dots preparation method is stated, CdSe/ZnSe core-shell quanta dots can be made.In another embodiment, the first quantum dot
For InP, InP/ZnSe core-shell quanta dots can be made using aforementioned core-shell quanta dots preparation method for ZnSe in the second quantum dot.
In a further embodiment, the first quantum dot is ZnSe, and the second quantum dot is ZnS, using aforementioned core-shell quanta dots preparation method,
ZnSe/ZnS core-shell quanta dots can be made.Above first quantum dot, the second quantum dot are not exhausted enumerate.
In some embodiments, ligand is trialkyl phosphine, and trialkyl phosphine is conducive to improve core-shell quanta dots as ligand
Fluorescence quantum yield.Trialkyl phosphine can be selected from one or more of: tributylphosphine, tri octyl phosphine.
In some embodiments, the volume fraction of the fatty amine in the first solution is 25%~100%.First solution can be with
All fatty amines, the first solution also may include fatty amine and non-coordinating solvent (such as octadecylene).Preferably, fatty amine is carbon
The saturation of chain length 8~22 or unsaturated primary amine.
In some embodiments, the difference of the partial size of the partial size of the first quantum dot and the second quantum dot is not less than 2nm.Wherein,
The particle size range of first quantum dot is preferably in 3nm~10nm, and the particle size range of the second quantum dot is preferably in 1nm~5nm.
After first quantum dot and the second quantum dot are respectively synthesized and purify, can mix according to a certain percentage be dispersed in it is molten
It in agent, can also respectively disperse in a solvent, distinguish feeding according still further to certain ratio when use.By adjusting reactant
The ratio of first quantum dot and the second quantum dot in system, fluorescence peak position and the shell that can control final core-shell quanta dots are thick
Degree.
In some embodiments, before mixing with the first solution, the first quantum dot, the second quantum dot are dispersed in solvent respectively
In, to obtain the first quantum dot solution and the second quantum dot solution, the first quantum dot solution and the second quantum dot solution it is molten
Agent is identical or different.In subsequent step, the first quantum dot solution, the second quantum dot solution, ligand and the first solution are mixed into shape
At reaction system, it is preferable that the concentration of the first initial quantum dot is greater than the concentration of the second initial quantum dot in reaction system.
In further embodiments, before being mixed with the first solution, the first quantum dot and the second quantum dot mixing be dispersed in it is molten
Quantum dot mixed solution is formed in agent, the first quantum dot and the second quantum dot can relatively steadily in quantum dot mixed solution
It coexists.Preferably, in quantum dot mixed solution, the concentration of the first quantum dot is greater than
The concentration of second quantum dot.In these embodiments, ligand, which can first be added in quantum dot mixed solution, forms
Two solution, then the second solution is mixed to form reaction system with the first solution again, can also successively be added into the first solution
Ligand and quantum dot mixed solution form reaction system.
There are sizes to be distributed focusing phenomenon in the growth course of quantum dot, during the reaction, the size point of quantum dot
Cloth first reduces to a certain extent, then with the progress in reaction time, occurs Ostwald curing, particle size distribution become from
There are a critical dimensions in the scattered namely growth course of quantum dot, when quantum dot size is less than critical dimension, small size amount
Son puts the fast of growth, and large-size quantum dots are grown slow, so that size distribution gradually becomes smaller, when quantum dot size is greater than critical ruler
After very little, particle takes place ripening phenomenon, and this process be it is concentration dependent with reacting precursor, when quantum dot start it is ripe
When change, reacting precursor is added, size distribution focusing phenomenon can occur again again.In addition, during Quantum Dots Growth, there is also rulers
Very little Self-focusing, in the higher situation of quantum dot concentration, the dissolution of small size quantum dot generates monomer, so that large scale quantum
Point growth, when the concentration of quantum dot becomes smaller to a certain extent, classical Ostwald ripening phenomenon occurs, quantum dot size point
Cloth starts to broaden.
Based on the above analysis, in the reaction system, when reacting just beginning, the second quantum dot is not completely dissolved also, in solution
The difference of the sub- spot size of two amounts be gradually expanded with reaction, and the size distribution of quantum dot is larger, with holding for reaction
Continuous to carry out, most of second quantum dot is dissolved, and the size distribution of quantum dot is smaller in solution at this time, if continued anti-
It answers, then the core-shell quanta dots in solution are easy curing, cause quantum dot size distribution to broaden again, so that core-shell quanta dots
Fluorescence quantum yield reduce, half-peak breadth becomes larger, and therefore, it is necessary to control the reaction time in reasonable range.Preferably, make anti-
It answers the temperature of system to be maintained at 200 DEG C~310 DEG C, reacts 5min~30min, core-shell quanta dots are made.
