CN109971466B - Quantum dot and preparation method thereof - Google Patents
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Abstract
The invention discloses a quantum dot and a preparation method thereof, wherein the method comprises the following steps: providing a quantum dot cation precursor, an organic solvent and liquid tertiary mercaptan; and mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere, and reacting to obtain the quantum dot. The quantum dots prepared by the prior art are overlarge in size and have the problem of blue shift of a luminescence peak position.
Description
Technical Field
The invention relates to the technical field of quantum dots, in particular to a quantum dot and a preparation method thereof.
Background
The quantum dots have wide excitation wavelength range, continuously adjustable emission peak position, narrow half-peak width and strong photochemical stability, and are widely concerned in the fields of display, illumination, light energy utilization, biological marking and the like.
The optical characteristics of quantum dots are generated based on a quantum confinement effect according to which the band gap of a cell (element) increases when the size of the cell is reduced to be equal to or less than the intrinsic bohr exciton radius. Accordingly, when the wavelength of light incident on a quantum dot has energy higher than the band gap energy, the quantum dot absorbs the light so that the quantum dot is in an excited state, and then the quantum dot emits light having a specific wavelength and returns to a ground state, and the light emitted from the quantum dot may have a wavelength corresponding to the band gap energy. Thus, the light emitting characteristics of quantum dots can be selected by controlling the size and composition of the quantum dots, and thus the quantum dots have been widely used in various light emitting devices.
The current methods for controlling the size of quantum dots are mainly to adjust the ratio of reactants or by adjusting the reaction time. However, when the quantum dot size is controlled by adjusting the ratio of the reactants, the ratio of some reactants is too low, which results in a phenomenon that the yield of the target product is too low to cause a decrease in luminescence, so that there is a bottleneck in adjustment. When the size of the quantum dot is controlled by adjusting the reaction time, if a reactant is injected once, the quantum dot is instantaneously supersaturated in the solvent to be separated out, and the particle size is gradually increased along with the prolonging of the Ostwald curing time; if the reactants are continuously injected, the particle size gradually increases as the amount of the reactants increases. Therefore, whether the quantum dots are prepared by injecting the reactant once or continuously, the quantum dots cannot be prepared by a size smaller than the initial size because the size is gradually increased based on the initial size.
Therefore, the prior art has yet to be improved.
Disclosure of Invention
The invention aims to provide a quantum dot and a preparation method thereof, and aims to solve the problems that the quantum dot prepared by the prior art is overlarge in size and blue shift of a luminescence peak exists.
The technical scheme of the invention is as follows:
a preparation method of quantum dots comprises the following steps:
providing a quantum dot cation precursor, an organic solvent and liquid tertiary mercaptan;
and mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere, and reacting to obtain the quantum dot.
The preparation method of the quantum dot comprises the step of preparing the liquid tertiary mercaptan, wherein the molecular formula of the liquid tertiary mercaptan is CnH2nAmSH, wherein A is tertiary carbon chain, m is more than or equal to 1 and more than 7 and m + n is less than 20, and m and n are natural numbers.
The preparation method of the quantum dot comprises the step of preparing a liquid tertiary mercaptan, wherein the liquid tertiary mercaptan is tert-octyl mercaptan, tert-nonyl mercaptan, tert-dodecyl mercaptan or tert-hexadecyl mercaptan.
The preparation method of the quantum dot comprises the following steps of (1) selecting a cation precursor of the quantum dot from precursors of metal elements in a group I, a group II, a group III or a group IV; and/or the organic solvent is selected from one or more of long chain alkanes, long chain alkenes, long chain alcohols, long chain amines, long chain esters, long chain fatty acids, long chain thiols, trialkylphosphines, trialkylphosphine oxides and deionised water.
The preparation method of the quantum dot comprises the following steps of mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere, and reacting to obtain the quantum dot: and mixing the quantum dot cation precursor with an organic solvent to obtain a mixed solution, placing the mixed solution in an inert gas atmosphere, injecting liquid tertiary mercaptan into the mixed solution, heating, and reacting to obtain the quantum dot.
