CN113861977B - III-V family quantum dot and preparation method thereof - Google Patents
III-V family quantum dot and preparation method thereof Download PDFInfo
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- CN113861977B CN113861977B CN202111354421.0A CN202111354421A CN113861977B CN 113861977 B CN113861977 B CN 113861977B CN 202111354421 A CN202111354421 A CN 202111354421A CN 113861977 B CN113861977 B CN 113861977B
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Abstract
A III-V family quantum dot and a preparation method thereof belong to the technical field of quantum dot synthesis. The preparation method of the III-V group quantum dot comprises the following steps: reacting a III-group cation precursor with organic phosphine with lone pair electrons in a first solvent to obtain a first solution; and mixing the first solution and the V-group anion precursor for reaction to generate a quantum dot core and growing the quantum dot core. The problems of small size and wide size distribution of the existing III-V family quantum dots can be solved.
Description
Technical Field
The application relates to the technical field of quantum dot synthesis, in particular to a III-V family quantum dot and a preparation method thereof.
Background
The quantum dots have excellent optical properties, and the entire visible light region, even including the near infrared region, can be covered by controlling the size and composition of the quantum dots. By virtue of excellent optical and electrical properties, quantum dots are widely applied to the fields of cell imaging, fluorescent probes, quantum dot sensitized solar cells, light emitting diodes and the like.
The quantum dots can be broadly classified into cadmium-containing quantum dots and cadmium-free quantum dots based on cadmium-free quantum dots, which are distinguished according to the kinds of materials. Cadmium-containing substances may cause leakage during the whole production and use processes, and have the risk of causing irreversible damage to personnel and the environment. After the european union has further limited the use of cadmium-containing quantum dots, iii-v group cadmium-free quantum dots have shown great potential to be replacements for cadmium-containing quantum dots.
There are many difficulties in the synthesis process of the III-V group quantum dots. The quantum dots synthesized by the prior art are usually small in size and wide in size distribution.
Disclosure of Invention
The application provides a III-V family quantum dot and a preparation method thereof, which can solve the problems of small size and wide size distribution of the existing III-V family quantum dot.
The embodiment of the application is realized as follows:
in a first aspect, embodiments of the present application provide a method for preparing a group iii-v quantum dot, including:
reacting a III-group cation precursor with organic phosphine with lone pair electrons in a first solvent to obtain a first solution;
and mixing the first solution and the V-family anion precursor for reaction to generate a quantum dot core and growing the quantum dot core.
In a second aspect, embodiments of the present application provide a group iii-v quantum dot, which is prepared by the method for preparing the group iii-v quantum dot of the first aspect, wherein the group iii-v quantum dot has an average particle size a and a D90 particle size B.
The embodiment of the application at least comprises the following beneficial effects:
the organic phosphine with lone pair electrons has certain coordination capacity with cations in the III family cation precursor, and the organic phosphine with lone pair electrons reacts with the III family cation precursor to generate an intermediate, wherein the activity of the intermediate is higher than that of the III family cation precursor. The first solution and the V-group anion precursor are mixed and reacted, the number of generated nano-clusters of the quantum dot core is increased, the size distribution of the quantum dot core formation stage is improved, the quantum dot core growth to a large size is promoted, and the finally formed quantum dot is narrow in size distribution and large in size.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a spectrum of visible light absorption of group III-V quantum dots of example 1 of the present application;
FIG. 2 is a spectrum of visible light absorption of group III-V quantum dots of example 2 herein;
FIG. 3 is a spectrum of visible light absorption of group III-V quantum dots of example 3 herein;
FIG. 4 is a spectrum of visible light absorption of group III-V quantum dots of example 4 herein;
FIG. 5 is a spectrum of visible light absorption of the group III-V quantum dots of comparative example 1 of the present application;
fig. 6 is a visible light absorption spectrum of group iii-v quantum dots of comparative example 2 of the present application.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under 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 following is a detailed description of the group iii-v quantum dots and the preparation method thereof according to the embodiments of the present application:
in a first aspect, embodiments of the present application provide a method for preparing a group iii-v quantum dot, including:
(1) The method comprises the following steps of reacting a III group cation precursor with organic phosphine with lone pair electrons in a first solvent to obtain a first solution.
