CN114316949B - Preparation method of quantum dot material, quantum dot material and application - Google Patents
Preparation method of quantum dot material, quantum dot material and application Download PDFInfo
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- CN114316949B CN114316949B CN202210030909.6A CN202210030909A CN114316949B CN 114316949 B CN114316949 B CN 114316949B CN 202210030909 A CN202210030909 A CN 202210030909A CN 114316949 B CN114316949 B CN 114316949B
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Abstract
The invention discloses a preparation method of a quantum dot material, the quantum dot material and application, and relates to the technical field of optical display. The preparation method of the quantum dot material comprises the following steps: blending and extruding the capsules loaded with the anion precursor and the cation precursor and the plastic master batch; wherein the capsule is provided with at least two independent loading cavities, the anion precursor and the cation precursor are loaded in different loading cavities, and the melting point of the material adopted by the capsule is lower than the temperature of blending extrusion. The anion precursor and the cation precursor are not mixed before blending and extrusion, and the capsule is melted during blending and extrusion to contact the anion precursor and the cation precursor for reaction to generate the quantum dot. By adopting the process provided by the embodiment of the invention, the quantum dot material with higher quality can be prepared, the half-peak width is narrower, and the quantum yield is higher. In addition, by adopting the process provided by the embodiment of the invention, the capsules capable of synthesizing quantum dots with different colors can be simultaneously blended and extruded to prepare the quantum dots containing multiple colors.
Description
Technical Field
The invention relates to the technical field of optical display, in particular to a preparation method of a quantum dot material, the quantum dot material and application.
Background
The quantum dots are quasi-zero-dimensional semiconductor nanocrystals with the size radius smaller than or equal to the radius of the bol exciton, and are widely applied to the fields of biomedical marking, solar cells, illumination, display and the like due to the properties of continuous adjustability of fluorescence emission wavelength, high quantum yield, narrow half-peak width and the like.
At present, the main application form of quantum dots in the field of photoelectric display is quantum dot optical diffusion plates. The device is formed by blending and extruding the prepared quantum dot material and the plastic master batch at a high temperature, so that the quantum dot material is dispersed in a common diffusion plate, and due to the excellent optical property of the quantum dot, the display color gamut can be remarkably improved, and the display energy consumption is reduced.
However, in the prior art, a quantum dot material is synthesized, then is separated and purified, and finally is blended with plastic master batches and extruded. The process flow is long and complex, and the quantum dots are not uniformly dispersed in the diffusion plate. In addition, the quantum dots synthesized by the prior art generally have the problems of non-ideal half-peak width and quantum yield.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of a quantum dot material, the quantum dot material and application, and aims to improve the quality of prepared quantum dots and obtain a product with lower half-peak width and higher quantum yield.
The invention is realized by the following steps:
in a first aspect, the present invention provides a method for preparing a quantum dot material, comprising:
blending and extruding the capsules loaded with the anion precursor and the cation precursor and the plastic master batch so as to react the anion precursor and the cation precursor to obtain quantum dots;
wherein the capsule is provided with at least two independent loading cavities, the anion precursor and the cation precursor are loaded in different loading cavities, and the melting point of the material adopted by the capsule is lower than the temperature of blending extrusion.
In alternative embodiments, both the anionic precursor and the cationic precursor are selected from at least one of group II-VI compounds, group III-V compounds, group IV-VI compounds, group II-III-IV compounds, and group I-II-IV-VI compounds;
preferably, the group II-VI compound is selected from at least one of CdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, mgSe, mgS, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, mgZnSe, mgZnS, hgZnTeS, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeTe, cdHgSTe, hgZnSeS, HZnSgZnSeTe and HgHgTe;
the III-V compound is selected from at least one of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaGaGaAs, gaSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlN, inNAs, inAsInSb, inAPAs, and InPSb;
the group IV-VI compound is at least one selected from SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe and SnPbSTe;
the II-III-IV group compound is at least one selected from CuInSe2, cuInS2, cuInGaSe and CuInGaS;
the I-II-IV-VI compound is at least one selected from CuZnSnSe and CuZnSnS.
In an alternative embodiment, the types and ratios of the cationic precursors in the capsules are adjusted to classify the capsules for the blend extrusion into different color types.
In an alternative embodiment, the capsule includes a first capsule for synthesizing green quantum dots and a second capsule for synthesizing red quantum dots.
In an alternative embodiment, the capsule has 2 independent loading chambers, and the anion precursor and the cation precursor are loaded in 1 independent loading chamber, respectively.
