CN106381146B - Quantum dot purification method - Google Patents
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Abstract
The invention discloses a quantum dot purification method, which comprises the following steps: step A, adding organic fatty acid with a preset proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors; step B, then carrying out dissolution and reaction at a preset temperature; and C, cooling to room temperature, and performing centrifugal separation to obtain the quantum dots without unreacted precursors. According to the method, a high-purity quantum dot sample without unreacted precursors can be obtained by adding organic fatty acid in a certain proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors, dissolving and reacting at a proper temperature, cooling to room temperature for precipitation, and then performing centrifugal separation.
Description
Technical Field
The invention relates to the field of quantum dot materials, in particular to a quantum dot purification method.
Background
The quantum dots have a plurality of unique nanometer properties due to the remarkable quantum confinement effect of the quantum dots: the emission wavelength is continuously adjustable, the light-emitting wavelength is narrow, the absorption spectrum is wide, the light-emitting intensity is high, the fluorescence lifetime is long, and the like. Due to the characteristics, the quantum dots have wide application prospects in the photoelectric fields of flat panel display, solid-state illumination, photovoltaic solar energy and the like.
As is well known, in optoelectronic devices such as semiconductor display devices, lighting devices and solar devices, the requirement for the purity of optoelectronic materials is very high, and the introduction of trace impurities not only affects the optical and electrical properties of the optoelectronic materials, but also affects the carriers and excitons in the optoelectronic devices, thereby greatly reducing the performance of the corresponding optoelectronic devices.
The semiconductor colloid quantum dots currently used in the photoelectric field are mostly prepared by a metallorganic thermal decomposition synthesis method. In the method, the reaction system of the anion precursor and the cation precursor reaches the instant supersaturation of reactants at high temperature, so that the nucleation reaction and the subsequent growth reaction occur in a short time, and finally the quantum dots with good size monodispersity are formed. Due to the difference in reactivity of different precursors and the different requirements of the components of the formed quantum dots, one or more excess or residual precursor reactants often still exist in the reaction system after the quantum dots are formed.
For these excess or residual precursor reactants, the conventional treatment method is to remove them by multiple precipitation and centrifugation, but some residual precursors such as zinc oleate precipitate from the reaction system to different degrees at a certain temperature, and the solubility in conventional dispersing solvents such as n-hexane, chloroform, toluene and the like is low, so that they precipitate together with the quantum dots during centrifugation, thereby greatly affecting the purity of the quantum dot product.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a quantum dot purification method, which aims to solve the problem that the prior art cannot purify quantum dots quickly and effectively.
The technical scheme of the invention is as follows:
a quantum dot purification method, comprising:
step A, adding organic fatty acid with a preset proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors;
step B, then carrying out dissolution and reaction at a preset temperature;
and C, finally cooling to room temperature, precipitating, and then performing centrifugal separation to obtain the quantum dots without unreacted precursors.
The quantum dot purification method comprises the steps that the quantum dot reaction system is a II-VI group quantum dot reaction system, a III-V group quantum dot reaction system or an IV-VI group quantum dot reaction system, and the quantum dot solution system is a II-VI group quantum dot solution system, a III-V group quantum dot solution system or an IV-VI group quantum dot solution system.
The quantum dot purification method is characterized in that the quantum dots in the quantum dot reaction system or the quantum dot solution system are of a quantum dot uniform binary component mononuclear structure, a quantum dot uniform multi-component alloy component mononuclear structure, a quantum dot multi-component gradually-changed mononuclear structure, a quantum dot binary component discrete core-shell structure, a quantum dot multi-component alloy component discrete core-shell structure or a quantum dot multi-component gradually-changed core-shell structure.
In the quantum dot purification method, in the quantum dot reaction system or the quantum dot solution system, the core and shell compounds of the quantum dots are CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdSeSTe, ZnSeTe or CdZnSeTe of II-VI groups; or InP, InAs or InAsP from group III-V; or group IV-VI PbS, PbSe, PbTe, PbSeS, PbSeTe or PbSTe; or a combination of any one or more of the above.
The quantum dot purification method is characterized in that the organic fatty acid is monounsaturated fatty acid, polyunsaturated fatty acid or saturated fatty acid.
The quantum dot purification method, wherein the residual or excess unreacted precursor is a cation precursor or an anion precursor.
