CN111410961A - Nanocrystalline and nanocrystalline preparation method - Google Patents
Nanocrystalline and nanocrystalline preparation method Download PDFInfo
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
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- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 description 1
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- OUMZKMRZMVDEOF-UHFFFAOYSA-N tris(trimethylsilyl)phosphane Chemical compound C[Si](C)(C)P([Si](C)(C)C)[Si](C)(C)C OUMZKMRZMVDEOF-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/088—Other phosphides containing plural metal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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Abstract
The invention provides a nanocrystal and a preparation method thereof. The nanocrystal comprises a first nanostructure and a plurality of second nanostructures, wherein the first nanostructure is InZnP/ZnSe, the second nanostructure is ZnS, the second nanostructures surround the first nanostructure, at least one part of the second nanostructures are not connected with the first nanostructure, at least one part of the second nanostructures are connected with the first nanostructure, and the plurality of second nanostructures cover the surface of at least one part of the first nanostructure. The nanocrystalline has a flower shape, and is more beneficial to the design of the surface structure and the optimization of the light-emitting performance. Meanwhile, the method for preparing the nanocrystalline is simple and controllable, and the prepared nanocrystalline is good in dispersion, uniform in size and good in performance.
Description
Technical Field
The invention relates to the technical field of nanocrystals, in particular to a nanocrystal and a preparation method thereof.
Background
The physical and chemical properties of the nano-materials have a close relationship with the morphology and size of the nano-materials, so that the research of the nano-materials is concerned. The nanoflower has unique performance due to the fact that the nanoflower has a multi-branch structure and a rough surface, and therefore has wide application prospects in the fields of catalysis, photoelectronic devices, biological marking and detection, surface-enhanced Raman scattering, photothermal therapy and the like. Such as gold nanoflowers described in CN108500293A, ZnO nanoflowers described in CN105036180A, CdS nanoflowers described in CN107043124A, etc.
In recent years, the research of II-VI group-based nano materials containing CdSe, CdS and the like is greatly advanced, the efficiency, half-peak width, stability and other properties of the nano materials are greatly improved, and the nano materials are applied to the fields of display, biology, catalysis and the like. However, since Cd is a toxic heavy metal, the european union "legislation on chemical registration, evaluation, permission and restriction" (REACH for short) strictly regulates the Cd content in goods entering its market, and its wide application is limited, so people's research on environment-friendly cadmium-free nanocrystals has never been abandoned. In cadmium-free nanocrystals, III-V group InP-based quantum dots become a hotspot for research, and are expected to replace Cd-containing based nanocrystals.
Disclosure of Invention
The invention mainly aims to provide a method for simply preparing cadmium-free flower-shaped InZnP/ZnSe/ZnS nanocrystals and the flower-shaped InZnP/ZnSe/ZnS nanocrystals which have good dispersion, uniform size and good performance and are simple and controllable.
In order to achieve the above object, according to one aspect of the present invention, there is provided a nanocrystal comprising a first nanostructure and a plurality of second nanostructures, the first nanostructure being InZnP/ZnSe, the second nanostructure being ZnS, the second nanostructure surrounding the first nanostructure, and at least a portion of the second nanostructure not being connected to the first nanostructure, and at least a portion of the second nanostructure being connected to the first nanostructure, the plurality of second nanostructures covering at least a portion of a surface of the first nanostructure.
Further, at least two second nanostructures in the plurality of second nanostructures are connected with each other, and preferably, the fluorescence peak wavelength of the nanocrystal is in a range of 610-630 nm.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1.
According to an aspect of the present invention, there is provided a method for preparing a nanocrystal, comprising the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc and the first non-coordination solvent in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a container at a second temperature, reacting for a certain time, adding a first long-chain fatty acid, then adding a Se precursor into the container at the second temperature, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1.
According to an aspect of the present invention, there is provided a method for preparing a nanocrystal, comprising the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the adding amount of the Se precursor and the adding amount of the S precursor is less than 1.
According to an aspect of the present invention, there is provided a method for preparing a nanocrystal, comprising the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a first container at a first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordinating solvent to obtain an InZnP/ZnSe nanocrystalline solution; s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding an InZnP/ZnSe nanocrystal solution into a second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1.
According to an aspect of the present invention, there is provided a method for preparing a nanocrystal, comprising the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a first container at a first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordinating solvent to obtain an InZnP/ZnSe nanocrystalline solution; s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding an InZnP/ZnSe nanocrystal solution into a second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the adding amount of the Se precursor and the adding amount of the S precursor is less than 1.