In the research of the inventor, the group v anion precursor has much higher reactivity than the group iii cation precursor, and the imbalance of the reaction rate results in the wide size distribution and the generally smaller size of the quantum dot. In the embodiment of the application, the organic phosphine with lone pair electrons has certain coordination capacity with cations in the III family cation precursor, the organic phosphine with lone pair electrons reacts with the III family cation precursor to generate an intermediate, and the activity of the intermediate is greater than that of the III family cation precursor.
The organic phosphine having a lone pair of electrons means that the P atom contains a lone pair of electrons and the P atom is bonded with an organic group.
In some embodiments, the organic group in the organophosphine having a lone pair of electrons comprises at least one of a chain group, an alicyclic group, and an aromatic group. Alternatively, the organic phosphine having a lone pair of electrons comprises at least one of tris (1-adamantyl) phosphine, n-butyl bis (1-adamantyl) phosphine, cyclohexyl di-t-butyl phosphine, and t-butyl dicyclohexylphosphine, wherein the tris (1-adamantyl) phosphine has the following structural formula:
in some embodiments, the temperature at which the group iii cation precursor is reacted with the organophosphine having a lone pair of electrons in the first solvent is from 60 ℃ to 220 ℃.
At the temperature of 60-220 ℃, the reaction degree of the III group cation precursor and the organic phosphine with the lone pair of electrons is high, and other side reactions can not occur.
Optionally, the temperature at which the group iii cation precursor is reacted with the organophosphine having a lone pair of electrons in the first solvent is in a range between any or any of 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃ and 220 ℃.
Further, the reaction of the group iii cation precursor with the organophosphine having a lone pair of electrons in the first solvent is carried out in an inert atmosphere.
The group III cation precursor and the organic phosphine with the lone pair of electrons react in the inert atmosphere, and the inert atmosphere is used as a protective atmosphere to further prevent side reactions. The reaction of the group iii cation precursor with the organic phosphine having a lone pair of electrons in the first solvent may be carried out in air.
In some embodiments, the step of reacting a group iii cation precursor with an organic phosphine having a lone pair of electrons in a first solvent to obtain a first solution comprises: mixing a III group cation precursor with a first solvent to obtain a first mixed solution, and then mixing the first mixed solution with organic phosphine with lone pair electrons.
Illustratively, the concentration of the group III cation precursor in the first mixed solution is from 0.01 to 100mmol/mL, e.g., 0.01mmol/mL, 0.05mmol/mL, 0.1mmol/mL, 0.5mmol/mL, 1mmol/mL, 5mmol/mL, 10mmol/mL, 20mmol/mL, 30mmol/mL, 40mmol/mL, 50mmol/mL, 60mmol/mL, 70mmol/mL, 80mmol/mL, 90mmol/mL, or 100mmol/mL.
In other embodiments, the step of reacting a group iii cation precursor with an organic phosphine having a lone pair of electrons in a first solvent to obtain a first solution comprises: mixing organic phosphine with lone pair electrons with a first solvent to obtain a second mixed solution, and then mixing the second mixed solution with a III-group cation precursor.
Illustratively, the concentration of the organophosphine having a lone electron pair in the second mixed solution is from 0.01 to 100mmol/mL, for example, 0.01mmol/mL, 0.05mmol/mL, 0.1mmol/mL, 0.5mmol/mL, 1mmol/mL, 5mmol/mL, 10mmol/mL, 20mmol/mL, 30mmol/mL, 40mmol/mL, 50mmol/mL, 60mmol/mL, 70mmol/mL, 80mmol/mL, 90mmol/mL, or 100mmol/mL.
It should be noted that the first solvent does not participate in the reaction of the group iii cation precursor with the organophosphine having a lone pair of electrons. Optionally, the first solvent comprises at least one of 1-octadecene, chlorobenzene, chloroform, and dichloromethane.
Illustratively, the cation of the group iii cation precursor includes at least one of an Al ion, a Ga ion, and an In ion. It should be noted that the cation of the group iii cation precursor may have a valence of +2 or +3, and the valence of the cation of the group iii cation precursor is not specifically limited in the embodiment of the present application.
