CN109971466A - A kind of quantum dot and preparation method thereof - Google Patents
A kind of quantum dot and preparation method thereof Download PDFInfo
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- CN109971466A CN109971466A CN201711450475.0A CN201711450475A CN109971466A CN 109971466 A CN109971466 A CN 109971466A CN 201711450475 A CN201711450475 A CN 201711450475A CN 109971466 A CN109971466 A CN 109971466A
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- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
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Abstract
The present invention discloses a kind of quantum dot and preparation method, and method includes: to provide quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid;In inert gas atmosphere, the quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are mixed and heated, reaction obtains quantum dot.The quantum dot size of prior art preparation of the present invention is excessive, there are problems that luminous peak position blue shift.
Description
Technical field
The present invention relates to technology of quantum dots fields more particularly to a kind of quantum dot and preparation method thereof.
Background technique
The excitation wavelength range of quantum dot is wide, and transmitting peak position is continuously adjusted and half-peak width, and photochemical stability is strong,
The fields such as display, illumination, light-use, biomarker obtain extensive concern.
The optical characteristics of quantum dot is generated based on quantum limitation effect, according to quantum limitation effect, works as unit
(element) when being reduced in size to equal to or less than intrinsic bohr exciton radii, the band gap of the unit increases.Therefore, when entering
When penetrating the wavelength of light over the qds has the energy higher than the band-gap energy, which absorbs the light and makes the quantum dot
In excitation state, then the quantum dot emission has the light of specific wavelength and returns to ground state, and from the light of the quantum dot emission
There can be the wavelength corresponding to the band-gap energy.Thus, by controlling the size of quantum dot and forming the hair of optional quantum dot
Light characteristic, therefore quantum dot is widely used in various light emitting devices.
The method of control quantum dot size is mainly to adjust the ratio of reactant or by adjusting the reaction time at present.So
And when controlling quantum dot size by adjusting the ratio of reactant, the ratio of certain reactants is too low to will cause target product
Yield it is very few and the phenomenon that lead to luminescent decay, so there is adjustment bottleneck.And quantum dot is controlled by adjusting the reaction time
When size, if once injecting reactant, moment reaches supersaturation and is precipitated quantum dot in a solvent, as Ostwald is cured
The extension of time, partial size become larger;If persistently inject reactant, with the increase of reaction volume, partial size is gradually increased.
Thus either once still persistently injection reactant prepares quantum dot to injection reactant, is all based on an initial size then
The size is gradually increased, and can not prepare the quantum dot also small compared with initial size.
Therefore, the prior art could be improved.
Summary of the invention
The purpose of the present invention is to provide a kind of quantum dots and preparation method thereof, it is intended to solve the quantum of prior art preparation
Spot size is excessive, there are problems that luminous peak position blue shift.
Technical scheme is as follows:
A kind of preparation method of quantum dot, wherein comprising steps of
Quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are provided;
In inert gas atmosphere, the quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are mixed and heated,
Reaction obtains quantum dot.
The preparation method of the quantum dot, wherein the molecular formula of the tertiary base mercaptan of liquid is CnH2nAmSH, wherein A
For tertiary base carbochain, m >=1 and 7 < m+n < 20, m and n are natural number.
The preparation method of the quantum dot, wherein the tertiary base mercaptan of liquid be tert octyl mercaptan, tertiary nonyl mercaptan,
Tert-dodecylmercaotan or tertiary hexadecyl mercaptan.
The preparation method of the quantum dot, wherein the quantum dot cation precursor is selected from the Ith race, the IIth race, the
The precursor of III race or the IVth race's metallic element;And/or the organic solvent is selected from long chain alkane, long-chain olefin, long-chain alcohol, length
One of streptamine, long-chain ester, long chain fatty acids, long chain mercaptans, trialkyl phosphine, trialkyl phosphine oxides and deionized water are more
Kind.
The preparation method of the quantum dot, wherein in inert gas atmosphere, by the quantum dot cation precursor,
The step of organic solvent and the tertiary base mercaptan of liquid are mixed and heated, and reaction obtains quantum dot includes: by body before quantum dot cation
Body and organic solvent are mixed to get mixed liquor, are placed in inert gas atmosphere, and the tertiary base mercaptan of liquid is injected in Xiang Suoshu mixed liquor
And heat, reaction obtains quantum dot.
The preparation method of the quantum dot, wherein the step is in inert gas atmosphere, by the quantum dot cation
Precursor, organic solvent and the tertiary base mercaptan of liquid are mixed and heated, and it further includes before to the mixed liquor that reaction, which obtains quantum dot,
The step of being de-gassed.
