CN113046054B - Post-treatment method of oil-soluble quantum dots - Google Patents
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Abstract
The invention discloses a post-treatment method of oil-soluble quantum dots, which comprises the following steps: providing an oil-soluble quantum dot mixed solution containing a cation precursor; mixing the oil-soluble quantum dot mixed solution with a nonpolar solvent to obtain a first mixed solution; adding organic amine into the first mixed solution for reaction to obtain a second mixed solution; and adding a polar solvent into the second mixed solution, and purifying to obtain the oil-soluble quantum dot. Diluting the oil-soluble quantum dot mixed solution by using a nonpolar solvent, and complexing the oil-soluble quantum dot mixed solution with a cationic precursor, so that the problem that the precipitation of the oil-soluble quantum dot precipitates and wraps the cationic precursor to block the precipitation of the cationic precursor from complexing with the organic amine when the organic amine is added is avoided; finally adding a polar solvent for precipitation separation to obtain the oil-soluble quantum dots with higher purity. The post-treatment method has simple and easy operation flow, almost no requirement on temperature and atmosphere conditions, good reproducibility and large-scale popularization.
Description
Technical Field
The invention relates to the technical field of quantum dot purification, in particular to a post-treatment method of oil-soluble quantum dots.
Background
The remarkable quantum confinement effect of the quantum dots enables the quantum dots to have a plurality of unique nano properties: the emission wavelength is continuously adjustable, the emission wavelength is narrow, the absorption spectrum is wide, the emission intensity is high, the fluorescence lifetime is long, and the like. The characteristics lead the quantum dots to have wide application prospect in the photoelectric fields such as flat panel display, solid state lighting, photovoltaic solar energy and the like.
It is known that in optoelectronic devices such as semiconductor display devices, lighting devices and solar devices, the purity requirements for the optoelectronic materials are very high, and the introduction of trace impurities not only affects the optical and electrical properties of the optoelectronic materials themselves, but also affects the behavior of carriers, excitons and the like in the overall optoelectronic devices, thereby greatly reducing the performance of the corresponding optoelectronic devices. The current oil-soluble quantum dots used in the photoelectric field are mostly prepared by a colloid method, and the oil-soluble quantum dot mixed solution prepared by the colloid method often contains a large amount of unreacted cationic precursors and nonpolar solvents, and the applicable high-purity oil-soluble quantum dots are required to be obtained by purification after the preparation is finished; however, some cationic precursors such as zinc oleate are easy to be separated out when the temperature of the mixed solution is lower than a certain temperature, so that a lot of difficulties are brought to the cleaning and purification of the quantum dots, and it is reported that the solubility of the cationic precursors is improved by firstly adding organic amine into the mixed solution of the soluble quantum dots to be purified to complex with the cationic precursors, and then adding a polar solvent to precipitate and separate the oil-soluble quantum dots, so that the high-purity oil-soluble quantum dots are obtained.
However, the inventors have found that the organic amine, while complexing with the cationic precursor increases the solubility of the cationic precursor, has a polarity that also causes the oil-soluble quantum dots to precipitate in advance in the form of a precipitate, and the precipitated oil-soluble quantum dot precipitate will encapsulate the cation precursor precipitate that has not reached the complexation with the organic amine and hinder the binding of the cation precursor precipitate to the organic amine, resulting in that the unreacted cation precursor is difficult to be completely removed.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a post-treatment method of oil-soluble quantum dots, which aims to solve the problem that the conventional post-treatment method of oil-soluble quantum dots is difficult to completely remove unreacted cation precursors.
The technical scheme of the invention is as follows:
a post-treatment method of oil-soluble quantum dots comprises the following steps:
providing an oil-soluble quantum dot mixed solution containing a cation precursor;
mixing the oil-soluble quantum dot mixed solution with a nonpolar solvent to obtain a first mixed solution;
adding organic amine into the first mixed solution for reaction to obtain a second mixed solution;
and adding a polar solvent into the second mixed solution, and purifying to obtain the oil-soluble quantum dot.