The preparation method of the quantum dot comprises the steps of mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere, and degassing the mixed solution before reacting to obtain the quantum dot.
The preparation method of the quantum dot comprises the step of degassing for 25-60 mins.
The preparation method of the quantum dots comprises the step of degassing the mixed solution and simultaneously carrying out preheating treatment at the temperature of 80-180 ℃.
The preparation method of the quantum dot comprises the steps of mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan at the heating temperature of 220-250 ℃.
The quantum dot is prepared by the preparation method of the quantum dot, and the average particle size of the quantum dot is 3 nm-10 nm.
Has the advantages that: the invention takes the liquid tertiary mercaptan as the sulfur source to react with the quantum dot precursor to prepare the quantum dot, the liquid tertiary mercaptan not only has the sulfydryl participating in the formation of the quantum dot, but also has the characteristics of tertiary carbon chain occupying larger space volume, in the Ostwald ripening stage, as the tertiary carbon chain in the liquid tertiary mercaptan occupies larger steric hindrance, further combination between quantum dots in all directions becomes difficult, thereby effectively preventing the particle size of the quantum dots from increasing along with the prolonging of the curing time, and the steric hindrance suffered by the quantum dots at the Ostwald curing stage in the synthetic process is larger along with the more tertiary carbon chains in the added liquid tertiary mercaptan, therefore, the particle size of the synthesized quantum dot can be reduced by improving the proportion of tertiary carbon chains in the liquid tertiary mercaptan, and the problems of overlarge size and blue shift of a luminescence peak position of the quantum dot prepared by the prior art are solved.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a quantum dot provided by the invention.
Detailed Description
The present invention provides a quantum dot and a method for preparing the same, and the present invention is further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a preparation method of quantum dots, which comprises the following steps as shown in figure 1:
100. providing a quantum dot cation precursor, an organic solvent and liquid tertiary mercaptan;
200. and mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere, and reacting to obtain the quantum dot.
The invention utilizes the characteristics of tertiary mercaptan and tertiary carbon chain, wherein the mercapto is used for participating in the reaction to generate the quantum dots, and the tertiary carbon chain has large steric hindrance and can prevent the quantum dots from being combined, thereby achieving the effect of controlling the generation of the quantum dots with smaller particle size.
The above steps are described in detail below with reference to specific embodiments.
In the step 100, the molecular formula of the liquid tertiary mercaptan is CnH2nAmSH, where A is a tertiary carbon chain in which a mercapto group (-SH) may be attached to a C atom in the tertiary or to a C atom in the non-tertiary group, it is apparent that m.gtoreq.1, although the longer the carbon chain, the greater the steric hindrance occupied by a single liquid tertiary thiol, the more resistant it is to prevent quantum dots from being placed between themselvesHowever, too long carbon chains are not beneficial to effectively provide sulfydryl to participate in the formation of the quantum dots, preferably, m also needs to satisfy 7 < m + n < 20, wherein m and n are natural numbers, the synthesis of the quantum dots is not affected, the combination of the formed quantum dots can be effectively prevented, and the particle size of the quantum dots with the content is prevented from being increased.
Preferably, the liquid tertiary mercaptan is tert-octyl mercaptan, tert-nonyl mercaptan, tert-dodecyl mercaptan or tert-hexadecyl mercaptan.
The cation precursor of the quantum dot is selected from one or more precursors of metal elements In groups I, II, III and IV, As long As the cation precursor of the quantum dot can react with sulfydryl to generate a metal element precursor of the quantum dot, for example, Cs and the like In the group I, Zn, Hg, Cd, Cu and the like In the group II, Ga, In, As and the like In the group III, Pb and the like In the group IV can be oxides, halides or salts.
The organic solvent is selected from one or more of long-chain alkane, long-chain olefin, long-chain alcohol, long-chain amine, long-chain ester, long-chain fatty acid, long-chain mercaptan, trialkylphosphine oxide and deionized water, as long as the quantum dot cation precursor can be dissolved to allow the quantum dot cation to react with liquid tertiary thiol to generate the quantum dot.
