CN111826158A - Preparation method of indium phosphide nanocrystal - Google Patents
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Abstract
The application discloses a preparation method of indium phosphide nanocrystal, which is characterized by comprising the following steps: by adopting M- (O-C ≡ P)nAs one of reaction precursors, M is a metal element, and n is 1, 2 or 3. The application adopts M- (O-C ≡ P)nAs one of the reaction precursors, the metal element M and the metal element P are from the same reaction precursor, so that the nanocrystalline containing the nanocrystal core of In, P and the metal element M can be prepared; in addition, the proportion of the M element and the P element is fixed, and the preparation is easier to controlThe luminescent performance of the prepared indium phosphide nanocrystal is excellent due to the composition of elements in the nanocrystal.
Description
Technical Field
The application belongs to the field of nano materials, and particularly relates to a preparation method of indium phosphide nanocrystals.
Background
The nano-crystal has the advantages of narrow half-peak width, high quantum yield and the like, and has great application prospect in the fields of display, illumination and the like. Compared with II-VI element quantum dots, III-V element quantum dots represented by indium phosphide quantum dots do not contain heavy metal elements, have wider application range and are gradually receiving attention from the scientific research community and the industrial community.
However, the optical performance of the indium phosphide quantum dots prepared by the conventional common method still needs to be improved, and the optimization of the preparation method of the indium phosphide quantum dots has important significance.
Disclosure of Invention
In order to solve the technical problems, the application provides a preparation method of indium phosphide nanocrystal.
According to one aspect of the present application, there is provided a method for preparing indium phosphide nanocrystals, comprising the step of using M- (O-C ≡ P)nAs one of reaction precursors, M is a metal element, and n is 1, 2 or 3.
Further, said 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。
Further, the indium phosphide nanocrystal contains M, In and P elements.
Further, the reaction precursor further comprises an indium precursor.
Further, the reaction precursor further comprises a zinc precursor.
Further, comprising the steps of: for indium precursor, M- (O-C ≡ P)nAnd carrying out high-temperature treatment on the solution of the solvent to obtain the indium phosphide nanocrystal core.
Further, comprising the steps of: and coating a shell layer on the nanocrystal core.
Further, the solvent is a complex compound.
Further, the coordination compound is an amine or a carboxylic acid.
Further, the temperature of the high-temperature reaction is between 150 ℃ and 300 ℃.
Has the advantages that: this applicationBy adopting M- (O-C ≡ P)nAs one of the reaction precursors, the metal element M and the metal element P are from the same reaction precursor, so that the nanocrystalline containing the nanocrystal core of In, P and the metal element M can be prepared; in addition, the proportion of the M element and the P element is fixed, the composition of elements in the prepared nanocrystalline is easier to control, and the luminescent property of the prepared indium phosphide nanocrystalline is excellent.
Drawings
FIG. 1 is a schematic structural diagram of a nanocrystal in an exemplary embodiment of the present application;
FIG. 2 is a transmission electron microscope photograph of nanocrystals in example 1;
FIG. 3 is a fluorescence emission spectrum of the nanocrystal in example 1.
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.
FIG. 1 is a schematic structural diagram of an indium phosphide nanocrystal prepared In an exemplary embodiment of the present application, wherein nanocrystal 100 includes nanocrystal core 101, nanocrystal core 101 including In, P, and metal element M; and a shell 102 disposed on the nanocrystal core 101.
In an exemplary embodiment of the present application, a method for preparing indium phosphide nanocrystals includes the steps of: by adopting M- (O-C ≡ P)nAs one of reaction precursors, M is a metal element, and n is 1, 2 or 3.
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. Preferably, 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。
By adopting M- (O-C ≡ P)nWhen the precursor is used as a reaction precursor, alloy indium phosphide nano-cores containing P element and M element can be obtained, thereby improving the phosphorizationLuminescent property of the indium nanocrystal. And because the M element and the P element are from the same reaction precursor, the problem that the proportion is not easy to control when the M element and the P element are from different precursors in the prior art can be avoided.