In an alternative embodiment, the capsule has separate left and right chambers.
In an alternative embodiment, the capsule has a separate inner chamber and an outer chamber that encases the inner chamber.
In an alternative embodiment, the extrusion temperature of the blending extrusion is 220 to 350 ℃;
preferably, the capsule and the plastic master batch are both made of polystyrene.
In a second aspect, the present invention provides a quantum dot material prepared by the preparation method of any one of the preceding embodiments.
In a third aspect, the present invention provides the use of the quantum dot material of the previous embodiments in the manufacture of a display.
The invention has the following beneficial effects: the anion precursor and the cation precursor are respectively loaded in different loading cavities of the capsule, so that the anion precursor and the cation precursor are not mixed before blending extrusion, the capsule is melted during blending extrusion, the anion precursor and the cation precursor are contacted, and the quantum dots are generated through reaction. By adopting the process provided by the embodiment of the invention, the quantum dot material with higher quality can be prepared, the half-peak width is narrower, and the quantum yield is higher.
In addition, by adopting the process provided by the embodiment of the invention, the capsules capable of synthesizing quantum dots with different colors can be simultaneously blended and extruded to prepare the quantum dots containing multiple colors.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
Fig. 1 is a schematic diagram of a capsule in a preparation method provided by an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a preparation method of a quantum dot material, which comprises the following steps:
s1, preparation of precursor capsules
The capsule is provided with at least two independent loading cavities, the anion precursor and the cation precursor are loaded in different loading cavities, and the melting point of the material adopted by the capsule is lower than the blending extrusion temperature, so that the capsule is melted during blending extrusion, and the anion precursor and the cation precursor are mixed and react to obtain the quantum dots.
In particular, the number of loading chambers on the capsule is not limited, and can be 2, 3, 4, etc. The material of the loading cavity is common high polymer material, and can be the same as the material of the plastic master batch.
It should be noted that the capsule having the independent loading chamber can be prepared by the existing preparation method, and is not limited herein. In some embodiments, capsules with independent loading chambers may be prepared by: generating microcapsules by emulsion polymerization of precursors and monomers for forming the microcapsules; the capsule structure is manufactured by the extrusion and injection molding processes of plastics, and the anion and cation precursors are injected into the capsule.
In some embodiments, the capsule has 2 independent loading chambers, and the anion precursor and the cation precursor are loaded in 1 independent loading chamber, respectively. The left chamber and the right chamber can be independent, or the inner chamber and the outer chamber in fig. 1 can be inner chambers and outer chambers which are covered in the inner chambers.
The present invention is not particularly limited in the kind of the anion precursor and the cation precursor, and it is understood that the anion precursor and the cation precursor correspond to each other and can react with each other to form the quantum dot material.
Specifically, the anionic precursor and the cationic precursor are each selected from at least one of group II-VI compounds, group III-V compounds, group IV-VI compounds, group II-III-IV compounds, and group I-II-IV-VI compounds; preferably, the group II-VI compound is selected from at least one of CdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, mgSe, mgS, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, mgZnSe, mgZnS, hgZnTeS, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeTe, cdHgSTe, hgZnSeS, HZnSgZnSeTe and HgHgTe; the III-V compound is selected from at least one of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaGaGaAs, gaSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlN, inNAs, inAsInSb, inAPAs, and InPSb; the group IV-VI compound is at least one selected from SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe and SnPbSTe; the II-III-IV group compound is at least one selected from CuInSe2, cuInS2, cuInGaSe and CuInGaS; the I-II-IV-VI compound is at least one selected from CuZnSnSe and CuZnSnS.
It should be noted that, a person skilled in the art can select specific substances contained in the first precursor and the second precursor according to different target materials.
Furthermore, the capsules for blending extrusion are divided into different color types by regulating the types and the proportion of the cation precursors in the capsules, so that quantum dots with different colors can be synthesized in the one-step blending extrusion process, and the problem that only one type of quantum dots can be prepared by one-step blending extrusion in the prior art is solved.
In some embodiments, the capsules include a first capsule for synthesizing green quantum dots and a second capsule for synthesizing red quantum dots. The green quantum dots and the red quantum dots are the most common materials for preparing the optical diffusion plate, the anion and cation precursors adopted by the green quantum dots and the red quantum dots can refer to the prior art, and are not specifically limited herein, and the technical scheme in the prior art for synthesizing the green quantum dots and the red quantum dots is within the protection scope of the application.
It should be noted that the conventional precursors for synthesizing green quantum dots and red quantum dots are within the scope of the present application.