The quantum dot purification method is characterized in that the adding proportion of the organic fatty acid is 0.05 to 10 times of the total volume of the quantum dot reaction system or the quantum dot solution system.
The quantum dot purification method comprises the step B, wherein the preset temperature is 10-400 ℃.
In the quantum dot purification method, in the step B, the total time of dissolution and reaction is 5 seconds to 10 hours.
The quantum dot purification method comprises the step A of adding organic fatty acid in an inert atmosphere, an air atmosphere or vacuum.
Has the advantages that: according to the invention, a high-purity quantum dot sample without unreacted precursors can be obtained by adding organic fatty acid in a certain proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors, dissolving and reacting at a proper temperature, cooling to room temperature for precipitation, and then performing centrifugal separation and purification.
Drawings
Fig. 1 is a flow chart of a quantum dot purification method according to a preferred embodiment of the present invention.
Detailed Description
The invention provides a quantum dot purification method, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the 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.
Referring to fig. 1, fig. 1 is a flow chart of a quantum dot purification method according to a preferred embodiment of the present invention, as shown in the figure, it includes:
step S1, adding organic fatty acid with a preset proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors;
step S2, then carrying out dissolution and reaction at a predetermined temperature;
and step S3, finally cooling to room temperature, precipitating, and then carrying out centrifugal separation to obtain the quantum dots containing no unreacted precursor.
According to the invention, the organic fatty acid is added into the quantum dot reaction system or the quantum dot solution system containing the residual or excessive unreacted precursor, and the dissolution reaction and the centrifugal separation are carried out, so that the unreacted precursor is effectively removed, the purity of the final product of the quantum dot is improved, and the requirement of the photoelectric device application on the purity of the quantum dot can be fully met.
Further, the quantum dot reaction system is a II-VI group quantum dot reaction system, a III-V group quantum dot reaction system or an IV-VI group quantum dot reaction system, and the quantum dot solution system is a II-VI group quantum dot solution system, a III-V group quantum dot solution system or an IV-VI group quantum dot solution system.
Further, the quantum dots in the quantum dot reaction system or the quantum dot solution system are of a single-core structure with uniform binary components of the quantum dots, a single-core structure with uniform multi-component alloy components of the quantum dots, a gradient single-core structure with multi-component alloy components of the quantum dots, a discrete core-shell structure with binary components of the quantum dots, a discrete core-shell structure with multi-component alloy components of the quantum dots or a gradient core-shell structure with multi-component alloy components of the quantum dots.
Further, in the quantum dot reaction system or the quantum dot solution system, the core and shell compounds of the quantum dots are CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeTe or CdZnSeTe of II-VI groups; or InP, InAs or InAsP from group III-V; or group IV-VI PbS, PbSe, PbTe, PbSeS, PbSeTe or PbSTe; or a combination of any one or more of the above.
Further, the organic fatty acid is a monounsaturated fatty acid, a polyunsaturated fatty acid, or a saturated fatty acid. Wherein, the monounsaturated fatty acid can be oleic acid, myristoleic acid, palmitoleic acid, erucic acid or the like; the polyunsaturated fatty acid may be eicosapentaenoic acid (EPA) or docosahexaenoic acid (DHA), etc.; the saturated fatty acid may be caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, or the like.
Further, the residual or excess unreacted precursor is a cationic precursor or an anionic precursor. Wherein the cation precursor is fatty acid cadmium, fatty acid zinc, fatty acid lead or fatty acid indium, wherein the fatty acid is any one of the organic fatty acids listed above; the anion precursor can be a compound formed by any combination of three elements of sulfur, selenium or tellurium and the following organic substances: trioctylphosphine (abbreviated as TOP, the same below), Octadecene (1-octadiene, abbreviated as ODE, the same below), Oleic acid (abbreviated as OA, the same below), Octadecylamine (abbreviated as ODA, the same below), Trioctylamine (abbreviated as TOA, the same below), Octadecylphosphonic acid (abbreviated as ODPA, the same below), 9-octadecenylamine (Octylamine).
Further, the organic fatty acid is added in a proportion of 0.05 to 10 times of the total volume of the quantum dot reaction system, for example, specifically 0.05, 0.1, 0.2, 0.5, 1, 2, 5 or 10 times of the total volume of the quantum dot reaction system.