In any of the above nanocrystal preparation methods, further, the molar ratio of the amount of the Se precursor added to the amount of the S precursor added is 1:2.7 to 1: 96.
In any of the above methods for preparing a nanocrystal, the first temperature is 200 to 220 ℃, the second temperature is 300 to 320 ℃, the third temperature is 300 to 320 ℃, and the fourth temperature is 230 to 250 ℃.
In any of the above nanocrystal preparation methods, further, each short chain fatty acid zinc is independently selected from one or more of fatty acid zinc having a C atom number of less than 8, and each long chain fatty acid is independently selected from one or more of fatty acid having a C atom number of greater than 8.
In any of the above nanocrystal preparation methods, further, the Se precursor is one or more of Se-TBP, Se-TOP and Se-ODE, and the S precursor is one or more of S-TBP, S-TOP and S-ODE.
By applying the technical scheme of the invention, the flower-shaped nanocrystalline is more beneficial to the design of the surface structure and the optimization of the light-emitting performance. Meanwhile, the method for preparing the flower-shaped nanocrystal is simple and controllable, and the prepared flower-shaped nanocrystal is good in dispersion, uniform in size and good in performance.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a transmission electron micrograph of a nanocrystal obtained in example 1 of the present application;
FIG. 2 is a transmission electron micrograph of a nanocrystal obtained in example 2 of the present application;
FIG. 3 is a transmission electron micrograph of a nanocrystal obtained in example 3 of the present application;
FIG. 4 is a transmission electron micrograph of a nanocrystal obtained in example 4 of the present application;
FIG. 5 is a transmission electron micrograph of nanocrystals obtained in example 5 of the present application;
FIG. 6 is a transmission electron micrograph of a nanocrystal obtained in example 6 of the present application;
FIG. 7 is a transmission electron micrograph of an intermediate nanocrystal obtained in example 7 of the present application;
FIG. 8 is a transmission electron micrograph of a nanocrystal obtained in example 7 of the present application; and
FIG. 9 is a transmission electron micrograph of nanocrystals obtained in comparative example 1 of the present application.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. "/" represents a core-shell structure as understood by those skilled in the art.
The terms "comprises," "comprising," and "having," and any variations thereof, in the description and claims of this application, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In an exemplary embodiment of the present application, there is provided a nanocrystal comprising a first nanostructure and a plurality of second nanostructures, the first nanostructure being InZnP/ZnSe, the second nanostructure being ZnS, the second nanostructures surrounding the first nanostructure, and at least a portion of the second nanostructures not being connected to the first nanostructure, and at least a portion of the second nanostructures being connected to the first nanostructure, the plurality of second nanostructures covering at least a portion of a surface of the first nanostructure. The shape of the observed nanocrystal on a two-dimensional plane is similar to a flower and comprises a flower core and petals, for convenience of description, flower-shaped quantum dots are hereinafter referred to, and the specific structure is based on the character description. From the structural point of view, the surface of the nanocrystalline is coated with ZnSe and ZnS, so that the outer layer structure can be adjusted, and the outer shell layer is different from the prior art only containing ZnSe or ZnS or ZnSeS alloy. In addition, the petal-shaped nanocrystals form the outer surface similar to a fold, the surface area of the petal-shaped nanocrystals is larger, and the petal-shaped nanocrystals have better application prospects in the fields of catalysis, loading and the like. On the aspect of luminous performance, the nanocrystalline effectively forms flower cores of InZnP/ZnSe and petals of ZnS, the design of the energy band is similar to that of the prior art, but different compositions of the surface of the nanocrystalline can influence exciton transmission and recombination, and the surface defects of the nanocrystalline can be adjusted.
In some embodiments, at least two of the plurality of second nanostructures are connected to each other. It is understood that there is a phenomenon of a connection between at least a portion of the second nanostructures. In some embodiments, the nanocrystals have a peak fluorescence emission wavelength in the range of 610 to 630 nm. In some embodiments, the nanocrystals have a peak fluorescence emission wavelength ranging from 622 to 630 nm. In some embodiments, the quantum yield of the nanocrystals is 44-53%. In some embodiments, the nanocrystals have a half-peak width of 38 to 43 nm. The luminous performance of the flower-shaped nanocrystal is close to the existing level, but the flower-shaped nanocrystal is more beneficial to the design of the surface structure and the optimization of the luminous performance, and a new development idea is provided for the existing cadmium-free nanocrystal.