In some embodiments, the cation precursor in both the first and second capsules comprises a solvent, a zinc precursor, and a cadmium precursor; the dosage ratio of the zinc precursor to the cadmium precursor in the first capsule is controlled to be 4.5-5.5; the dosage ratio of the zinc precursor and the cadmium precursor in the second capsule is controlled to be 0.5-1.5. By controlling the proportion of zinc and cadmium adopted in the first capsule and the second capsule, the quantum dots of the final product are green and red.
Specifically, the molar ratio of zinc ions to cadmium ions in the first capsule can be controlled to be 4.5; the molar ratio of zinc ions to cadmium ions in the second capsule can be controlled to be 0.5.
Specifically, the zinc precursor is selected from one or more of TOP-Se, TBP-Se and ODE-Se; the cadmium precursor is selected from one or more of cadmium-containing precursors such as cadmium oxide, cadmium stearate, cadmium oleate and the like; the solvent is at least one selected from octadecene, TOPO, liquid paraffin and TOA. The types of the zinc precursor, the cadmium precursor and the solvent may be one or more, and are not limited herein.
It should be noted that the above precursor is only limited by way of example, and can be any raw material for synthesizing CdSe/ZnS quantum dot materials.
In some embodiments, the cationic precursor in both the first capsule and the second capsule comprise a ligand; the ligand is at least one selected from unsaturated fatty acid, alkyl mercaptan, fatty amine, fatty acid and phosphonic acid. The ligand may be one or more of the above, and is not limited herein, and may be selected according to the group requirement required for the reaction.
In some embodiments, the anion precursor in the first capsule and the anion precursor in the second capsule each comprise a sulfur precursor and a selenium precursor, and the dosage ratio of the sulfur precursor to the selenium precursor is controlled to be 1 to 0.5 molar ratio of sulfur ions to selenium ions; preferably 1; specifically, the molar ratio of the sulfide ion to the selenide ion may be 1.
Generally, the precursor of the anions and cations in one capsule is a reaction unit, the concentration of the ions is not limited, but the concentration of the anions and cations meets the proportion requirement of the anions and cations in the reaction.
Specifically, the sulfur precursor is selected from at least one of S-ODE, S-TOP and S-OA; the selenium precursor is at least one selected from Se-ODE, se-TOP and Se-OA. The types of common sulfur precursors and selenium precursors are suitable for the methods provided by the embodiments of the present invention, and the above are examples of common anion precursors, and the types of the anion precursors are not limited to the above.
S2, blending and extruding
And (3) blending and extruding the capsules loaded with the anion precursor and the cation precursor and the plastic master batch, wherein the extrusion temperature of blending and extruding is 220-350 ℃. During blending and extrusion, the capsule is melted, and the anion precursor and the cation precursor are contacted and react to generate the quantum dot.
Specifically, the temperature of the blending and extrusion may be 220 ℃, 230 ℃, 240 ℃,250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃, 350 ℃ or the like, or may be any value between the above adjacent temperature values.
In some embodiments, the capsule and the plastic masterbatch are made of Polystyrene (PS). The material of the capsule is close to the extrusion temperature, and can be the same as the plastic master batch.
The quantum dot material is prepared by the preparation method, has a narrow half-peak width and a high quantum yield, and can be further prepared into a display.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a quantum dot material, which comprises the following steps:
(1) Preparing a microcapsule structure: the microcapsule structure (the capsule material is polystyrene PS) in fig. 1 is prepared by melting polystyrene at high temperature, injecting into a mold for preparing the capsule, and cooling to obtain the final product. The volume of the inner chamber was 0.2mL and the volume of the outer chamber was 3mL.
(2) Preparation of the first capsule: the cationic precursor and the anionic precursor are injected into the outer layer chamber and the inner layer chamber of the microcapsule structure, respectively. The composition of the cation precursor is as follows: 2mL of Octadecene (ODE), 0.25mL of oleic acid, 0.125mmol of zinc oxide, and 0.025mmol of cadmium oxide. The composition of the anion precursor is as follows: 0.075mL of TOP-S (1 mmol/mL), 0.075mL of TOP-Se (1 mmol/mL).
(3) Preparation of the second capsule: the cation precursor and the anion precursor are injected into the outer layer chamber and the inner layer chamber of the microcapsule structure respectively. The composition of the cation precursor is as follows: 2mL Octadecene (ODE), 0.25mL oleic acid, 0.075mmol zinc oxide, and 0.075mmol cadmium oxide. The composition of the anion precursor is as follows: 0.075mL of TOP-S (1 mmol/mL), 0.075mL of Se-TOP (1 mmol/mL).