In some embodiments, core-shell quanta dots preparation method of the invention is further comprising the steps of:
Fatty amine is mixed with solvent, 200 DEG C~310 DEG C is maintained the temperature at, obtains the first solution；
Be respectively synthesized the first quantum dot and the second quantum dot, the first quantum dot is mixed with the second quantum dot be dispersed in it is molten
Quantum dot mixed solution is formed in agent, ligand is then added into quantum dot mixed solution, and maintain the temperature at 200 DEG C~310
DEG C, obtain the second solution；
It mixes the first solution and the second solution and forms reaction system, maintain the temperature at 200 DEG C~310 DEG C, reaction 5min~
30min obtains core-shell quanta dots in the solution after reaction.
The another aspect of the application additionally provides a kind of quantum dot optoelectronic devices, before quantum dot optoelectronic devices include of the invention
State the core-shell quanta dots of method preparation.Photoelectric device can be quantum dot light conversion film, quantum stippling film and its make with LED junction conjunction
Device, light emitting diode with quantum dots etc..In the present invention, the material for growing shell is initially formed lesser second amount of size
It is sub-, then lesser second quantum dot of size is mixed in solution with larger-size first quantum dot, in certain item
Under part, the second quantum dot dissolves in the solution, and the product of dissolution can form shell in the first quantum dot outgrowth, is made
Core-shell quanta dots monodispersity is good, fluorescence half-peak width.The thus photoelectricity of the core-shell quanta dots as made from aforementioned preparation process
Device luminous efficiency with higher.
Precursors preparation:
The preparation of 0.1mmol/mL selenium powder suspension: selenium powder (0.0237g, 0.3mmol) is distributed in the ODE of 3mL, is surpassed
It is configured to 0.1mmol/mL suspension within sound 5 minutes.The preparation of the selenium powder suspension of other concentration is similar, need to only change selenium powder
Amount.It is shaken up before use.
The preparation of 0.1mmol/mL S-ODE solution: sulphur powder (0.032g, 1mmol) is distributed in the ODE of 10mL, ultrasound
Concussion dissolution.The preparation of the S-ODE solution of other concentration is similar, need to only change the amount of sulphur powder.
[embodiment 1]
Synthesize the first quantum dot (CdSe quantum dot of average grain diameter 6nm): by CdO (0.1280g, 1mmol), tetradecylic acid
(0.5g, 2.2mmol) and ODE (4mL) are put into the three-necked bottle of 25mL, and stirring ventilation after ten minutes, is warming up to 280 DEG C, obtains
Clear solution, temperature control is at 250 DEG C；The selenium powder suspension that 1mL concentration is 0.05mmol/mL is rapidly injected in three-necked bottle, it will
Reaction temperature is controlled at 250 DEG C, and 0.1mL concentration is added after ten minutes, with the speed of 0.9mL/h as the selenium of 0.1mmol/mL in reaction
Powder suspension, after dripping off selenium powder suspension, the reaction was continued 5 minutes, 1.5mmol oleic acid then is added with the speed of 12mL/h, instead
Should 0.1mL concentration be added as the selenium powder suspension of 0.1mmol/mL with the speed of 0.9mL/h, then react 10 points after five minutes
The above-mentioned selenium powder suspension of 0.1mL is added again, circuits sequentially for clock, and until obtaining target size quantum dot, purification is dissolved in a small amount of
In ODE, the first quantum dot solution is formed.
Synthesize the second quantum dot (CdS quantum dot of average grain diameter 3nm): by CdO (0.0256g, 0.2mmol), oleic acid
(0.282g, 1mmol) and ODE (4mL) are put into 25mL three-necked bottle, and stirring ventilation after ten minutes, is warming up to 280 DEG C, obtains clear
The S-ODE solution that 1mL concentration is 0.1mmol/mL is rapidly injected in three-necked bottle, will react at 250 DEG C by clear solution, temperature control
Temperature is controlled at 250 DEG C, is reacted 15 minutes, and reaction is stopped, and purification is dissolved in a small amount of ODE, forms the second quantum dot solution.