In a first exemplary embodiment of the present application, there is provided a method for preparing a nanocrystal, including the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1. The prepared nanocrystal is flower-shaped quantum dots, and has good dispersibility and uniform size. Meanwhile, the preparation method has simple process.
In a second exemplary embodiment of the present application, there is provided a method for preparing a nanocrystal, including the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc and the first non-coordination solvent in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a container at a second temperature, reacting for a certain time, adding a first long-chain fatty acid, then adding a Se precursor into the container at the second temperature, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1. The prepared nanocrystal is flower-shaped quantum dots, and has good dispersibility and uniform size. Meanwhile, the preparation method has simple process.
In a third exemplary embodiment of the present application, there is provided a method for preparing a nanocrystal, including the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure; s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the adding amount of the Se precursor and the adding amount of the S precursor is less than 1. The prepared nanocrystal is flower-shaped quantum dots, and has good dispersibility and uniform size. Meanwhile, the preparation method has simple process.
In a fourth exemplary embodiment of the present application, there is provided a method for preparing a nanocrystal, including the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a first container at a first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordinating solvent to obtain an InZnP/ZnSe nanocrystalline solution; s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding an InZnP/ZnSe nanocrystal solution into a second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the molar ratio of the Se precursor to the S precursor is less than 1. The prepared nanocrystal is flower-shaped quantum dots, and has good dispersibility and uniform size. Meanwhile, the preparation method has simple process.
In a fifth exemplary embodiment of the present application, there is provided a method for preparing a nanocrystal, including the steps of: s1, preparing an InZnP nanocrystalline solution; s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding an InZnP nanocrystalline solution into a first container at a first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordinating solvent to obtain an InZnP/ZnSe nanocrystalline solution; s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding an InZnP/ZnSe nanocrystal solution into a second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction; wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the adding amount of the Se precursor and the adding amount of the S precursor is less than 1. The prepared nanocrystal is flower-shaped quantum dots, and has good dispersibility and uniform size. Meanwhile, the preparation method has simple process.
In any of the above exemplary embodiments, the inventors speculate from the experimental results that the key to the formation of the flower-like quantum dots is that the molar ratio of the added amounts of the Se precursor and the S precursor is less than 1, possibly because the growth rates of different crystal planes are different, thereby obtaining anisotropic nanocrystals. Specifically, in the quantum dot shell coating, the adding amount of the Se precursor is less than that of the S precursor, so that the ZnS layer coating amount is easily large, part of crystal faces grow fast, other crystal faces grow slow, and flower-shaped nanocrystals are finally formed.
In some embodiments, the first short chain fatty acid zinc and the second short chain fatty acid zinc can be the same or different.
In some embodiments, the first non-coordinating solvent, the second non-coordinating solvent, and the third non-coordinating solvent may be the same or different. Octadecene, which is common in the art, can be used as a coordinating solvent.
In some embodiments, the first long chain fatty acid, the second long chain fatty acid, the third long chain fatty acid may be the same or different.
In some embodiments, the molar ratio of Se precursor addition to S precursor addition is from 1:2.7 to 1: 96.
In some embodiments, the first temperature is lower than the second temperature, the third temperature, and the fourth temperature. Considerations for the second temperature, the third temperature, and the fourth temperature include the reaction rate and the volatility of the reaction medium (typically below the boiling point of the reaction medium).
In some embodiments, the fourth temperature is greater than the first temperature but less than the third temperature.
In some embodiments, the first temperature is 200 to 220 ℃, the second temperature is 300 to 320 ℃, the third temperature is 300 to 320 ℃, and the fourth temperature is 230 to 250 ℃.
In some embodiments, the first temperature, the second temperature, the third temperature, and the fourth temperature are all constant temperatures.
In some embodiments, each short chain fatty acid zinc is independently selected from one or more of fatty acids with a C atom number less than 8, and each long chain fatty acid is independently selected from one or more of fatty acids with a C atom number greater than 8.
In some embodiments, the Se precursor is one or more of Se-TBP, Se-TOP and Se-ODE and the S precursor is one or more of S-TBP, S-TOP and S-ODE.
