CN111909699B - Preparation method of indium phosphide nanocrystal and product prepared by same - Google Patents
Preparation method of indium phosphide nanocrystal and product prepared by same Download PDFInfo
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- CN111909699B CN111909699B CN201910388638.XA CN201910388638A CN111909699B CN 111909699 B CN111909699 B CN 111909699B CN 201910388638 A CN201910388638 A CN 201910388638A CN 111909699 B CN111909699 B CN 111909699B
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- C09K11/883—Chalcogenides with zinc or cadmium
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Abstract
The application discloses a preparation method of indium phosphide nanocrystal and a product prepared by the same. The preparation method of the indium phosphide nanocrystal comprises the following steps: and mixing and reacting the first solution system containing the indium source and the second solution system containing the phosphorus source at a preset temperature to obtain the indium phosphide nanocrystal. The first solution system containing the indium source comprises the indium source and a first organic solvent for dispersing the indium source, the second solution system containing the phosphorus source comprises a phosphorus source and a second organic solvent for dispersing the phosphorus source, the first organic solvent and the second organic solvent are different, and the boiling point of the second organic solvent is lower than the preset temperature. By the preparation method, the indium phosphide nanocrystalline with the wavelength range of 700-900 nm can be directly obtained in one step, and the application of the indium phosphide nanocrystalline in the near-infrared wavelength range is realized, so that the application range of the indium phosphide nanocrystalline is widened.
Description
Technical Field
The application belongs to the field of nano materials, and particularly relates to a preparation method of indium phosphide nanocrystals and a product prepared by the indium phosphide nanocrystals.
Background
Compared with organic fluorescent dye, the nanocrystal has the advantages of photobleaching resistance, high quantum yield and the like, and has great application prospect in the field of biological imaging. However, the II-VI element quantum dots (cadmium selenide, cadmium telluride and the like) which are most researched and applied in the prior art contain high-toxicity elements such as cadmium and the like, have obvious neurotoxicity, and limit the application of the quantum dots such as the cadmium selenide and the like in organisms.
Compared with II-VI element quantum dots, III-V element quantum dots represented by indium phosphide quantum dots have no inherent toxicity and wider application range, and are gradually receiving attention from the scientific research community and the industrial community. However, the emission wavelength of the indium phosphide quantum dots synthesized by the prior art is generally 450-700 nm, which limits the application of the indium phosphide quantum dots in the wavelength range above 700 nm.
Disclosure of Invention
In order to solve the technical problems, the application provides a preparation method of a large-wavelength indium phosphide nanocrystal.
According to one aspect of the present application, there is provided a method for preparing indium phosphide nanocrystals, comprising the steps of:
s1, obtaining a first solution system containing an indium source and a second solution system containing a phosphorus source;
s2, mixing and reacting a first solution system containing an indium source and a second solution system containing a phosphorus source at a preset temperature to obtain indium phosphide nanocrystalline;
wherein the first solution system containing the indium source comprises the indium source and a first organic solvent for dispersing the indium source, the second solution system containing the phosphorus source comprises a phosphorus source and a second organic solvent for dispersing the phosphorus source, the first organic solvent and the second organic solvent are different, and the boiling point of the second organic solvent is lower than the preset temperature.
Further, the boiling point of the second organic solvent is at least 30 ℃ lower than the predetermined temperature.
Further, the range of the preset temperature is 180-320 ℃, and the boiling point of the second organic solvent is 60-150 ℃.
Further, the chemical structural formula of the phosphorus source is M- (O-C ≡ P)nWherein M is a metal element, and n is 1, 2 or 3.
Further, the second organic solvent includes at least one of benzene, toluene, cyclohexane, n-hexane, n-heptane, n-octane, tetrahydrofuran, and chloroform.
Further, the indium source is indium halide.
Further, the first organic solvent is at least one of saturated or unsaturated amines having 6 or more carbon atoms.
Further, the first solution system comprising the indium source also comprises a zinc source.
Further, a shell layer is coated on the indium phosphide nanocrystal.
According to another aspect of the application, an indium phosphide nanocrystal prepared by the preparation method is provided.