The reaction precursor further includes an indium precursor, and the indium precursor is preferably an indium halide, such as indium chloride, indium bromide, and indium iodide. The reaction precursor may also include a zinc precursor, which preferably includes a zinc carboxylate.
The preparation of the indium phosphide nanocrystal comprises first preparing an indium phosphide nanocrystal core, followed by including a shell layer on the surface of the indium phosphide nanocrystal core. The preparation of the indium phosphide nanocrystal core comprises the following steps: for indium precursor, M- (O-C ≡ P)nAnd a solvent, wherein the temperature of the high-temperature treatment is preferably between 150 ℃ and 300 ℃, more preferably between 180 ℃ and 240 ℃. The solvent is preferably a complex compound including carboxylic acids such as oleic acid, myristic acid, and the like; the coordination compound may also be an amine, such as oleylamine, octadecylamine, tetradecylamine, and the like.
The preparation method according to some exemplary embodiments of the present application will be described in more detail below with reference to the following examples; however, the exemplary embodiments of the present application are not limited thereto.
Example 1
The indium phosphide nanocrystal core is composed of three elements of In, P and Li, 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, 0.75mmol of Li-O-C [ identical to ] P and 10mL of oleylamine at 25 ℃ to obtain a first solution system;
s2, heating the first solution system to 180 ℃ under the nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s3, heating, adding 24mmol of zinc stearate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S4, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Example 2
The indium phosphide nanocrystal core 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, 0.75mmol of Na-O-C [ identical to ] P and 10mL of oleylamine at 25 ℃ to obtain a first solution system;
s2, heating the first solution system to 180 ℃ under the nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s3, heating, adding 24mmol of zinc stearate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S4, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Example 3
The indium phosphide nanocrystal core is composed of three elements of In, P 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, adding 0.5mmol of indium chloride and 0.75mmol of Zn- (O-C.ident.P) at 25 DEG C2Mixing with 10mL of oleylamine to obtain a first solution system;
s2, heating the first solution system to 180 ℃ under the nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s3, heating, adding 24mmol of zinc stearate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S4, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Example 4
The indium phosphide nanocrystal core is composed of three elements of In, P and Ga, 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, adding 0.5mmol of indium chloride and 0.75mmol of Ga- (O-C.ident.P) at 25 DEG C3Mixing with 10mL of oleylamine to obtain a first solution system;
s2, heating the first solution system to 180 ℃ under the nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s3, heating, adding 24mmol of zinc stearate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S4, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Example 5
The indium phosphide nanocrystal core 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, 4.0mmol of zinc chloride, 0.75mmol of Na-O-C [ identical to ] P and 10mL of oleylamine at 30 ℃ to obtain a first solution system;
s2, heating the first solution system to 180 ℃ under the nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s3, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S4, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Comparative example 1
The indium phosphide nanocrystal core is composed of three elements of In, P and Li, 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 0.15mmol of indium acetate, 0.1mmol of lithium acetate, 0.1mmol of tris (trimethylsilyl) phosphine (dispersed in 1mL of TOP), 0.3mmol of tetradecanoic acid and 10mL of octadecene, keeping the temperature at 180 ℃ in a nitrogen-exhausted state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s2, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S3, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Comparative example 2
The indium phosphide nanocrystal core 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 0.15mmol of indium acetate, 0.1mmol of sodium acetate, 0.1mmol of tris (trimethylsilyl) phosphine (dispersed in 1mL of TOP), 0.3mmol of tetradecanoic acid and 10mL of octadecene, keeping the temperature at 180 ℃ in a nitrogen-exhausted state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s2, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S3, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Comparative example 3
The indium phosphide nanocrystal core is composed of three elements of In, P 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 0.15mmol of indium acetate, 0.1mmol of zinc acetate, 0.1mmol of tris (trimethylsilyl) phosphine (dispersed in 1mL of TOP), 0.3mmol of tetradecanoic acid and 10mL of octadecene, keeping the temperature at 180 ℃ in a nitrogen exhaust state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s2, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S3, after the reaction is finished, separating and purifying to obtain the nanocrystal.