In some embodiments, the reaction is terminated, and then the nanocrystalline solution is cooled and purified, and the nanocrystalline solution is extracted, precipitated and redissolved in sequence; in some embodiments, the extraction solvent used for extraction is selected from alcohols such as methanol, ethanol, butanol, etc.; in some embodiments, the precipitation is performed with ketones such as acetone, butanone, and the like; in some embodiments, the redissolution is carried out using an organic solvent such as octadecene, n-octane, n-butane, and the like.
The advantageous effects of the present application will be further described with reference to specific examples.
Oleic acid is abbreviated as OA, trioctylamine is abbreviated as TOA, tributylphosphine is abbreviated as TBP, 1-octadecene is abbreviated as ODE, trioctylphosphine is abbreviated as TOP, the absorbance is abbreviated as OD, and the OD450nm refers to the absorbance measured at 450nm and represents the concentration of the quantum dots.
Preparing a nanocrystal core:
synthesis of InZnP nanocrystal core: adding 0.3mmol of In (Ac)3(indium acetate), 0.1mmol of Zn (Ac)2(Zinc acetate), 1.2mmol of myristic acid and 10.0g of octadecene were charged into a 100m L three-necked flask2Heating to 180 ℃ in an exhaust state, keeping the temperature at 180 ℃ for 30min, cooling to room temperature, quickly injecting a mixed solution of 0.15mmol of TMS-P (tri (trimethylsilyl) phosphine) and 0.3mmol of trioctylamine, heating to 300 ℃, and reacting at 300 ℃ for 5min to obtain an InZnP nuclear solution; and keeping the reaction temperature at 300 ℃, and continuously replenishing the P precursor and the In precursor or replenishing the InZnP cluster to continuously grow the InZnP nucleus to a required position. Extracting twice with methanol, precipitating with acetone, centrifuging, and dissolving the precipitate in ODE to obtain the InZnPS nanocrystal solution.
Example 1(Se/S ═ 1:10)
A50 m L flask was charged with 4mmol Zn (Ac)210g of ODE, exhausting at 200 ℃ for 35min, heating to 300 ℃, injecting nanocrystal core with OD450nm being 50, injecting 5mmol of OA after reacting for 15min, injecting 0.4mmol of Se/TBP (with the concentration of 0.5M) when the temperature rises to 300 ℃, injecting 4mmol of S/TBP (with the concentration of 4M) after 15min, reacting for 30min, cooling and purifying. The obtained nanocrystalline is in flower shape and has uniform size distribution as shown in figure 1.
Example 2(Se/S ═ 1:96)
A50 m L flask was charged with 4mmol Zn (Ac)210g of ODE, exhausting at 220 ℃ for 35min, heating to 320 ℃, injecting nanocrystal core with OD450nm being 50, injecting 3mmol of OA after reacting for 15min, injecting 0.5mmol of Se/TBP (0.5M) when the temperature rises to 320 ℃, injecting 3mmol of OA after 15min, adding 4.8mmol of S/TBP (the concentration is 4M) when the temperature returns to 320 ℃, reacting for 30min, and cooling and purifying. The obtained nanocrystalline is in flower shape and has uniform size distribution as shown in figure 2.
Example 3(TOA, Se/S ═ 1:4)
A50 m L flask was charged with 4.0mmol Zn (Ac)24.5mmol TOA, 16.4mmol OA, 4.0g ODE, exhausting at 200 ℃ for 35min, heating to 320 ℃, injecting nanocrystal core with OD450nm being 50, immediately injecting 0.4mmol Se-TBP (with concentration being 1.0mmol/m L), reacting for 60min, injecting 1.6mmol S-TBP (with concentration being 2.0mmol/m L) at 320 ℃, heating to 320 ℃, reacting for 45min, cooling and purifying, and obtaining the nanocrystal which is flower-shaped and has more uniform size distribution, as shown in an electron microscope picture of the obtained nanocrystal, and the nanocrystal is prepared by the method.
Example 4(Se/S ═ 1:3.3)
A50 m L flask was charged with 4.5mmol Zn (Ac)216.4mmol OA, 4.0g ODE, exhausting at 220 ℃ for 35min, raising the temperature to 320 ℃, injecting 0.3mmol Se-TBP (with the concentration of 1.0mmol/m L) immediately after injecting nanocrystal core with OD450nm being 50, raising the temperature to 320 ℃, reacting for 60min, injecting 1.0mmol S-TBP (with the concentration of 2.0mmol/m L) at 316 ℃, raising the temperature to 320 ℃, reacting for 45min, and cooling and purifying to obtain the nanocrystal, wherein the nanocrystal is in a flower shape and has uniform size distribution as shown in an electron microscope picture of figure 4.