Furthermore, the peak value of the emission peak of the indium phosphide nanocrystal is 700-900 nm.
Has the advantages that: according to the preparation method, the first solution system containing the indium source and the second solution system containing the phosphorus source are mixed and react at the preset temperature, and the boiling point of the second organic solvent is lower than the preset temperature, so that the indium phosphide nanocrystal with the wavelength range of 700-900 nm can be directly obtained in one step, the application of the indium phosphide nanocrystal in the near-infrared wavelength range is realized, and the application range of the indium phosphide nanocrystal is widened.
Detailed Description
The following describes technical solutions in the examples of the present application in detail with reference to the embodiments of the present application. It should be noted that the described embodiments are only some embodiments of the present application, and not all embodiments.
It should be understood that the preparation method of the present invention is the same as the reaction environment required for preparing the nanocrystal in the prior art unless otherwise specified. Before the reaction, moisture and oxygen in the reaction vessel were removed using an inert gas atmosphere or an air atmosphere from which moisture and oxygen had been removed, and each reaction process in the experiment was carried out under the protection of an inert gas atmosphere. Wherein the inert gas atmosphere comprises at least one of nitrogen, argon, or a rare gas.
It is to be understood that the boiling points of the solvents in this application are all indicated at sub-atmospheric pressure, due to the different boiling points of the solvents at different pressures.
The application provides a preparation method of indium phosphide nanocrystal, which comprises the following steps:
s1, obtaining a first solution system containing an indium source and a second solution system containing a phosphorus source;
s2, mixing and reacting a first solution system containing an indium source and a second solution system containing a phosphorus source at a preset temperature to obtain indium phosphide nanocrystalline;
wherein the first solution system containing the indium source comprises the indium source and a first organic solvent for dispersing the indium source, the second solution system containing the phosphorus source comprises a phosphorus source and a second organic solvent for dispersing the phosphorus source, the first organic solvent and the second organic solvent are different, and the boiling point of the second organic solvent is lower than the preset temperature.
In a preferred embodiment of the present application, the boiling point of the second organic solvent is at least 30 ℃ lower than the predetermined temperature.
According to a preferred embodiment of the present invention, the temperature range of mixing and reacting the first solution system including the indium source and the second solution system including the phosphorus source in S2 is 180 to 320 ℃, and the boiling point of the second organic solvent is 60 to 150 ℃.
In a specific embodiment, firstly, adjusting the temperature of a first solution system containing an indium source to 180-280 ℃, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system; and then, heating the indium-phosphorus mixed solution system to 280-320 ℃, preserving the temperature and reacting for a period of time to obtain a solution system containing the indium phosphide nanocrystal.
According to a preferred embodiment of the present application, the phosphorus source has the chemical formula M- (O-C.ident.P)nWherein M is a metal element, and n is 1, 2 or 3.
Further, when the M element is a monovalent metal element such as Li, Na, K, Rb, Cs, etc., n is 1. When the M element is a divalent metal element such as Zn, Ca, Mn, Sr, etc., n is 2. When the M element is a trivalent metal element such as Al, Ga, Tl, etc., n is 3.
In a specific embodiment, the phosphorus source M- (O-C ≡ P)nIs Li-O-C.ident. P, Na-O-C.ident. P, K-O-C.ident. P, Zn- (O-C.ident.P)2Or Ga- (O-C ≡ P)3。
In the present application, M- (O-C.ident.P) is chosennAs a new phosphorus source for synthesizing indium phosphide nanocrystals. Combining a source of indium with M- (O-C ≡ P)nMixing and reacting at a preset temperature, and obtaining the indium phosphide nanocrystal with the wavelength range of 700-900 nm only by one-time feeding. Meanwhile, the phosphorus source M- (O-C ≡ P) of the applicationnAnd the metal element M can be provided, so that the nanocrystalline with the alloy core consisting of In, P and the metal element M is prepared, and the optical performance of the indium phosphide nanocrystalline is further optimized.
According to a preferred embodiment of the present application, the second organic solvent comprises at least one of benzene, toluene, cyclohexane, n-hexane, n-heptane, n-octane, tetrahydrofuran, chloroform.