Further, in the step S2, the predetermined temperature is 10 to 400 ℃, for example, the predetermined temperature is 10 ℃, 20 ℃, 50 ℃, 100 ℃, 150 ℃, 200 ℃, 220 ℃, 300 ℃ and 400 ℃.
Further, in the step S2, the total time period of the dissolution and the reaction is 5 seconds to 10 hours, for example, the total time period of the dissolution and the reaction is 5 seconds, 10 seconds, 1 minute, 5 minutes, 30 minutes, 1 hour, 5 hours, or 10 hours.
Further, in the step S1, the atmosphere to which the organic fatty acid is added is an inert atmosphere, an air atmosphere, or a vacuum. Wherein the vacuum pressure is less than 100 Pa.
In the invention, the organic fatty acid is added into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors, so that the organic fatty acid and the residual or excessive unreacted precursors can be mutually dissolved with the reaction system in a dissolving or coordination reaction mode, and cannot be separated out when the temperature is reduced to room temperature or precipitation and centrifugation are carried out, and thus, a high-purity quantum dot sample can be obtained by fully separating from the quantum dots.
Example 1
The quantum dot reaction system containing excess zinc oleate cation precursor was directly treated with oleic acid OA:
a. reducing the temperature of a quantum dot reaction system (the total volume is 20 ml) after the reaction in the three-mouth bottle from 300 ℃ to 150 ℃;
b. adding 5 ml of oleic acid into the quantum dot reaction system, and keeping the temperature at 150 ℃ for dissolving and reacting for 30 minutes;
c. cooling the quantum dot reaction system to room temperature, then precipitating, and then carrying out centrifugal separation, wherein the method specifically comprises the following steps: adding acetone into the quantum dot reaction system to obtain a precipitate, performing centrifugal separation, removing a liquid phase, re-dispersing a solid phase in n-hexane, adding acetone, re-precipitating, performing centrifugal separation, and repeating the steps for 5 times to obtain a high-purity quantum dot sample.
Example 2
Treating a quantum dot solution system containing excess zinc oleate cation precursor with stearic acid:
a. under the protection of inert atmosphere, 15 ml of n-hexane solution containing excessive zinc oleate cation precursor quantum dots is injected into a three-necked bottle containing 15 ml of Octadecene (ODE);
b. heating the quantum dot solution system in the three-necked bottle to 80 ℃ and maintaining for 30 minutes so as to completely remove n-hexane in the quantum dot solution system;
c. continuously heating the quantum dot solution system to 150 ℃, adding 3 ml of stearic acid into the quantum dot solution system, and reacting for 30 minutes at the temperature of 150 ℃;
d. cooling the reaction system to room temperature, and then carrying out conventional precipitation, centrifugal separation and purification: adding acetone to obtain a precipitate, performing centrifugal separation, pouring off a liquid phase, re-dispersing a solid phase obtained by centrifugation into n-hexane, adding acetone to re-precipitate and centrifuge, and repeating the steps for 5 times to obtain a high-purity quantum dot sample.
Example 3
Quantum dot reaction systems containing excess S-TOP (thio-trioctylphosphine) anion precursor were treated directly with oleic acid OA:
a. reducing the temperature of a quantum dot reaction system (the total volume is 20 ml) after the reaction in the three-necked bottle from 300 ℃ to 150 ℃;
b. adding 10 ml of oleic acid into the quantum dot reaction system, and reacting for 180 minutes at 220 ℃;
c. after cooling the quantum dot reaction system to room temperature, carrying out centrifugal separation after precipitation, and specifically comprising the following steps: adding acetone to obtain a precipitate, performing centrifugal separation, removing a liquid phase, re-dispersing a solid phase in n-hexane, adding acetone to re-precipitate, performing centrifugal separation, and repeating the steps for 5 times to obtain a high-purity quantum dot sample.
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 (9)
1. A quantum dot purification method is characterized by comprising the following steps:
step A, adding organic fatty acid with a preset proportion into a quantum dot reaction system or a quantum dot solution system containing residual or excessive unreacted precursors;
step B, then carrying out dissolution and reaction at a preset temperature;
step C, finally cooling to room temperature, precipitating, and then carrying out centrifugal separation to obtain quantum dots without unreacted precursors;
the residual or excessive unreacted precursor is a cation precursor or an anion precursor;
the cation precursor is fatty acid cadmium, fatty acid zinc, fatty acid lead or fatty acid indium;
the anion precursor is a compound formed by combining three elements of sulfur, selenium or tellurium and an organic matter.