In the step 200, the quantum dot cation precursor and the organic solvent are uniformly mixed in an inert gas atmosphere, and the inert gas atmosphere can avoid interference of oxygen and the like on the quantum dot generation reaction. And then adding liquid tertiary mercaptan, mixing and heating, reacting to obtain quantum dots, cooling the reaction liquid to room temperature, repeatedly dissolving and precipitating the product by using toluene and absolute ethyl alcohol in sequence, and carrying out centrifugal purification to obtain the quantum dots, wherein the quantum dots have smaller particle sizes than the quantum dots obtained by the conventional method.
Further, in the step 200, the particle size of the synthesized quantum dot can be controlled by adding the amount of the liquid tertiary mercaptan, and the more the liquid tertiary mercaptan is added, the smaller the particle size of the quantum dot is obtained.
Preferably, before the mixed solution of the quantum dot cation precursor and the organic solvent is reacted with the liquid tertiary mercaptan, degassing the mixed solution in vacuum for 25-60 mins to discharge impurity gases dissolved in the mixed solution, so as to obtain a degassed mixed solution; preferably, the degassing treatment is performed by preheating, and the temperature of the mixed solution is increased to 80-180 ℃ to more thoroughly discharge the impurity gas dissolved in the mixed solution;
and then placing the degassed mixed solution in an inert gas atmosphere such as nitrogen or argon, heating to 220-250 ℃, injecting liquid tertiary mercaptan below the liquid level of the degassed mixed solution, reacting the liquid tertiary mercaptan with a quantum dot cation precursor in the mixed solution to obtain a quantum dot initial product, cooling to room temperature after the reaction is finished, and repeatedly dissolving, precipitating, centrifuging and purifying the initial product by using toluene and absolute ethyl alcohol to obtain the quantum dot with smaller size.
Preferably, the heating process is performed by heating to 100-110 ℃ in a staged manner, preserving heat for 0.5-1 h, and then heating to 230-250 ℃ for reaction.
The preparation method of the quantum dot comprises the step of heating at 220-250 ℃.
The invention provides a quantum dot, which is prepared by adopting the preparation method of the quantum dot, wherein the average particle size of the quantum dot is 3 nm-10 nm, the particle size can be as small as 3nm, and the prepared quantum dot has a smaller particle size than that prepared by a conventional method, can meet the size specification requirement of smaller particle size, and breaks through the blue shift bottleneck of the luminescent peak position of the quantum dot.
The present invention will be described in detail below with reference to examples.
Example 1
The purple luminous CdS quantum dots are prepared as follows:
mixing 15 mL of octadecene (1-octadecene), 1 mL of Oleic acid (Oleic acid) and 128.4 mg of cadmium oxide (CdO) in an inert gas atmosphere, heating the mixed solution to 120 ℃ in vacuum, degassing for 60mins, heating the degassed mixed solution to 250 ℃ in the inert atmosphere, reducing the temperature to 230 ℃ after the solution becomes clear to form a Cd precursor, taking 0.5 mL of tert-octyl mercaptan, injecting the tert-octyl mercaptan below the liquid level of the Cd precursor in 0.2 s, reacting for 60 secs, rapidly cooling to room temperature, repeatedly dissolving and precipitating the product with toluene and anhydrous methanol, and performing centrifugal purification to obtain the purple luminous CdS quantum dot with the average particle size of 3 nm.
Example 2
Yellow emitting CuInS2The preparation of the alloy quantum dots is as follows:
mixing 221 mg of anhydrous indium chloride (InCl 3) and 191 mg of cuprous iodide (CuI) with 2 mL of Tert-dodecyl mercaptan (Tert-dodecyl mercaptan) and 20 mL of Oleylamine (Oleylamine), heating to 80 ℃ under vacuum, degassing for 60mins, heating the degassed mixture to 110 ℃ under inert atmosphere, keeping the temperature for 1h, continuing to heat to 215 ℃, and reacting for 1h to obtain CuInS2Stopping heating the primary alloy quantum dot product, cooling the reaction liquid to room temperature, repeatedly dissolving and precipitating the product with toluene and anhydrous methanol, and centrifugally purifying to obtain yellow luminous CuInS with the average particle size of 5 nm2And (3) alloying the quantum dots.