The beneficial effects are that: diluting an oil-soluble quantum dot mixed solution by using a nonpolar solvent, and complexing by using organic amine and an unreacted cation precursor; avoiding that the precipitation of the oil-soluble quantum dots is separated out to wrap the precipitation of the cation precursor when the organic amine is added first so as to prevent the precipitation of the cation precursor from complexing with the organic amine; finally, the solubility of the cationic precursor in the polar solvent is enhanced by adding the polar solvent and complexing the cationic precursor with the organic amine, so that the cationic precursor in the oil-soluble quantum dot mixed solution can be completely removed by fully complexing the cationic precursor with the organic amine, and the oil-soluble quantum dot with higher purity is obtained. The post-treatment method of the oil-soluble quantum dots has the advantages of simple and easy operation flow, almost no requirement on temperature and atmosphere conditions, good reproducibility, complete removal of the cation precursor and large-scale popularization and application.
Drawings
Fig. 1 is a flowchart of a post-processing method of an oil-soluble quantum dot according to an embodiment of the present invention.
FIG. 2a is a graph showing the UV-visible absorption spectrum and fluorescence spectrum of a blue-emitting CdSe/ZnSe oil-soluble quantum dot solution of a residual Zn ion precursor in example 1 of the present invention;
FIG. 2b is a graph showing the UV-visible absorption spectrum and fluorescence spectrum of a blue light-emitting CdSe/ZnSe oil-soluble quantum dot solution treated in example 1 according to the invention.
FIG. 3a is a graph showing the UV-visible absorption spectrum and fluorescence spectrum of a red-light-emitting CdZnSeS oil-soluble quantum dot solution of a residual Zn ion precursor in example 2 of the present invention;
FIG. 3b is a graph showing the ultraviolet-visible absorption spectrum and fluorescence spectrum of the red-light-emitting CdZnSeS oil-soluble quantum dot solution treated in example 2 of the present invention.
Detailed Description
The invention provides a post-treatment method of oil-soluble quantum dots, which is used for making the purposes, technical schemes and effects of the invention clearer and more definite, and is further described in detail below. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides a post-treatment method of oil-soluble quantum dots, which is shown in fig. 1 and comprises the following steps:
s1, providing an oil-soluble quantum dot mixed solution containing a cation precursor;
s2, mixing the oil-soluble quantum dot mixed solution with a nonpolar solvent to obtain a first mixed solution;
s3, adding organic amine into the first mixed solution for reaction to obtain a second mixed solution;
s4, adding a polar solvent into the second mixed solution, and purifying to obtain the oil-soluble quantum dot.
In the embodiment, the oil-soluble quantum dot mixed solution is diluted by using a nonpolar solvent, and then is complexed with unreacted cationic precursor by using organic amine; avoiding that the precipitation of the oil-soluble quantum dots is separated out to wrap the precipitation of the cation precursor when the organic amine is added first so as to prevent the precipitation of the cation precursor from complexing with the organic amine; finally, the solubility of the cationic precursor in the polar solvent is enhanced by adding the polar solvent and complexing the cationic precursor with the organic amine, so that the cationic precursor in the oil-soluble quantum dot mixed solution can be completely removed by fully complexing the cationic precursor with the organic amine, and the oil-soluble quantum dot with higher purity is obtained. The post-treatment method of the oil-soluble quantum dots is simple and feasible in operation flow, almost free of requirements on temperature and atmosphere conditions, good in reproducibility, complete in removal of the cation precursor and capable of being popularized and used on a large scale.
It should be noted that, the obtaining route of the oil-soluble quantum dot mixed solution containing the cation precursor provided in step S1 of the embodiment of the present invention is not specifically limited, and the oil-soluble quantum dot mixed solution of the residual cation precursor directly obtained in the preparation process of the oil-soluble quantum dot may be adopted; the obtained oil-soluble quantum dot can also be dissolved, and then the obtained oil-soluble quantum dot mixed solution containing the cation precursor can be prepared by adding the cation precursor.
In one embodiment, in step S1, the cationic precursor comprises a metal selected from the group consisting of Zn 2+ 、Cd 2+ 、Pb 2+ 、In 3+ At least one of the compounds formed with fatty acid anions including, but not limited to, C n H 2n+1 COO - Or C n H 2n-1 COO - Wherein 11.ltoreq.n.ltoreq.18, such as zinc oleate; and/or the oil-soluble quantum dot mixture includes, but is not limited to, one or more of group II-VI compounds, group III-V compounds, and group IV-VI compounds.