The group III cation precursor may have, in addition to the group III cation, an anion for maintaining the group III cation precursor electrically neutral, optionally the anion in the group III cation precursor may include F - 、Cl - 、OH - 、CH 3 COO - And CO 3 2- At least one of (1).
(2) And mixing the first solution and the V-group anion precursor for reaction to generate a quantum dot core and growing the quantum dot core.
The organic phosphine with lone pair electrons reacts with the precursor of the III group cation, and the activity of the generated intermediate is greater than that of the precursor of the III group cation. The first solution and the V-group anion precursor are mixed and reacted, the number of generated nano-clusters of the quantum dot core is increased, the size distribution of the quantum dot core formation stage is improved, the quantum dot core growth to a large size is promoted, and the finally formed quantum dot is narrow in size distribution and large in size.
It should be noted that, the inventors of the present application found in the research that if the content of the organic phosphine having a lone pair electron is too large, the quantum dot is prevented from growing to a large size. It is probably because the organophosphine having a lone pair electron is not likely to be excessive because the organophosphine having a lone pair electron is large in steric hindrance and affects the growth of the quantum dot as a ligand. Illustratively, in the present embodiments, the weight of the organophosphine having a lone pair of electrons is 1 to 20% of the weight of the group v anion precursor, e.g., 1%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, or 20%.
In some embodiments, the anion in the group v anion precursor comprises at least one of an N ion, a P ion, and an As ion.
Illustratively, the group V anion precursor comprises Na 3 P、PCl 3 、H 3 P and Na 3 At least one of As.
In some embodiments, the temperature at which the reaction produces the quantum dot core is 60 to 220 ℃.
At the temperature of 60-220 ℃, the intermediate in the first solution and the V-group anion precursor have high reaction degree, and no other side reaction occurs.
Optionally, the temperature at which the reaction produces the quantum dot core is any one of 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃ and 220 ℃, or a range between any two.
The temperature range of 160-300 ℃ is more beneficial to the growth of quantum dot cores, so that the prepared quantum dots have larger size. Optionally, the temperature of growth is 160-300 ℃, e.g., is any one of 160 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃ and 300 ℃, or a range between any two.
Further, the mixing reaction of the first solution and the group v anion precursor is performed in an inert atmosphere.
The intermediate in the first solution reacts with the group v anion precursor in an inert atmosphere, which serves as a protective atmosphere to further prevent side reactions.
Optionally, the growing of the quantum dot core is also performed in an inert atmosphere.
The first solution may be mixed with the group v anion precursor, or may be mixed with the group v anion precursor in air.
In some embodiments, the group v anion precursor can be mixed with the second solvent to form a third mixed solution, and then mixed with the first solution.
Optionally, the second solvent comprises at least one of 1-octadecene, chlorobenzene, chloroform, and dichloromethane.
Alternatively, the concentration of the group V anion precursor in the third mixed solution is 0.01 to 100mmol/mL, for example, 0.01mmol/mL, 0.05mmol/mL, 0.1mmol/mL, 0.5mmol/mL, 1mmol/mL, 5mmol/mL, 10mmol/mL, 20mmol/mL, 30mmol/mL, 40mmol/mL, 50mmol/mL, 60mmol/mL, 70mmol/mL, 80mmol/mL, 90mmol/mL, or 100mmol/mL.
In a second aspect, embodiments of the present application provide a group iii-v quantum dot, which is prepared by the method for preparing the group iii-v quantum dot of the embodiment of the first aspect.
The group iii-v quantum dots and the preparation method thereof according to the present application are further described in detail with reference to the following examples.
Example 1
This example provides a method for preparing iii-v group quantum dots, which comprises the following steps:
s1, adding 0.72mmol of In (Ac) 3 2.16mmol of Oleic Acid (OA) and 3.6mL of 1-Octadecene (ODE) were mixed, and the mixture was cooled to 200 ℃ under a nitrogen atmosphereReacting at the temperature of (1) for 2h, and cooling to 130 ℃ to obtain a first mixed solution.