(4) Blending and extruding: mixing 1kg of PS master batch with 50 first capsules and 15 second capsules, adding the mixture into a micro extruder, and blending and extruding at a high temperature of 250 ℃ to obtain the quantum dot optical diffusion plate.
Example 2
The only difference from example 1 is: the temperature of the high-temperature blending extrusion is 220 ℃.
Example 3
The only difference from example 1 is: the temperature of the high-temperature blending extrusion is 280 ℃.
Comparative example 1
The present comparative example provides a method of preparing a quantum dot material without using a capsule structure to separate a cation precursor and an anion precursor prior to extrusion, comprising the steps of: and mixing the components in the cation precursor to obtain a first mixture, adding the anion precursor into the first mixture, adding the obtained mixture into a micro extruder, and performing high-temperature blending extrusion at 250 ℃ to obtain the quantum dot optical diffusion plate.
Wherein, the composition of the cation precursor and the anion precursor is referred to the composition of the first capsule in example 1.
Comparative example 2
The present comparative example provides a method of preparing a quantum dot material that does not employ a capsule structure to separate a cationic precursor and an anionic precursor prior to extrusion, comprising the steps of: and mixing the components in the cation precursor to obtain a first mixture, adding the anion precursor into the first mixture, adding the obtained mixture into a micro extruder, and performing high-temperature blending extrusion at 250 ℃ to obtain the quantum dot optical diffusion plate.
Wherein the composition of the cation precursor and the anion precursor is referred to the composition of the second capsule in example 1.
Test example 1
The performance of the quantum dot optical diffusion plates prepared in the test examples and comparative examples was measured, and the wavelength, half-peak width and quantum yield were measured by a conventional method, and the results are shown in table 1.
TABLE 1 Performance test results for Quantum dot materials
As can be seen from table 1, the quantum dot material prepared by the method provided in the embodiment of the present invention has better performance, smaller half-peak width and higher quantum yield.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a quantum dot material is characterized by comprising the following steps:
blending and extruding a capsule loaded with an anion precursor and a cation precursor and a plastic master batch so as to enable the anion precursor and the cation precursor to react to obtain quantum dots;
wherein the capsule is provided with at least two independent loading cavities, the anion precursor and the cation precursor are loaded in the different loading cavities, and the melting point of the material adopted by the capsule is lower than the temperature of the blending extrusion;
the compound formed by the reaction of the anionic precursor and the cationic precursor is at least one selected from the group consisting of group II-VI compounds, group III-V compounds, group IV-VI compounds, group II-III-IV compounds, and group I-II-IV-VI compounds.
2. A method for producing a quantum dot material according to claim 1, wherein the group II-VI compound is selected from at least one of CdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, mgSe, mgS, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnSe, hgZnTe, mgZnSe, mgZnS, hgZnTeS, cdzneses, cdZnSeTe, cdZnSTe, cdHgSeS, cdhghte, hghtsns, hgesete, cdSe/ZnS, and ggznte;
the III-V compound is at least one selected from the group consisting of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaGaGaAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inNP, inAlN, inNAs, inNSb, inAPAs, and InAlPSb;
the group IV-VI compound is at least one selected from SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe and SnPbSTe;
the II-III-IV group compound is at least one selected from CuInSe2, cuInS2, cuInGaSe and CuInGaS;
the I-II-IV-VI compound is at least one of CuZnSnSe and CuZnSnS.
3. The method for preparing quantum dot material according to claim 2, wherein the kind and ratio of the cation precursor in the capsule are adjusted to classify the capsule for blending extrusion into different color types.
4. The method of claim 3, wherein the capsules comprise a first capsule for synthesizing green quantum dots and a second capsule for synthesizing red quantum dots.
5. The method of claim 1, wherein the capsule has 2 independent loading chambers, and the anion precursor and the cation precursor are loaded in 1 independent loading chamber respectively.
6. The method of claim 5, wherein the capsule has a left chamber and a right chamber which are independent.
7. The method of claim 5, wherein the capsule has a separate inner chamber and an outer chamber surrounding the inner chamber.
8. The method for preparing the quantum dot material according to any one of claims 1 to 7, wherein the extrusion temperature of the blending extrusion is 220-350 ℃.
9. The method for preparing the quantum dot material according to claim 8, wherein the capsule and the plastic master batch are both made of polystyrene.
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