According to a preferred embodiment of the present application, the indium source is an indium halide.
In a particular embodiment, the indium source comprises at least one of indium chloride, indium bromide, indium iodide.
According to a preferred embodiment of the present application, the first organic solvent is at least one of a saturated or unsaturated amine having 6 or more carbon atoms.
In a specific embodiment, the first organic solvent comprises at least one of hexylamine, heptylamine, octylamine, trioctylamine, nonylamine, decylamine, decaenamine, undecylamine, dodecylamine, tridecylamine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, oleylamine, decaenamine, undecenylamine, dodecenylamine, tridecylamine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecelamine, octadecylamine.
According to a preferred embodiment of the present application, the first solution system comprising the source of indium further comprises a source of zinc.
In a particular embodiment, the zinc source comprises at least one of zinc acetate, zinc chloride, zinc carbonate, zinc decate, zinc undecylenate, zinc stearate, zinc oleate, and zinc diethyldithiocarbamate.
The inventor finds that in the process of preparing the indium phosphide nanocrystal, a certain amount of zinc source is introduced into a reaction system, so that the surface defects of the nanocrystal core can be further reduced, and the energy level luminous efficiency of the nanocrystal can be enhanced.
According to a preferred embodiment of the present application, a shell layer is coated on the indium phosphide nanocrystal.
In one embodiment, precursor materials required for synthesizing the shell are added to the solution system containing the nanocrystals to obtain the shell-coated indium phosphide nanocrystals. The precursor material required for synthesizing the shell layer comprises a zinc source and at least one of a sulfur source and a selenium source.
According to a preferred embodiment of the present application, in order to further improve the optical properties of the prepared indium phosphide nanocrystal, after the indium phosphide nanocrystal is obtained, the method further comprises the step of removing unreacted raw materials and other impurities, and particularly comprises separation and purification. These steps are well known methods in the art and will not be described further herein.
According to a preferred embodiment of the application, the indium phosphide nanocrystal is prepared by the preparation method, and the emission peak value of the indium phosphide nanocrystal is 700-900 nm.
In the prior art, in order to obtain indium phosphide nanocrystals with large wavelength, a method of increasing the size of the indium phosphide nanocrystals is often adopted. However, this method often causes problems such as increase of surface defects and difficulty in wavelength control, and cannot meet application requirements. The preparation method can directly obtain the indium phosphide nanocrystal with the emission wavelength of 700-900 nm only by a one-step method.
According to a preferred embodiment of the present application, the indium phosphide nanocrystal contains M, In and P element, where M is a metal element. The inventor finds that the indium phosphide nanocrystal containing M, In and P has fewer surface defects compared with the indium phosphide nanocrystal consisting of In and P, and the luminescent center of the indium phosphide nanocrystal does not contain heavy metal elements, so that the indium phosphide nanocrystal is more environment-friendly and has a wide application range.
In a specific embodiment, the constituent elements of the indium phosphide nanocrystals further include Zn, but the constituent elements of the indium phosphide nanocrystals of the present invention are not limited thereto.
According to a preferred embodiment of the present application, the indium phosphide nanocrystal is externally coated with a shell layer, wherein the shell layer contains a Zn element and at least one of an S element and a Se element.
In a specific embodiment, the shell layer is at least one of ZnS, ZnSe, and ZnSeS.
The inventor finds that the ZnS and/or ZnSe and/or ZnSeS shell layer is grown on the surface of the indium phosphide nanocrystal, so that the indium phosphide nanocrystal with better stability and better optical property can be obtained.
Hereinafter, embodiments of the present invention will be described in more detail with reference to examples. However, they are exemplary embodiments of the present invention, and the present invention is not limited thereto.