S2, adding 0.05mM of tri (1-adamantyl) phosphine into the first mixed solution obtained in the step S1, and stirring for 0.5h at the temperature of 130 ℃ in a nitrogen atmosphere to obtain a first solution.
S3-0.36 mM of tris (trimethylsilanyl) phosphine (TMS) 3 P) was injected into the first solution obtained in step S2, and reacted at a temperature of 130 ℃ for 1 hour in an atmosphere of nitrogen.
And S4, heating the solution obtained in the step S3 to 260 ℃, and reacting for 20min in a nitrogen atmosphere to obtain the III-V family quantum dots.
Example 2
This example provides a method for preparing iii-v group quantum dots, which comprises the following steps:
s1, adding 0.72mmol of In (Ac) 3 Mixing 2.16mmol of Oleic Acid (OA) and 3.6mL of 1-Octadecene (ODE), reacting at 120 ℃ for 3 hours in a nitrogen atmosphere, and cooling to 130 ℃ to obtain a first mixed solution.
S2, adding 0.05mM of n-butyl di (1-adamantyl) phosphine into the first mixed solution obtained in the step S1, and stirring for 0.5h at the temperature of 130 ℃ in a nitrogen atmosphere to obtain a first solution.
S3, adding 0.36mM of Na 3 As is injected into the first solution obtained in the step S2, and reacts at a temperature of 130 ℃ for 1h in an atmosphere of nitrogen.
And S4, heating the solution obtained in the step S3 to 240 ℃, and reacting for 20min in a nitrogen atmosphere to obtain the III-V family quantum dots.
Example 3
This example provides a method for preparing iii-v quantum dots, comprising the steps of:
s1, adding 0.8mmol of GaCl 3 2.5mmol of Oleic Acid (OA) and 4mL of chlorobenzene are mixed, and the mixture reacts at the temperature of 180 ℃ for 3 hours in the environment of nitrogen atmosphere and then is cooled to 130 ℃ to obtain a first mixed solution.
S2, adding 0.05mM of cyclohexyl di-tert-butylphosphine into the first mixed solution obtained in the step S1, and stirring for 0.5h at the temperature of 130 ℃ in a nitrogen atmosphere to obtain a first solution.
S3, adding 0.36mM of Na 3 As is injected into the first solution obtained in the step S2, and reacts at a temperature of 130 ℃ for 1h in an atmosphere of nitrogen.
And S4, heating the solution obtained in the step S3 to 240 ℃, and reacting for 20min in a nitrogen atmosphere to obtain the III-V family quantum dots.
Example 4
This example provides a method of making group iii-v quantum dots, which differs from example 1 only in the substitution of tris (1-adamantyl) phosphine of example 1 for t-butyldicyclohexylphosphine.
Comparative example 1
Comparative example 1 provides a method for preparing iii-v group quantum dots, which is different from example 1 only in that comparative example 1 omits step S2.
Comparative example 2
Comparative example 2 provides a method for preparing iii-v group quantum dots, which is different from example 2 only in that comparative example 1 omits the step S2.
Test example 1
The visible light absorption spectra of the group iii-v quantum dots prepared in examples 1 to 4 and comparative examples 1 to 2 were measured to obtain the wavelength-absorbance spectra shown in fig. 1 to 6.
As can be seen from a comparison between fig. 1 and fig. 5, the maximum absorption wavelength of the iii-v group quantum dot prepared in example 1 of the present application is 564nm, and the maximum absorption wavelength of the iii-v group quantum dot prepared in comparative example 1 is 542nm, and the spectrogram of the iii-v group quantum dot prepared in example 1 of the present application is red-shifted (longer in wavelength) compared to the spectrogram of comparative example 1, which indicates that the size of the iii-v group quantum dot is larger due to the addition of the organophosphine having a lone pair electron in example 1. It can be seen from fig. 1 that the wavelength =0.69 for the wavelength/trough corresponding to the peak, and from fig. 5 that the wavelength =0.77 for the wavelength/trough corresponding to the peak, the size distribution of the iii-v group quantum dots corresponding to fig. 1 is more concentrated, and the organic phosphine having a lone pair electron is added in example 1 of the present application, so that the size distribution of the quantum dots is narrower.