The preparation method of the quantum dot, wherein the degassing process time is 25 ~ 60mins.
The preparation method of the quantum dot, wherein carried out at preheating while being de-gassed to the mixed liquor
Reason, the pre-heat treatment temperature are 80 ~ 180 DEG C.
The preparation method of the quantum dot, wherein by the quantum dot cation precursor, organic solvent and liquid uncle
The heating temperature that base mercaptan is mixed and heated is 220 ~ 250 DEG C.
A kind of quantum dot, wherein be prepared using the preparation method of quantum dot as described above, the quantum dot is put down
Equal partial size is 3nm -10nm.
The utility model has the advantages that the present invention react with quantum dot precursor preparing quantum using the tertiary base mercaptan of liquid as sulphur source
Point, the tertiary base mercaptan of liquid, which not only has, participates in the sulfydryl that quantum dot is formed, while having tertiary base carbochain, occupies larger space volume
Characteristic, in Ostwald maturation stage, since tertiary base carbochain occupies larger space steric hindrance in the tertiary base mercaptan of liquid, quantum dot it
Between all directions further combined with becoming difficult, so that the partial size of quantum dot effectively be prevented to increase as the curing time extends
Greatly, and as the tertiary base carbochain in the tertiary base mercaptan of the liquid of addition is more, rank is cured in Ostwald in quantum dot synthesis process
The steric hindrance being subject to when section is bigger, thus can reduce synthetic quantity by improving the accounting of tertiary base carbochain in the tertiary base mercaptan of liquid
The partial size of son point, solves the problems, such as that the quantum dot size of prior art preparation is excessive, there are luminous peak position blue shifts.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the preparation method of quantum dot provided by the invention.
Specific embodiment
The present invention provides a kind of quantum dot and preparation method thereof, to make the purpose of the present invention, technical solution and effect more
Clear, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only used to
It explains the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method of quantum dot, as shown in Figure 1, comprising steps of
100, quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are provided;
200, in inert gas atmosphere, the quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are mixed simultaneously
Heating, reaction obtain quantum dot.
The present invention has the characteristic of sulfydryl and tertiary base carbochain using tertiary base mercaptan, and sulfydryl generates quantum for participating in reaction
Point, and since tertiary base carbochain has large space steric hindrance, the combination between quantum dot can be prevented, so that it is smaller to reach control generation
The effect of the quantum dot of particle size.
Above-mentioned steps are described in detail below by specific embodiment.
In the step 100, the molecular formula of the tertiary base mercaptan of liquid is CnH2nAmSH, wherein A is tertiary base carbochain, wherein
Sulfydryl (- SH) can connect on the C atom in tertiary base or on the C atom of non-tertiary base, it is clear that m >=1, it is single although carbochain is longer
The steric hindrance that a tertiary base mercaptan of liquid occupies is bigger, can more prevent the combination between quantum dot, but too long carbochain is not yet
Conducive to effective sulfydryl that provides to participate in the formation of quantum dot, preferably, m also needs to meet 7 < m+n < 20, wherein m and n is nature
Number, neither influences the synthesis of quantum dot, and can effectively prevent the combination between established quantum dot, avoids content quantum dot
Partial size becomes larger.
Preferably, the tertiary base mercaptan of liquid is tert octyl mercaptan, tertiary nonyl mercaptan, tert-dodecylmercaotan or uncle 16
Alkyl hydrosulfide.
The quantum dot cation precursor is selected from the precursor of the Ith race, the IIth race, the IIIth race and the IVth race's metallic element
One of or it is a variety of, as long as the metallic element precursor that can generate quantum dot, such as the Ith race can be reacted with sulfydryl
Cs etc., Zn, Hg, Cd, Cu of the IIth race etc., Ga, In, As etc. of the IIIth race, the Pb etc. of the IVth race can be oxide,
It can be halide or salt.
The organic solvent is selected from long chain alkane, long-chain olefin, long-chain alcohol, long-chain amine, long-chain ester, long chain fatty acids, length
One of chain mercaptan, trialkyl phosphine, trialkyl phosphine oxides and deionized water are a variety of, as long as can be by quantum dot cation
Precursor dissolution, which is thought, allows quantum dot cation to carry out reacting generation quantum dot with the tertiary base mercaptan of liquid.