Example 1
The indium phosphide nanocrystal 1 is composed of three elements of In, P and Na, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 0.5mmol of indium chloride with 10mL of oleylamine at 25 ℃ to obtain a first solution system containing an indium source;
mixing 0.75mmol of NaOCP with 5mL of toluene to obtain a second solution system containing a phosphorus source;
s2, heating a first solution system containing an indium source to 200 ℃ under the nitrogen exhaust state, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system;
s3, heating the indium-phosphorus mixed solution system obtained in the step S2 to 280 ℃, and reacting for 60min to obtain a solution system containing indium phosphide nanocrystals;
s4, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the indium phosphide nanocrystal, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 1.
Example 2
The indium phosphide nanocrystal 2 is composed of In, P, Na and Zn, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 0.5mmol of indium chloride, 2mmol of zinc chloride and 10mL of oleylamine at 30 ℃ to obtain a first solution system containing an indium source;
mixing 0.75mmol of NaOCP with 5mL of toluene to obtain a second solution system containing a phosphorus source;
s2, heating a first solution system containing an indium source to 200 ℃ under the nitrogen exhaust state, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system;
s3, heating the indium-phosphorus mixed solution system obtained in the step S2 to 280 ℃, and reacting for 60min to obtain a solution system containing indium phosphide nanocrystals;
s4, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the indium phosphide nanocrystal, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 2.
Example 3
The indium phosphide nanocrystal 3 is composed of In, P, K and Zn, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 0.5mmol of indium chloride, 2mmol of zinc chloride and 10mL of oleylamine at 25 ℃ to obtain a first solution system containing an indium source;
mixing 0.75mmol KOCP with 5mL toluene to obtain a second solution system containing a phosphorus source;
s2, heating the first solution system to 200 ℃ under the nitrogen exhaust state, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system;
s3, heating the indium-phosphorus mixed solution system obtained in the step S2 to 280 ℃, and reacting for 60min to obtain a solution system containing indium phosphide nanocrystals;
s4, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the indium phosphide nanocrystal, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 3.
Example 4
The indium phosphide nanocrystal 4 is composed of three elements of In, P and K, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 0.5mmol of indium chloride with 10mL of oleylamine at 25 ℃ to obtain a first solution system containing an indium source;
mixing 0.75mmol KOCP with 5mL toluene to obtain a second solution system containing a phosphorus source;
s2, heating a first solution system containing an indium source to 240 ℃ under the nitrogen gas exhaust state, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system;
s3, heating the indium-phosphorus mixed solution system obtained in the step S2 to 300 ℃, and reacting for 60min to obtain a solution system containing indium phosphide nanocrystals;
s4, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the indium phosphide nanocrystal, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 4.
Comparative example 1
The indium phosphide nanocrystal 5 is composed of three elements of In, P and Na, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 0.5mmol of indium chloride with 10mL of oleylamine at 25 ℃ to obtain a first solution system containing an indium source; mixing 0.75mmol of NaOCP with 5mL of oleylamine to obtain a second solution system containing a phosphorus source;
s2, heating a first solution system containing an indium source to 240 ℃ under the nitrogen gas exhaust state, and adding a second solution system containing a phosphorus source to obtain an indium-phosphorus mixed solution system;
s3, heating the indium-phosphorus mixed solution system obtained in the step S2 to 300 ℃, and reacting for 60min to obtain a solution system containing indium phosphide nanocrystals;
s4, heating, reacting 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine (2mmol/mL) to obtain a ZnSe shell coated on the indium phosphide nanocrystal; then 6mL of sulfur-trioctylphosphine (2mmol/mL) is added and reacts to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 5.
Comparative example 2
The indium phosphide nanocrystal 6 is composed of three elements of In, Zn and P, and the shell is a double-shell layer composed of ZnSe and ZnS.
The preparation process of the indium phosphide nanocrystal comprises the following steps:
s1, mixing 50mg of indium chloride, 150mg of zinc chloride and 3mL of oleylamine, and keeping the temperature at 120 ℃ for 1h under the nitrogen exhaust state;
s2, heating to 180 ℃, quickly injecting tris (diethylamino) phosphine, and reacting for 60 min;
s3, adding 0.5mL of selenium-trioctylphosphine solution (1mmol/mL), and reacting for 60min to obtain a ZnSe shell coated on the indium phosphide nanocrystal;
s4, adding 500mg of zinc stearate and 2mL of octadecene, heating to 200 ℃, reacting for 30min, adding 0.5mL of sulfur-trioctylphosphine solution (1mmol/mL), and reacting for 30min to obtain a ZnS shell coated on the ZnSe shell;
and S5, separating and purifying after the reaction is finished to obtain the indium phosphide nanocrystal 6.