The synthesis of CdSe/CdS core-shell quanta dots:
(1) by aforementioned first quantum dot solution and the second quantum dot solution of a quarter be mixed to get quantum dot mix it is molten
Liquid；
(2) ODE of 3mL is put into 25mL three-neck flask with the oleyl amine of 2mL and is mixed, stirring ventilation after ten minutes, increases
Temperature injects the tributylphosphine (TBP) of 0.1mL to 250 DEG C, is then rapidly injected the quantum dot mixed solution of step (1), reaction
20min stops reaction.
[embodiment 2]
The synthesis of first quantum dot InP quantum dot: 0.15mmol (0.043g) indium acetate, 0.45mmol are weighed
(0.1036g) tetradecylic acid, 10mL ODE are put into 50mL three-neck flask, are warming up to 180 DEG C and are vented 30 minutes, then reduce temperature
To room temperature, inject 0.1mmol (TMS)3Then the mixed solution of P and 1mL TOP increases temperature to 260 DEG C, reacts 5 minutes, mention
It is pure, it is dissolved in 1mL ODE.
Synthesis small size ZnSe quantum dot: weighing 0.1mmol zinc stearate, in 5mLODE and 25mL three-neck flask, increases
Temperature injects 1mL0.05mmol/mLSe-ODE suspension to 280 DEG C, reacts 5min, stops reaction, and purification is dissolved in 1mL ODE
In.
The synthesis of InP/ZnSe core-shell quanta dots:
(1) by aforementioned first quantum dot solution and the second quantum dot solution of a quarter be mixed to get quantum dot mix it is molten
Liquid；
(2) ODE of 3mL is put into 25mL three-neck flask with the oleyl amine of 2mL and is mixed, stirring ventilation after ten minutes, increases
Temperature injects the tributylphosphine (TBP) of 0.1mL to 250 DEG C, is then rapidly injected the quantum dot mixed solution of step (1), reaction
20min stops reaction.
[embodiment 3]
First quantum dot: the red light emission wavelength 620nm CdSe/CdZnS nucleocapsid of NNCrystal Technology Co., Ltd.'s production
Quantum dot.
Synthesis small size ZnS quantum dot: weighing 0.1mmol zinc stearate, in 5mL ODE and 25mL three-neck flask, raising
Temperature injects 1mL 0.05mmol/mL S-ODE solution to 280 DEG C, reacts 5min, stops reaction, and purification is dissolved in 1mL ODE
In.
The synthesis of CdSe/CdZnS/ZnS core-shell quanta dots:
(1) by aforementioned first quantum dot solution and the second quantum dot solution of a quarter be mixed to get quantum dot mix it is molten
Liquid；
(2) ODE of 3mL is put into 25mL three-neck flask with the oleyl amine of 2mL and is mixed, stirring ventilation after ten minutes, increases
Temperature injects the tributylphosphine (TBP) of 0.1mL to 250 DEG C, is then rapidly injected the quantum dot mixed solution of step (1), reaction
20min stops reaction.
[embodiment 4]
With the difference of embodiment 1 are as follows: the oleyl amine of 5mL is put into 25mL three-neck flask by step (2), is not needed mixed with ODE
It closes.
[embodiment 5]
With the difference of embodiment 1 are as follows: eight amine of the ODE of 3mL and 2mL are put into 25mL three-neck flask in step (2) and are mixed
It closes.
[embodiment 6]
With the difference of embodiment 1 are as follows: it is rapidly injected the quantum dot mixed solution of step (1) in step (2), reacts 5min,
Stop reaction.
[embodiment 7]
With the difference of embodiment 1 are as follows: it is rapidly injected the quantum dot mixed solution of step (1) in step (2), reacts 30min,
Stop reaction.
[comparative example 1]
The CdSe quantum dot of average grain diameter 3nm: by CdO (0.0256g, 0.1mmol), stearic acid (0.142g, 0.5mmol)
It is put into the three-necked bottle of 25mL with ODE (4mL), stirring ventilation after ten minutes, is warming up to 280 DEG C, obtains clear solution, temperature control exists
250℃；The selenium powder suspension that 1mL concentration is 0.1mmol/mL is rapidly injected in three-necked bottle, reaction temperature is controlled 250
DEG C, reaction after ten minutes, every 5 minutes, injects the selenium powder suspension that 0.1mL concentration is 0.1mmol/mL, until obtaining target
Dimensional quantum point, purification are dissolved in a small amount of ODE.