In the step 200, in inert gas atmosphere, first the quantum dot cation precursor, organic solvent are mixed
Uniformly, inert gas atmosphere can be avoided oxygen etc. other to quantum dot generate reaction interfere.Then the tertiary base of liquid is added
Mercaptan is mixed and heated, and reaction obtains quantum dot, after reaction solution is cooled to room temperature, will successively be produced with toluene and dehydrated alcohol
After object is dissolved repeatedly, precipitated, to get quantum dot is arrived, the quantum dot has partial size more smaller than conventional method for centrifugation purification.
Further, in the step 200, the quantum dot grain of synthesis can be controlled by the way that the amount of the tertiary base mercaptan of liquid is added
Diameter size, addition it is more, obtained quantum point grain diameter is smaller.
Preferably, before by the mixed liquor of quantum dot cation precursor and organic solvent and the tertiary base thiol reaction of liquid,
Mixed liquor is placed under vacuum and is de-gassed 25 ~ 60mins, the foreign gas being dissolved in mixed liquor is discharged, is taken off
Mixed liquor after gas disposal;It is particularly preferred that carrying out the pre-heat treatment when being de-gassed, mixed liquor is warming up to 80 ~ 180 DEG C,
With the foreign gas discharge being more thoroughly dissolved in mixed liquor;
Then the mixed liquor after degassing process is placed in the inert gas atmospheres such as nitrogen or argon gas, is heated to 220 ~ 250 DEG C, and
The liquid level of mixed liquor after injecting the tertiary base mercaptan to degassing process of liquid is hereinafter, the tertiary base mercaptan of liquid and the quantum dot in mixed liquor
Cationic precursor is reacted, and is obtained quantum dot head product, is cooled to room temperature after reaction, and with toluene, dehydrated alcohol
Head product is dissolved repeatedly, precipitated and is centrifuged purification to get to smaller size of quantum dot.
It is particularly preferred that the heating process carries out in a manner of heating up stage by stage, it is first heated to 100 ~ 110 DEG C, heat preservation 0.5 ~
1h is then heated to 230 ~ 250 DEG C and is reacted.
The preparation method of the quantum dot, wherein the heating temperature is 220 ~ 250 DEG C.
The present invention provides a kind of quantum dots, wherein is prepared using the preparation method of quantum dot as described above, institute
The average grain diameter for stating quantum dot is 3nm -10nm, and partial size can be as small as 3nm, and preparation-obtained quantum dot is prepared compared with conventional method
What is obtained has smaller particle, can satisfy the requirement of smaller particle dimensions, breaks through the blue shift bottleneck of quantum dot light emitting peak position.
Below by embodiment, the present invention is described in detail.
Embodiment 1
Preparing for the CdS quantum dot of violet light is as follows:
Under atmosphere of inert gases, by 15 mL octadecylenes (1-octadecene), 1 mL oleic acid (Oleic acid) and 128.4
Mixed liquor is then heated to 120 DEG C and 60 mins that deaerate by mg cadmium oxide (CdO) mixing under vacuum, then will be after degassing
Mixed liquor is heated to 250 DEG C under inert atmosphere, becomes that temperature is reduced to 230 DEG C after clarification forms Cd precursor after solution, then
It takes the tertiary spicy thioalcohol of 0.5 mL and is injected into Cd precursor liquid level in 0.2 s hereinafter, being then cooled to rapidly after 60 secs of reaction
Product is dissolved repeatedly with toluene and anhydrous methanol, is precipitated by room temperature, and centrifugation purification, obtaining average grain diameter is 3 nm violet lights
CdS quantum dot.
Embodiment 2
Yellow luminous CuInS2Preparing for alloy quantum dot is as follows:
By 221 mg anhydrous indium chlorides (InCl3), 191 mg cuprous iodides (CuI) simultaneously with 2 mL tert-dodecylmercaotans
(Tert-dodecylthiol) and 20 ml oleyl amines (Oleylamine) mixing, heating under vacuum to 80 DEG C and deaerate 60 mins,
Then the mixed liquor after degassing is heated to 110 DEG C under inert atmosphere, keeps the temperature 1h, continued to be heated to 215 DEG C, react 1h, produce
Raw CuInS2Alloy quantum dot head product stops heating, is cooled to room temperature to reaction solution, and again with toluene and anhydrous methanol are by product
It dissolves, precipitate repeatedly, centrifugation purification, obtaining average grain diameter is the Yellow luminous CuInS of 5 nm2Alloy quantum dot.