Further in one embodiment, in step S1, the group II-VI compounds include, but are not limited to, one or more of CdSe, cdS, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe, cdZnSTe, cdSeSTe, znSeSTe and CdZnSeSTe; and/or the III-V compounds include, but are not limited to, one or more of InP, inAs, and InAsP; and/or the IV-VI compound includes, but is not limited to, one or more of PbS, pbSe, pbTe, pbSeS, pbSeTe and pbsce.
In one embodiment, in step S2, the volume ratio of the oil-soluble quantum dot mixed solution to the nonpolar solvent is 1:1-5. In the volume ratio range, the nonpolar solvent can sufficiently dilute the oil-soluble quantum dot mixed solution, so that the oil-soluble quantum dot cannot be separated out when the organic amine is added; when the addition amount of the nonpolar solvent is too small and the organic amine is added, the oil-soluble quantum dots are separated out to wrap the precipitation of the cationic precursor, so that the precipitation of the cationic precursor is prevented from complexing with the organic amine; excessive addition of the nonpolar solvent can cause more polar solvent to be consumed when the oil-soluble quantum dots are finally precipitated by the polar solvent, so that the solvent is wasted, and excessive loss of the oil-soluble quantum dots is caused. The oil-soluble quantum dot mixed solution and the nonpolar solvent can be mixed by ultrasonic, stirring, oscillating and other mixing modes; determining mixing time according to the selected mixing mode, and uniformly mixing the two; the temperature of the mixing treatment may be any temperature between room temperature and the boiling point of the nonpolar solvent, and the mixing treatment is performed in an air atmosphere or an inert atmosphere, respectively.
In one embodiment, in step S2, the conditions for mixing the oil-soluble quantum dot mixed solution with the nonpolar solvent are as follows: mixing at 25-200deg.C in inert atmosphere; alternatively, the mixing treatment is carried out in an air atmosphere at 25-150 ℃.
Further in one embodiment, in step S2, the non-polar solvent includes, but is not limited to, at least one of toluene, chloroform, n-hexane, cyclohexane, and chlorobenzene.
In one embodiment, in step S3, the molar ratio of the cationic precursor to the organic amine in the second mixed solution is 1:2-5 (e.g., a molar ratio of 1:2.5, 1:5); within this molar ratio range, the cationic precursor may be completely complexed, while the amount of organic amine does not result in precipitation of oil-soluble quantum dots in the second mixed solution. Excessive amount of organic amine causes raw material waste, and the organic amine has a great threat to the environment; too little does not facilitate adequate complexation of the cationic precursor, resulting in incomplete removal.
In one embodiment, in step S3, the condition of adding the organic amine to the first mixed solution for reaction is: carrying out the reaction under the inert atmosphere of 25-200 ℃; or, carrying out the reaction in an air atmosphere at 25-150 ℃; and/or the reaction time is 2.5S-30min. Wherein the inert atmosphere includes, but is not limited to, a nitrogen atmosphere or an argon atmosphere. Under the reaction conditions, the cationic precursor can be completely complexed, and no oil-soluble quantum dots are precipitated. Namely, when the reaction temperature is more than or equal to 25 ℃ and less than or equal to 150 ℃, the reaction can be carried out in an air atmosphere or an inert atmosphere; when the reaction temperature is 150 ℃ < 200 ℃ (for example, the reaction temperature is 180 ℃), the reaction is carried out under inert atmosphere in order to prevent the oxidation of the oil-soluble quantum dots (such as CdS and CdSe). Further in a preferred embodiment, the conditions for adding an organic amine to the first mixed solution to effect the reaction are: the reaction was carried out in an air atmosphere at 25 ℃ (room temperature). The reaction condition is more economical, convenient and safe.
In still further embodiments, in step S3, the organic amine includes, but is not limited to, at least one of oleylamine, ethylamine, propylamine, butylamine, pentylamine, n-hexylamine, heptylamine, octylamine, decylamine, dodecylamine, hexadecylamine, and octadecylamine. The organic amine can form a relatively stable complex with the cation precursor, and can not be dissociated in the subsequent separation process with the quantum dots; the polarity of the organic amine is weak, and the precipitation of oil-soluble quantum dots can not be caused when the organic amine is added. In a preferred embodiment, the organic amine is oleylamine. Because the complex formed by the oleylamine and the cation precursor has high activity and high stability; meanwhile, the polarity of the quantum dot is relatively weaker, and the influence on precipitation of the oil-soluble quantum dot is small.