The synthesis of CdSe/CdS core-shell quanta dots: by CdO (0.064g, 0.5mmol), oleic acid (1.5mmol) and ODE
(4mL) is put into the three-necked bottle of 25mL, and stirring ventilation after ten minutes, is warming up to 280 DEG C, obtains clear solution, temperature control is 250
℃.It is subsequently injected into a quarter CdSe core, every 10 minutes, it was 0.1mmol/mL that 0.1mL concentration, which is added, with the speed of 0.9mL/h
S-ODE liquid stops reaction until obtaining target size quantum dot (PL is in 620nm).
Using fluorescence emission spectrometer test the core-shell quanta dots of the various embodiments described above and comparative example fluorescence emission peak,
Half-peak breadth and quantum efficiency.Test the quantum efficiency of the core-shell quanta dots of the various embodiments described above and comparative example, quantum efficiency
Detection method are as follows: using 450nm blue LED lamp as light source, test the spectrum and thoroughly of blue-light source respectively using integrating sphere
Spectrum after crossing quantum dot solution calculates quantum dot luminous efficiency, quantum efficiency=(quantum dot hair using the integral area of spectrogram
Penetrate peak area)/(blue-light source peak area-penetrates unabsorbed blue peak area after quantum dot solution) * 100%.Test knot
Fruit is shown in Table 1.
Table 1
| Fluorescence emission peak/nm | Half-peak breadth/nm | Quantum efficiency/% | |
| Embodiment 1 | 650 | 21 | 95 |
| Embodiment 2 | 545 | 42 | 57 |
| Embodiment 3 | 625 | 23 | 95 |
| Embodiment 4 | 651 | 22 | 96 |
| Embodiment 5 | 651 | 23 | 92 |
| Embodiment 6 | 645 | 21 | 95 |
| Embodiment 7 | 653 | 23 | 93 |
| Comparative example 1 | 620 | 28 | 91 |
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of core-shell quanta dots preparation method, which comprises the following steps:
There is provided the first quantum dot, the second quantum dot, ligand and the first solution comprising fatty amine, wherein second quantum
The average grain diameter of point is less than the average grain diameter of first quantum dot；
It mixes first quantum dot, second quantum dot, the ligand and first solution and forms reaction system, In
In the reaction system, second quantum dot gradually dissolves, and the lysate of second quantum dot is in first quantum
Point outgrowth forms shell, so that core-shell quanta dots be made.
2. core-shell quanta dots preparation method according to claim 1, which is characterized in that first quantum dot is core quantum
Point or core-shell quanta dots, second quantum dot are nuclear quantum dot or core-shell quanta dots.
3. core-shell quanta dots preparation method according to claim 1, which is characterized in that the ligand is trialkyl phosphine, excellent
Selection of land, the trialkyl phosphine are selected from one or more of: tributylphosphine, tri octyl phosphine.
4. core-shell quanta dots preparation method according to claim 1, which is characterized in that the rouge in first solution
The volume fraction of fat amine is 25%~100%.
5. core-shell quanta dots preparation method according to claim 1, which is characterized in that the fatty amine is carbon chain lengths 8
~22 saturation or unsaturated primary amine.
6. core-shell quanta dots preparation method according to claim 1, which is characterized in that the partial size of first quantum dot with
The difference of the partial size of second quantum dot is not less than 2nm, it is preferable that the partial size of first quantum dot is 3nm~10nm, described
The partial size of second quantum dot is 1nm~5nm.
7. core-shell quanta dots preparation method according to claim 1, which is characterized in that in the reaction system, initial
The concentration of first quantum dot is greater than the concentration of initial second quantum dot.
8. core-shell quanta dots preparation method according to claim 1, which is characterized in that before being mixed with first solution,
First quantum dot is mixed with second quantum dot is scattered in formation quantum dot mixed solution in solvent, and the quantum dot is mixed
It closes in solution, the concentration of first quantum dot is greater than the concentration of second quantum dot, mixes the quantum dot mixed liquor, institute
It states ligand and first solution forms the reaction system.
9. -8 any core-shell quanta dots preparation method according to claim 1, which is characterized in that make the reaction system
Temperature is maintained at 200 DEG C~310 DEG C, reacts 5min~30min.
10. a kind of quantum dot optoelectronic devices, which is characterized in that including the core-shell quanta dots system as described in claim 1-9 is any
Quantum dot made from Preparation Method.
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