2. The quantum dot purification method according to claim 1, wherein the quantum dot reaction system is a group II-VI quantum dot reaction system, a group III-V quantum dot reaction system, or a group IV-VI quantum dot reaction system, and the quantum dot solution system is a group II-VI quantum dot solution system, a group III-V quantum dot solution system, or a group IV-VI quantum dot solution system.
3. The quantum dot purification method according to claim 1, wherein the quantum dots in the quantum dot reaction system or the quantum dot solution system are of a quantum dot homogeneous binary component single-core structure, a quantum dot homogeneous multi-component alloy component single-core structure, a quantum dot multi-component alloy component gradient single-core structure, a quantum dot binary component discrete core-shell structure, a quantum dot multi-component alloy component discrete core-shell structure or a quantum dot multi-component alloy component gradient core-shell structure.
4. The quantum dot purification method according to claim 1, wherein in the quantum dot reaction system or the quantum dot solution system, the core and shell compounds of the quantum dots are CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeTe or CdZnSeTe of groups II-VI; or InP, InAs or InAsP from group III-V; or group IV-VI PbS, PbSe, PbTe, PbSeS, PbSeTe or PbSTe; or a combination of any one or more of the above.
5. The quantum dot purification method according to claim 1, wherein the organic fatty acid is a monounsaturated fatty acid, a polyunsaturated fatty acid, or a saturated fatty acid.
6. The quantum dot purification method according to claim 1, wherein the organic fatty acid is added in a proportion of 0.05 to 10 times the total volume of the quantum dot reaction system or the quantum dot solution system.
7. The quantum dot purification method according to claim 1, wherein the predetermined temperature in the step B is 10 to 400 ℃.
8. The quantum dot purification method according to claim 1, wherein in the step B, the total time period of dissolution and reaction is 5 seconds to 10 hours.
9. The method for purifying quantum dots according to claim 1, wherein in the step A, the atmosphere to which the organic fatty acid is added is an inert atmosphere, an air atmosphere or a vacuum.
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| KR20180097201A (en) * | 2017-02-22 | 2018-08-31 | 시노코 유한회사 | Synthesis method of quantum dot with metal oxide shell by continuous crystal growth and quantum dot at the same |
| CN109535009B (en) * | 2017-09-21 | 2022-04-01 | Tcl科技集团股份有限公司 | Method for purifying amine organic matter |
| CN109666478A (en) * | 2017-10-16 | 2019-04-23 | Tcl集团股份有限公司 | A kind of method of purification of oil-soluble quantum dot |
| CN109971458A (en) * | 2017-12-27 | 2019-07-05 | 深圳Tcl工业研究院有限公司 | A kind of method of purification of quantum dot |
| CN108219792B (en) * | 2018-02-09 | 2021-05-07 | 纳晶科技股份有限公司 | Quantum dot purification method, quantum dot, device and quantum dot composition |
| EP3536761B1 (en) | 2018-03-09 | 2021-11-24 | Samsung Electronics Co., Ltd. | Quantum dots |
| US10954440B2 (en) | 2018-03-09 | 2021-03-23 | Samsung Electronics Co., Ltd. | Quantum dots and devices including the same |
| US11011720B2 (en) | 2018-03-09 | 2021-05-18 | Samsung Electronics Co., Ltd. | Semiconductor nanocrystal particles, production methods thereof, and devices including the same |
| CN108558648B (en) * | 2018-04-03 | 2021-07-02 | 苏州星烁纳米科技有限公司 | Method for treating zinc slag containing oil acid generated by synthesizing quantum dots |
| CN108484389B (en) * | 2018-04-17 | 2021-06-29 | 苏州星烁纳米科技有限公司 | Method for treating zinc slag containing oil acid generated by synthesizing quantum dots |
| CN111349439B (en) * | 2018-12-20 | 2022-05-24 | Tcl科技集团股份有限公司 | Quantum dot purification method |
| CN111375312B (en) * | 2018-12-27 | 2021-03-30 | Tcl科技集团股份有限公司 | Quantum dot purification method and quantum dot purification device |
| CN111378450A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Quantum dot purification method |
| CN111682118B (en) * | 2020-06-24 | 2023-06-09 | 合肥福纳科技有限公司 | Quantum dot preparation method, photosensitive layer and solar cell device |
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