Comparative example 4
The indium phosphide nanocrystal core is composed of three elements of In, P and Ga, 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 0.15mmol of indium acetate, 0.1mmol of gallium acetate, 0.1mmol of tris (trimethylsilyl) phosphine (dispersed in 1mL of TOP), 0.3mmol of tetradecanoic acid and 10mL of octadecene, keeping the temperature at 180 ℃ in a nitrogen-exhausted state, and reacting for 60min to obtain a solution system containing a nanocrystal core;
s2, heating, adding 24mmol of zinc acetate and 6mL of selenium-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnSe shell coated on the nanocrystal core, and adding 6mL of sulfur-trioctylphosphine solution (2mmol/mL) for reaction to obtain a ZnS shell coated on the ZnSe shell;
and S3, after the reaction is finished, separating and purifying to obtain the nanocrystal.
FIG. 2 is a transmission electron micrograph of the indium phosphide nanocrystals prepared as described in example 1, from which it can be seen that the size of the indium phosphide nanocrystals was about 3.5 nm.
FIG. 3 is a fluorescence emission spectrum of the InP nanocrystal of example 1, which shows a peak wavelength of 527 nm and a half-peak width of 37 nm.
In addition, the indium phosphide nanocrystals in examples 1 to 5 and comparative examples 1 to 4 were further tested for fluorescence properties. The test results are shown in the following table:
| peak wavelength (nm) | Peak width (nm) | Quantum yield (%) | |
| Example 1 | 527 | 37 | 61 |
| Example 2 | 531 | 38 | 73 |
| Example 3 | 525 | 36 | 74 |
| Example 4 | 521 | 40 | 75 |
| Example 5 | 530 | 38 | 75 |
| Comparative example 1 | 528 | 43 | 41 |
| Comparative example 2 | 533 | 45 | 38 |
| Comparative example 3 | 524 | 42 | 43 |
| Comparative example 4 | 523 | 46 | 36 |
As can be seen from the above table, M- (O-C ≡ P) is usednWhen the indium phosphide quantum dot is used as a reaction precursor of metal elements M and P, compared with the case of singly adopting the precursor M and the precursor P, the peak wavelength of the emission peak of the prepared indium phosphide quantum dot is basically unchanged, the half-peak width is obviously reduced, and the quantum yield is obviously increased, for example: compared with the comparative example 1, the half-peak width of the example 1 is reduced by 6 nanometers, and the quantum yield is increased by 20 percent; compared with the comparative example 2, the half-peak width of the embodiment 2 is reduced by 7 nanometers, and the quantum yield is increased by 35 percent; compared with the comparative example 3, the half-peak width of the embodiment 3 is reduced by 6 nanometers, and the quantum yield is increased by 31 percent; example 4 the half-peak width was reduced by 6 nm and the quantum yield increased by 39% compared to comparative example 4.
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 (10)
1. A preparation method of indium phosphide nanocrystal is characterized by comprising the following steps: by adopting M- (O-C ≡ P)nAs one of reaction precursors, M is a metal element, and n is 1, 2 or 3.
2. The process according to claim 1, wherein 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。
3. The method according to claim 1, wherein the indium phosphide nanocrystal contains M, In and P element.
4. The method of claim 1, wherein the reaction precursor further comprises an indium precursor.
5. The method of claim 1, wherein the reaction precursor further comprises a zinc precursor.
6. The method for preparing according to claim 1, characterized by comprising the steps of: for indium precursor, M- (O-C ≡ P)nAnd carrying out high-temperature treatment on the solution of the solvent to obtain the indium phosphide nanocrystal core.
7. The method for preparing according to claim 6, characterized by comprising the steps of: and coating a shell layer on the nanocrystal core.
8. The method according to claim 6, wherein the solvent is a complex compound.
9. The method according to claim 8, wherein the complex compound is an amine or a carboxylic acid.
10. The method of claim 6, wherein the high temperature reaction is at a temperature of between 150 ℃ and 300 ℃.
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| CN201910311285.3A CN111826158B (en) | 2019-04-18 | 2019-04-18 | Preparation method of indium phosphide nanocrystal |
| 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 |
| 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 |
| 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 |
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