In one embodiment, in step S4, the volume ratio of the second mixed solution to the polar solvent is 1:0.1-10. In this volume ratio range, the loss amount of the oil-soluble quantum dot is small, and the oil-soluble quantum dot having high purity can be obtained.
Further in one embodiment, in step S4, the polar solvent includes, but is not limited to, one or more of methanol, ethanol, isopropanol, n-butanol, methyl formate, ethyl formate, methyl acetate, and ethyl acetate. In the polar solvent, a complex formed by combining the cation precursor and the organic amine cannot be dissociated, and the solubility is good; the oil-soluble quantum dots can not be separated out in the process of precipitation, and the effect of complete separation from the oil-soluble quantum dots can be realized.
In one embodiment, in step S4, the purification process includes: centrifuging or filtering, then cleaning the solid, and drying to obtain oil-soluble quantum dots; the solvent used to clean the solids includes, but is not limited to, one or more of methanol, ethanol, isopropanol, n-butanol, methyl formate, ethyl formate, methyl acetate, and ethyl acetate.
The present invention will be described in detail with reference to the following examples.
Example 1 post-treatment of blue-emitting CdSe/ZnSe oil-soluble Quantum dots
(1) Taking 10mL of synthesized CdSe/ZnSe oil-soluble quantum dot original reaction liquid with residual Zn ion precursor and blue light, placing the original reaction liquid into a reaction bottle, wherein the original reaction liquid contains 6mmol of oleic acid, 6mL of 1-octadecene and residual Zn 2+ 2mmol.
(2) Under the air atmosphere, 20mL of normal hexane is added into a reaction bottle, and the mixture is fully stirred until the mixture is uniformly mixed, so as to obtain a first mixed solution.
(3) 5mmol of oleylamine is added into the first mixed solution under the air atmosphere, stirring reaction is carried out for 5s at 150 ℃, and after the reaction is finished, the second mixed solution is obtained at room temperature.
(4) And adding 10mL of ethanol into the second mixed solution, uniformly mixing, performing centrifugal separation, cleaning and drying to obtain the CdSe/ZnSe oil-soluble quantum dot which has no residual Zn ion precursor and emits blue light.
The ultraviolet-visible absorption spectrum and fluorescence spectrum of the blue light-emitting CdSe/ZnSe oil-soluble quantum dot solution of the residual Zn ion precursor are shown in fig. 2a, and the ultraviolet-visible absorption spectrum and fluorescence spectrum of the blue light-emitting CdSe/ZnSe oil-soluble quantum dot solution treated in example 1 are shown in fig. 2b, and the absorption intensity curves of both fig. 2a and 2b are compared and analyzed to see that: when the concentration of the quantum dots is the same (the fluorescence intensity can represent the concentration of the quantum dots because the impurities have no emission peak), the treated CdSe/ZnSe quantum dot solution has smaller absorption intensity; the method shows that the impurity content in the treated CdSe/ZnSe quantum dot is reduced (because the quantum dot and the impurity are absorbed), namely the purity of the treated CdSe/ZnSe quantum dot is higher.
Example 2 post-treatment of Red-emitting CdZnSeS oil-soluble Quantum dots
(1) Taking 10mL of synthesized original reaction liquid of CdZnSeS oil-soluble quantum dots with red light of residual Zn ion precursor, placing the original reaction liquid into a reaction bottle, wherein the original reaction liquid contains 10mmol of oleic acid, 9mL of 1-octadecene and residual Zn 2+ 4mmol.
(2) Under the air atmosphere, 20mL of cyclohexane is added into a reaction bottle, and the mixture is fully stirred until the mixture is uniformly mixed, so as to obtain a first mixed solution.
(3) And under the air atmosphere, adding 20mmol of oleylamine into the first mixed solution, stirring at room temperature for reaction for 30min, and cooling at room temperature after the reaction is finished to obtain a second mixed solution.
(4) And adding 10mL of ethanol into the second mixed solution, uniformly mixing, performing centrifugal separation, cleaning and drying to obtain the CdZnSeS oil-soluble quantum dot capable of emitting red light and free of Zn ion precursor residues.