As can be seen from comparing fig. 2 and fig. 6, the maximum absorption wavelength of the iii-v group quantum dot prepared in example 2 of the present application is 565nm, the wavelength =0.79 corresponding to the wavelength/trough corresponding to the peak, the maximum absorption wavelength of the iii-v group quantum dot prepared in comparative example 2 is 545nm, the wavelength =0.77 corresponding to the wavelength/trough corresponding to the peak, and the ratio of the wavelength/trough corresponding to the wavelength corresponding to the peak of the iii-v group quantum dot in example 2 of the present application is not much different from that of the iii-v group quantum dot in example 2 of the present application, but the spectrum of the iii-v group quantum dot in example 2 of the present application is red-shifted (longer in wavelength) compared with the spectrum of comparative example 2, which indicates that the organic phosphine having a lone pair electron is added in example 2 so that the iii-v group quantum dot is concentrated in a larger size range.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (6)
1. A method for preparing III-V group quantum dots is characterized by comprising the following steps:
reacting a III-group cation precursor with organic phosphine with lone pair electrons in a first solvent to obtain a first solution;
mixing the first solution and a V-group anion precursor for reaction to generate a quantum dot core and growing the quantum dot core;
the cation of the group III cation precursor is selected from at least one of Ga ions and In ions;
the anion in the group V anion precursor is selected from at least one of P ion and As ion;
the organic phosphine with a lone pair of electrons is selected from at least one of tri (1-adamantyl) phosphine, n-butyl di (1-adamantyl) phosphine, cyclohexyl di-tert-butyl phosphine and tert-butyl dicyclohexyl phosphine;
the first solvent is at least one selected from the group consisting of 1-octadecene, chlorobenzene, chloroform and dichloromethane.
2. The method of claim 1, wherein the group iii cation precursor is reacted with the organic phosphine having a lone pair of electrons in the first solvent at a temperature of 60-220 ℃.
3. The method of claim 2, wherein the reacting the group iii cation precursor with the organophosphine having a lone pair of electrons in the first solvent is performed in an inert atmosphere.
4. The method of making group iii-v quantum dots of any of claims 1~2, wherein the temperature of the reaction to form the quantum dot core is 60 to 220 ℃.
5. The method for preparing group III-V quantum dots according to any one of claims 1~2, wherein the temperature of growth is 160 to 300 ℃.
6. The method of preparing group iii-v quantum dots according to any of claims 1~2, wherein the mixing reaction of the first solution and group v anion precursor is performed in an inert atmosphere.
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| CN110373187A (en) * | 2019-07-01 | 2019-10-25 | 浙江大学 | The preparation method of iii-v quantum dot |
| KR102071688B1 (en) * | 2019-06-07 | 2020-04-01 | 주식회사 신아티앤씨 | Quantum dot particles comprising quantum dot ligands having thiol group and, hydroxy group or carboxyl group, and composition comprising the quantum dot particles, and preparation method of the quantum dot ligands |
| CN110964506A (en) * | 2018-09-30 | 2020-04-07 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN112538353A (en) * | 2019-09-20 | 2021-03-23 | Tcl集团股份有限公司 | Preparation method of quantum dot material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110964506A (en) * | 2018-09-30 | 2020-04-07 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| KR102071688B1 (en) * | 2019-06-07 | 2020-04-01 | 주식회사 신아티앤씨 | Quantum dot particles comprising quantum dot ligands having thiol group and, hydroxy group or carboxyl group, and composition comprising the quantum dot particles, and preparation method of the quantum dot ligands |
| CN110373187A (en) * | 2019-07-01 | 2019-10-25 | 浙江大学 | The preparation method of iii-v quantum dot |
| CN112538353A (en) * | 2019-09-20 | 2021-03-23 | Tcl集团股份有限公司 | Preparation method of quantum dot material |
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| Observation of Molecules Adsorbed on III-V Semiconductor Quantum Dots by Surface-Enhanced Raman Scatterin;Lucia G. Quagliano;《J. AM. CHEM. SOC.》;20040518;第126卷;第7393-7398页 * |
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