In conclusion the present invention react with quantum dot precursor preparing quantum using the tertiary base mercaptan of liquid as sulphur source
Point, the tertiary base mercaptan of liquid, which not only has, participates in the sulfydryl that quantum dot is formed, while having tertiary base carbochain, occupies larger space volume
Characteristic, in Ostwald maturation stage, since tertiary base carbochain occupies larger space steric hindrance in the tertiary base mercaptan of liquid, quantum dot it
Between all directions further combined with becoming difficult, so that the partial size of quantum dot effectively be prevented to increase as the curing time extends
Greatly, and as the tertiary base carbochain in the tertiary base mercaptan of the liquid of addition is more, rank is cured in Ostwald in quantum dot synthesis process
The steric hindrance being subject to when section is bigger, thus can reduce synthetic quantity by improving the accounting of tertiary base carbochain in the tertiary base mercaptan of liquid
The partial size of son point, solves the problems, such as that the quantum dot size of prior art preparation is excessive, there are luminous peak position blue shifts.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of quantum dot, which is characterized in that comprising steps of
Quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid are provided;
Under inert gas atmosphere, the quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid liquid are mixed
And heat, reaction obtains quantum dot.
2. the preparation method of quantum dot according to claim 1, which is characterized in that point of the tertiary base mercaptan of liquid liquid
Minor is CnH2nAmSH, wherein A is tertiary base carbochain, m >=1 and 7 < m+n < 20, and m and n are natural number.
3. the preparation method of quantum dot according to claim 1, which is characterized in that the tertiary base mercaptan of liquid liquid is uncle
Octyl mercaptan, tertiary nonyl mercaptan, tert-dodecylmercaotan or tertiary hexadecyl mercaptan.
4. the preparation method of quantum dot according to claim 1, which is characterized in that the quantum dot cation precursor is selected from
Ith race, the IIth race, the IIIth race or the IVth race's metallic element precursor;And/or the organic solvent is selected from long chain alkane, length
Olefine, long-chain alcohol, long-chain amine, long-chain ester, long chain fatty acids, long chain mercaptans, trialkyl phosphine, trialkyl phosphine oxides and go from
One of sub- water is a variety of.
5. the preparation method of quantum dot according to claim 1, which is characterized in that it is described in inert gas atmosphere, by institute
It states quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid to be mixed and heated, reacts the step of obtaining quantum dot packet
It includes:
Quantum dot cation precursor and organic solvent are mixed to get mixed liquor, are placed in inert gas atmosphere, is mixed to described
It closes the tertiary base mercaptan of liquid injection liquid and heats, reaction obtains quantum dot.
6. the preparation method of quantum dot according to claim 5, which is characterized in that it is described in inert gas atmosphere, by institute
Quantum dot cation precursor, organic solvent and the tertiary base mercaptan of liquid is stated to be mixed and heated, reaction the step of obtaining quantum dot it
Before further include being de-gassed to the mixed liquor.
7. the preparation method of quantum dot according to claim 6, which is characterized in that the degassing process time be 25 ~
60mins。
8. the preparation method of quantum dot according to claim 6, which is characterized in that be de-gassed to the mixed liquor
While the pre-heat treatment is carried out to mixed liquor, the temperature of the pre-heat treatment is 80 ~ 180 DEG C.
9. the preparation method of quantum dot according to claim 1, which is characterized in that by body before the quantum dot cation
The heating temperature that body, organic solvent and the tertiary base mercaptan of liquid are mixed and heated is 220 ~ 250 DEG C.
10. a kind of quantum dot, which is characterized in that using the preparation method system such as the described in any item quantum dots of claim 1-9
Standby to form, the average grain diameter of the quantum dot is 3nm -10nm.
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CN103265949A (en) * | 2013-04-28 | 2013-08-28 | 温州大学 | Method for preparing mononuclear AgInS2 quantum dot |
CN106701071A (en) * | 2016-11-17 | 2017-05-24 | 厦门大学 | Method for improving stability of perovskite quantum dot |
CN106833610A (en) * | 2017-01-20 | 2017-06-13 | 深圳天吉新创科技有限公司 | A kind of nuclear shell structure quantum point and preparation method thereof |
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CN103265949A (en) * | 2013-04-28 | 2013-08-28 | 温州大学 | Method for preparing mononuclear AgInS2 quantum dot |
CN106701071A (en) * | 2016-11-17 | 2017-05-24 | 厦门大学 | Method for improving stability of perovskite quantum dot |
CN106833610A (en) * | 2017-01-20 | 2017-06-13 | 深圳天吉新创科技有限公司 | A kind of nuclear shell structure quantum point and preparation method thereof |
Non-Patent Citations (2)
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AURÉLIE LEFRANÇOIS ET AL.,: ""Direct Synthesis of Highly Conductive tert-Butylthiol-Capped CuInS2 Nanocrystals"", 《CHEMPHYSCHEM》 * |
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