The ultraviolet-visible absorption spectrum and fluorescence spectrum of the red light-emitting CdZnSeS oil-soluble quantum dot solution of the residual Zn ion precursor are shown in fig. 3a, and the ultraviolet-visible absorption spectrum and fluorescence spectrum of the red light-emitting CdZnSeS oil-soluble quantum dot solution treated in example 2 are shown in fig. 3b, and the absorption intensity curves of both fig. 3a and 3b are compared and analyzed to see that: when the concentration of the quantum dots is the same (the fluorescence intensity can represent the concentration of the quantum dots because the impurities have no emission peak), the CdZnSeS quantum dot solution after treatment has smaller absorption intensity; the method shows that the impurity content in the treated CdZnSeS quantum dot is reduced (because the quantum dot and the impurity are absorbed), namely the purity of the treated CdZnSeS quantum dot is higher.
In summary, the present invention provides a post-treatment method for oil-soluble quantum dots, specifically, the method comprises diluting the oil-soluble quantum dot mixed solution with a nonpolar solvent, and then complexing with an organic amine and an unreacted cation precursor; avoiding that the precipitation of the oil-soluble quantum dots is separated out to wrap the precipitation of the cation precursor when the organic amine is added first so as to prevent the precipitation of the cation precursor from complexing with the organic amine; finally, the solubility of the cationic precursor in the polar solvent is enhanced by adding the polar solvent and complexing the cationic precursor with the organic amine, so that the cationic precursor in the oil-soluble quantum dot mixed solution can be completely removed by fully complexing the cationic precursor with the organic amine, and the oil-soluble quantum dot with higher purity is obtained. The post-treatment method of the oil-soluble quantum dots has the advantages of simple and easy operation flow, almost no requirement on temperature and atmosphere conditions, good reproducibility, complete removal of the cation precursor and large-scale popularization and application.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (6)
1. The post-treatment method of the oil-soluble quantum dot is characterized by comprising the following steps of:
providing an oil-soluble quantum dot mixed solution containing a cation precursor;
mixing the oil-soluble quantum dot mixed solution with a nonpolar solvent to obtain a first mixed solution;
adding organic amine into the first mixed solution for reaction to obtain a second mixed solution;
adding a polar solvent into the second mixed solution, and purifying to obtain the oil-soluble quantum dot;
the conditions for adding the organic amine into the first mixed solution for reaction are as follows: carrying out the reaction under the inert atmosphere of 25-200 ℃; or, carrying out the reaction in an air atmosphere at 25-150 ℃; the volume ratio of the oil-soluble quantum dot mixed solution to the nonpolar solvent is 1:1-5; in the second mixed solution, the molar ratio of the cationic precursor to the organic amine is 1:2-5; the volume ratio of the second mixed solution to the polar solvent is 1:0.1-10.
2. The post-treatment method according to claim 1, wherein the nonpolar solvent comprises at least one of toluene, chloroform, n-hexane, cyclohexane and chlorobenzene.
3. The aftertreatment method of claim 1, wherein the organic amine comprises at least one of oleylamine, ethylamine, propylamine, butylamine, pentylamine, n-hexylamine, heptylamine, octylamine, decylamine, dodecylamine, hexadecylamine, and octadecylamine.
4. The aftertreatment method of claim 1, wherein the polar solvent comprises one or more of methanol, ethanol, isopropanol, n-butanol, methyl formate, ethyl formate, methyl acetate, and ethyl acetate.
5. The aftertreatment method of claim 1, wherein the cationic precursor comprises a metal selected from the group consisting of Zn 2+ 、Cd 2+ 、Pb 2+ 、In 3+ And fatAt least one of the compounds formed by fatty acid anions including C n H 2n+ 1 COO-or C n H 2n-1 COO - Wherein n is more than or equal to 11 and less than or equal to 18; and/or
The oil-soluble quantum dot mixed solution comprises one or more of II-VI compounds, III-V compounds and IV-VI compounds.
6. The post-treatment process of claim 5, wherein the group II-VI compound comprises one or more of CdSe, cdS, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe, cdZnSTe, cdSeSTe, znSeSTe and CdZnSeSTe; and/or
The III-V compounds include one or more of InP, inAs, and InAsP; and/or the IV-VI compound comprises one or more of PbS, pbSe, pbTe, pbSeS, pbSeTe and pbsce.
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