In addition, the indium phosphide nanocrystals of examples 1 to 4 and comparative examples 1 to 2 were further tested for fluorescence properties. The test results are shown in the following table.
According to the above table, by the preparation method, the first solution system containing the indium source and the second solution system containing the phosphorus source are mixed and reacted at the preset temperature, and the boiling point of the second organic solvent is lower than the preset temperature, the indium phosphide nanocrystal with the wavelength range of 700-900 nm can be directly obtained in one step only in a one-time feeding mode, so that the application of the indium phosphide nanocrystal in the near-infrared wavelength range is realized, and the application range of the indium phosphide nanocrystal is widened.
Although the present disclosure has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent substitutions, will be apparent to those skilled in the art without departing from the spirit of the disclosure, and that no limitations to the present disclosure are intended or should be inferred therefrom.
Claims (9)
1. A preparation method of indium phosphide nanocrystal is characterized by comprising the following steps:
s1, obtaining a first solution system containing an indium source and a second solution system containing a phosphorus source;
s2, mixing and reacting the first solution system containing the indium source and the second solution system containing the phosphorus source at a preset temperature to obtain the indium phosphide nanocrystal;
said first solution system comprising a source of indium and a first organic solvent in which said source of indium is dispersed, said second solution system comprising a source of phosphorus and a second organic solvent in which said source of phosphorus is dispersed, said first organic solvent being different from said second organic solvent, said second organic solvent having a boiling point below said predetermined temperature, wherein said source of phosphorus is Li-O-C.ident. P, Na-O-C.ident. P, K-O-C.ident. P, Zn- (O-C.ident.P)2Or Ga- (O-C ≡ P)3。
2. The method of claim 1, wherein the second organic solvent has a boiling point at least 30 ℃ lower than the predetermined temperature.
3. The method according to claim 1, wherein the predetermined temperature is in the range of 180 to 320 ℃ and the boiling point of the second organic solvent is in the range of 60 to 150 ℃.
4. The method according to claim 1, wherein the second organic solvent comprises at least one of benzene, toluene, cyclohexane, n-hexane, n-heptane, n-octane, tetrahydrofuran, and chloroform.
5. The method of claim 1 wherein the indium source is an indium halide.
6. The method according to claim 1, wherein the first organic solvent is at least one of a saturated or unsaturated amine having 6 or more carbon atoms.
7. The method of claim 1 wherein the first solution system comprising a source of indium further comprises a source of zinc.
8. An indium phosphide nanocrystal characterized by being produced by the production method as set forth in any one of claims 1 to 7.
9. The indium phosphide nanocrystal of claim 8, wherein the indium phosphide nanocrystal has an emission peak to peak value of 700-900 nm.
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| CN201910388638.XA CN111909699B (en) | 2019-05-10 | 2019-05-10 | Preparation method of indium phosphide nanocrystal and product prepared by same |
| KR1020217037707A KR20220002392A (en) | 2019-04-18 | 2020-04-17 | Method for producing indium phosphide nanocrystals using novel phosphorus precursor and indium phosphide nanocrystals prepared thereby |
| PCT/CN2020/085274 WO2020211834A1 (en) | 2019-04-18 | 2020-04-17 | Method for preparing indium phosphide nanocrystals using novel phosphorus precursor and indium phosphide nanocrystals prepared using same |
| JP2021561728A JP7470135B2 (en) | 2019-04-18 | 2020-04-17 | Method for producing indium phosphide nanocrystals using a novel phosphorus precursor and the produced indium phosphide nanocrystals |
| US17/604,452 US11827827B2 (en) | 2019-04-18 | 2020-04-17 | Method for preparing indium phosphide nanocrystal by using novel phosphorus precursor and indium phosphide nanocrystal prepared by the same |
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