In conclusion, the liquid tertiary thiol is used as a sulfur source to react with the quantum dot precursor to prepare the quantum dot, the liquid tertiary thiol not only has sulfydryl participating in the formation of the quantum dot, but also has the characteristics of tertiary carbon chains and larger space volume occupation, in the Ostwald ripening stage, as the tertiary carbon chain in the liquid tertiary mercaptan occupies larger steric hindrance, further combination between quantum dots in all directions becomes difficult, thereby effectively preventing the particle size of the quantum dots from increasing along with the prolonging of the curing time, and the steric hindrance suffered by the quantum dots at the Ostwald curing stage in the synthetic process is larger along with the more tertiary carbon chains in the added liquid tertiary mercaptan, therefore, the particle size of the synthesized quantum dot can be reduced by improving the proportion of tertiary carbon chains in the liquid tertiary mercaptan, and the problems of overlarge size and blue shift of a luminescence peak position of the quantum dot prepared by the prior art are solved.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of quantum dots is characterized by comprising the following steps:
providing a quantum dot cation precursor, an organic solvent and liquid tertiary mercaptan;
under the atmosphere of inert gas, mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan, and reacting to obtain quantum dots; the liquid tertiary mercaptan is tert-octyl mercaptan, tert-nonyl mercaptan, tert-dodecyl mercaptan or tert-hexadecyl mercaptan.
2. The method for preparing the quantum dot according to claim 1, wherein the quantum dot cation precursor is selected from precursors of group I, group II, group III or group IV metal elements; and/or the organic solvent is selected from one or more of long-chain alkane, long-chain alkene, long-chain alcohol, long-chain amine, long-chain ester, long-chain fatty acid, long-chain mercaptan, trialkyl phosphine and trialkyl phosphine oxide.
3. The method for preparing the quantum dot according to claim 1, wherein the step of mixing and heating the quantum dot cation precursor, the organic solvent and the liquid tertiary mercaptan in an inert gas atmosphere to react to obtain the quantum dot comprises:
and mixing the quantum dot cation precursor with an organic solvent to obtain a mixed solution, placing the mixed solution in an inert gas atmosphere, injecting liquid tertiary mercaptan into the mixed solution, heating, and reacting to obtain the quantum dot.
4. The method according to claim 3, wherein the step of mixing and heating the quantum dot cation precursor, the organic solvent, and the liquid tertiary mercaptan in an inert gas atmosphere to obtain the quantum dot further comprises degassing the mixed solution.
5. The method for preparing the quantum dot according to claim 4, wherein the degassing treatment time is 25-60 min.
6. The method according to claim 4, wherein the mixed solution is degassed and simultaneously preheated at 80 to 180 ℃.
7. The method for preparing a quantum dot according to claim 1, wherein the heating temperature for mixing and heating the quantum dot cation precursor, the organic solvent, and the liquid tertiary thiol is 220 to 250 ℃.
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| CN201711450475.0A CN109971466B (en) | 2017-12-27 | 2017-12-27 | Quantum dot and preparation method thereof |
| PCT/CN2018/122153 WO2019128810A1 (en) | 2017-12-27 | 2018-12-19 | Quantum dot and preparation method therefor |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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)
| Title |
|---|
| "Direct Synthesis of Highly Conductive tert-Butylthiol-Capped CuInS2 Nanocrystals";Aurélie Lefrançois et al.,;《ChemPhysChem》;20151007;第17卷(第5期);第654-659页 * |
| "Highly luminescent InP/GaP/ZnS QDs emitting in the entire color range via a heating up process";Joong Pill Park et al.,;《SCIENCE REPORT》;20160720;第6卷;第30094(1-6)页 * |
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