Example 5(TOP, Se/S ═ 1:2.7)
A50 m L flask was charged with 4.5mmol Zn (Ac)26.7mmol TOP, 16.4mmol OA, 4.0g ODE, exhausting at 210 ℃ for 35min, heating to 320 ℃, injecting nanocrystal core with OD450nm being 50, immediately injecting 0.44mmol Se-TBP (with concentration of 1.0mmol/m L), heating to 320 ℃, reacting for 100min, injecting 1.2mmol S-TBP (with concentration of 2.0mmol/m L) at 320 ℃, heating to 320 ℃, reacting for 45min, cooling and purifying to obtain the nanocrystal electron microscope picture shown in figure 5, wherein the nanocrystal is flower-shaped and has uniform size distribution.
Example 6 (two-pot method Se: S ═ 1:3.3)
(1) A50 m L flask was charged with 4.5mmol Zn (Ac)29mmol of OA, 4.0g of ODE, exhausting at 200 ℃ for 3min, injecting a nanocrystal core with OD450nm being 50 for reaction for 15min, injecting 9.0mmol of OA, exhausting for reaction for 30min, heating to 250 ℃, injecting 0.3mmol of Se-TBP (1.0mmol/m L), heating to 310 ℃ for reaction for 90min, cooling, purifying and dissolving in ODE to obtain ZnSe coated nanocrystal for later use.
(2)2mmol Zn(Ac)24mmol OA, 2.0g ODE, 200 ℃ exhaust for 35min, temperature is raised to 315 ℃, nanocrystal (OD 450nm is 20) in (1) is injected, 0.4mmol S-TBP (concentration is 2.0mmol/m L) is injected immediately, temperature is lowered to 310 ℃, reaction is carried out for 60min, test is finished, the nanocrystal is dissolved in toluene, and the obtained nanocrystal is flower-shaped and has uniform size distribution as an electron microscope picture shown in figure 6.
Example 7 (two-pot method, TOP, Se: S ═ 1:7)
(1)4.5mmol Zn(Ac)24.5mmol TOP, 9.0mmol OA, 4.0g ODE in a flask, exhausting gas at 220 ℃ for 3min, injecting nanocrystal core with OD450nm of 50 for reaction for 15min, injecting 9.0mmol OA at 220 ℃, exhausting gas for 30min, heating to 250 ℃, injecting 0.46mmol Se-TBP (concentration of 1.0mmol/m L) for reaction for 30min, heating to 310 ℃ for reaction for 60min, cooling for purification and dissolving in ODE for standby, and obtaining the nanocrystal electron microscope picture of the intermediate, which is shown in figure 7.
(2)2.0mmol Zn(Ac)24.0mmol of OA, 2.0g of ODE are put into a flask, the gas is discharged for 35min at 220 ℃, the temperature is raised to 315 ℃, the nanocrystalline (OD 450nm is 20) is injected into the flask (1), then 0.6mmol of S-TBP (the concentration is 2.0mmol/m L) is injected immediately, the temperature is lowered to 310 ℃, the reaction is carried out for 60min, the temperature is lowered and the purification is carried out, and the obtained nanocrystalline is flower-shaped and has more uniform size distribution as an electron microscope picture shown in figure 8.
Comparative example 1
A50 m L flask was charged with 4mmol Zn (Ac)210g ODE, exhausting at 200 ℃ for 35min, heating to 300 ℃, injecting nanocrystal core with OD450nm being 50, injecting 5mmol OA after reacting for 15min, injecting 0.4mmol Se/TBP (with concentration of 0.5M) when the temperature rises to 300 ℃, injecting 0.4mmol S/TBP (with concentration of 4M) after reacting for 15min, coolingAnd (5) purifying. The obtained nanocrystalline is approximately spherical and has uniform size distribution by referring to an electron microscope image of fig. 9.
The nanocrystals purified in each of the above examples and comparative examples were dissolved in toluene to obtain a nanocrystal solution, and the fluorescence emission peak (nanocrystal concentration OD450 nm: 0.3), half-peak width (nanocrystal concentration OD450 nm: 0.3), and quantum yield (nanocrystal concentration OD450 nm: 4) were measured. The test method refers to GBT 36081-2018. The results are shown in table 1:
TABLE 1
It can be seen that the half-peak width of the flower-like nanocrystals in the above examples does not exceed 43nm, which indirectly indicates that the prepared nanocrystal population has better size uniformity. As can be seen from comparative example 1, the molar ratio of the amounts of Se precursor and S precursor added was more than 1, and flower-like nanocrystals could not be obtained.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (11)
1. A nanocrystal comprising a first nanostructure and a plurality of second nanostructures, wherein the first nanostructure is InZnP/ZnSe, the second nanostructure is ZnS, the second nanostructures surrounds the first nanostructure, and at least a portion of the second nanostructures are not attached to the first nanostructure, and at least a portion of the second nanostructures are attached to the first nanostructure, and wherein the plurality of second nanostructures covers at least a portion of a surface of the first nanostructure.
2. The nanocrystal of claim 1, wherein at least two of the plurality of second nanostructures are connected to each other, and preferably wherein the nanocrystal has a fluorescence peak wavelength ranging from 610 nm to 630 nm.
3. A method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution;
s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding the InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure;
s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction;
wherein the molar ratio of the Se precursor to the S precursor is less than 1.
4. A method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution;
s2, mixing the first short-chain fatty acid zinc and the first non-coordination solvent in a container, heating to a first temperature, and exhausting for a certain time; adding the InZnP nanocrystalline solution into the container at a second temperature, reacting for a certain time, adding a first long-chain fatty acid, then adding a Se precursor into the container at the second temperature, and reacting for a certain time to generate InZnP/ZnSe nanocrystalline with a core-shell structure;
s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction;
wherein the molar ratio of the Se precursor to the S precursor is less than 1.
5. A method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution;
s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a container, heating to a first temperature, and exhausting for a certain time; adding the InZnP nanocrystalline solution into the container at a second temperature, then adding a Se precursor into the container, and reacting for a certain time to generate InZnP/ZnSe nanocrystals with a core-shell structure;
s3, adding an S precursor into the container, reacting for a certain time at a third temperature, and then terminating the reaction;
wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the Se precursor to the S precursor is less than 1.
6. A method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution;
s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding the InZnP nanocrystalline solution into the first container at the first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordination solvent to obtain an InZnP/ZnSe nanocrystalline solution;
s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding the InZnP/ZnSe nanocrystalline solution into the second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction;
wherein the molar ratio of the Se precursor to the S precursor is less than 1.
7. A method for preparing a nanocrystal, comprising the steps of:
s1, preparing an InZnP nanocrystalline solution;
s2, mixing the first short-chain fatty acid zinc, the first non-coordination solvent, the ligand and the first long-chain fatty acid in a first container, heating to a first temperature, and exhausting for a certain time; adding the InZnP nanocrystalline solution into the first container at the first temperature, adding a third long-chain fatty acid, continuing exhausting for a certain time, then adding a Se precursor into the first container at a fourth temperature, reacting for a certain time at the third temperature, terminating the reaction, separating, purifying and re-dissolving in a third non-coordination solvent to obtain an InZnP/ZnSe nanocrystalline solution;
s3, mixing the second short-chain fatty acid zinc, the second non-coordination solvent and the second long-chain fatty acid in a second container, heating to the first temperature, and exhausting for a certain time; adding the InZnP/ZnSe nanocrystalline solution into the second container at a second temperature, then adding an S precursor into the second container, reacting for a certain time at a third temperature, and then terminating the reaction;
wherein the ligand is selected from one or more of trioctylamine and trioctylphosphine, and the molar ratio of the Se precursor to the S precursor is less than 1.
8. The method according to any one of claims 3 to 7, wherein the molar ratio of the Se precursor to the S precursor is 1:2.7 to 1: 96.
9. The method for producing a nanocrystal according to any one of claims 3 to 7, wherein the first temperature is 200 to 220 ℃, the second temperature is 300 to 320 ℃, the third temperature is 300 to 320 ℃, and the fourth temperature is 230 to 250 ℃.
10. The method for preparing the nanocrystal according to any one of claims 3 to 7, wherein each short-chain fatty acid zinc is independently selected from one or more fatty acid zinc with a C atom number of less than 8, and each long-chain fatty acid is independently selected from one or more fatty acid with a C atom number of more than 8.
11. The method according to any one of claims 3 to 7, wherein the Se precursor is one or more of Se-TBP, Se-TOP and Se-ODE, and the S precursor is one or more of S-TBP, S-TOP and S-ODE.
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