CN115710505A - Method for reducing fluorescence half-peak width of core-shell type indium phosphide quantum dots - Google Patents
Method for reducing fluorescence half-peak width of core-shell type indium phosphide quantum dots Download PDFInfo
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical class [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000011258 core-shell material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 30
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- 229910052725 zinc Inorganic materials 0.000 claims abstract description 34
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- 229910052738 indium Inorganic materials 0.000 claims abstract description 23
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003446 ligand Substances 0.000 claims abstract description 22
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- 238000002156 mixing Methods 0.000 claims abstract description 10
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- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 7
- 239000011574 phosphorus Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
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- 229940057499 anhydrous zinc acetate Drugs 0.000 claims description 6
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 claims description 6
- 229940102001 zinc bromide Drugs 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 5
- RMUKCGUDVKEQPL-UHFFFAOYSA-K triiodoindigane Chemical compound I[In](I)I RMUKCGUDVKEQPL-UHFFFAOYSA-K 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- XVDBWWRIXBMVJV-UHFFFAOYSA-N n-[bis(dimethylamino)phosphanyl]-n-methylmethanamine Chemical compound CN(C)P(N(C)C)N(C)C XVDBWWRIXBMVJV-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- FDIOSTIIZGWENY-UHFFFAOYSA-N n-[bis(diethylamino)phosphanyl]-n-ethylethanamine Chemical compound CCN(CC)P(N(CC)CC)N(CC)CC FDIOSTIIZGWENY-UHFFFAOYSA-N 0.000 claims description 3
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical compound CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 claims description 3
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- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 3
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 2
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 2
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- JKNHZOAONLKYQL-UHFFFAOYSA-K tribromoindigane Chemical compound Br[In](Br)Br JKNHZOAONLKYQL-UHFFFAOYSA-K 0.000 claims description 2
- 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 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
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- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 5
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Abstract
The invention provides a method for reducing fluorescence half-peak width of core-shell type indium phosphide quantum dots, which comprises the following steps: firstly, mixing an indium source and a phosphorus source in the presence of a raw material zinc halide, and reacting to obtain an indium phosphide nucleus; cooling to room temperature to purify and dissolve the indium phosphide nucleus to obtain a first product; secondly, adding ligand zinc halide into the first product, and then heating to the coating temperature of the shell layer; and finally, adding a zinc source, a selenium source and a sulfur source into the product obtained in the previous step for shell coating to obtain the core-shell type indium phosphide quantum dot. In the intermediate step of the synthesis of the core-shell type indium phosphide quantum dot, the surface modification of the quantum dot is carried out through ligand zinc halide, so that the surface defect of the indium phosphide quantum dot core is passivated, the Ostwald ripening in the heating process is relieved, and the obtained indium phosphide quantum dot has the advantages of narrower fluorescence half-peak width, environmental friendliness and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials and technologies, and particularly relates to a method for reducing fluorescence half-peak width of core-shell type indium phosphide quantum dots.
Background
Colloidal Quantum Dots (QDs) have wide applications due to their unique optical and electrical properties, comprises a display, an illumination,Bio-imaging, solar cells, etc. At present, quantum dots are mainly classified into three major categories: cadmium-based (CdSe, cdS and CdTe), cadmium-free (InP, cuInS) 2 Etc.) and novel perovskites (CsPbBr) 3 、CH 3 NH 3 PbBr 3 Etc.). Cadmium-based quantum dots and metal halide perovskites (CsPbX) for the needs of display technology 3 Wherein X = Cl, br or I) is well developed. However, cadmium-based and metal halide perovskites contain heavy metals, the release of which in the environment can pose potential hazards. Thus, european directive on restriction of hazardous substances (RoHS) limits the sale and use of products containing heavy metals. In the cadmium-free quantum dots, the Bohr exciton radius of the indium phosphide is 9.6nm, the band gap is 1.34eV, and the emission wavelength of the indium phosphide can cover the blue to near infrared region, which attracts people to pay attention.
However, the development of indium phosphide quantum dots at the present stage still lags far behind cadmium-based and novel perovskite quantum dots, mainly manifested in that they have a more broadened fluorescence half-width (FWHM) and a lower photoluminescence quantum yield (PLQY). At present, the overall fluorescence emission half-peak width of the CdSe quantum dot with better quality can be kept below 30nm and is almost consistent with the fluorescence emission half-peak width of a single quantum dot. However, for the indium phosphide quantum dot system, the half-peak width of the fluorescence peak of a single quantum dot is almost similar to that of a cadmium group, but the whole fluorescence emission half-peak width of the solution is hardly lower than 45nm, which is mainly due to the high reactivity of the phosphorus precursor. The method for synthesizing the quantum dots comprises a heating method, a thermal injection method, a microwave-assisted synthesis method and the like, wherein the thermal injection method is most commonly used, the monomer concentration is high at the moment of high-temperature injection, the reaction is rapidly nucleated, and then the concentration is rapidly reduced, so that the nucleation is stopped, and the growth is continued. The high reactivity of the phosphorus precursor makes the phosphorus precursor completely consumed in the nucleation step, and the monomer is not sufficiently supplied in the growth stage, so that the growth of the indium phosphide quantum dots can enter the Ostwald ripening stage prematurely, thereby causing the size polydispersity. The size affects the exciton energy level of the quantum dots, so that if the quantum dots are completely single in size, their exciton energy is completely single, and the corresponding emitted photons are completely single. The heterogeneity of the sample caused by the synthesis causes the emitted photons to be not single and show a wider emission peak in the spectrum. Therefore, the size distribution of the quantum dots can be judged by the emission peak width of the quantum dots.
At present, size sorting operation is generally adopted for broadening of half-peak width caused by Ostwald ripening in the indium phosphide synthesis process, namely, centrifugal separation is carried out according to different solubilities of quantum dots with different sizes in poor solvents, but the method is complicated. Therefore, it is very important to find a simple method for reducing the half-width of fluorescence emission.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method capable of effectively reducing the fluorescence half-peak width of the core-shell type indium phosphide quantum dot.
In order to solve the technical problems, the invention adopts the following technical scheme: the method for reducing the fluorescence half-peak width of the core-shell type indium phosphide quantum dot comprises the following steps:
s1, mixing an indium source and a phosphorus source in the presence of a raw material zinc halide, and reacting to obtain an indium phosphide nucleus; cooling to room temperature to purify and dissolve the indium phosphide nucleus to obtain a first product;
s2, adding ligand zinc halide into the first product, and then heating to a shell coating temperature;
and S3, adding a zinc source, a selenium source and a sulfur source into the product obtained in the step S2 for shell coating to obtain the core-shell type indium phosphide quantum dot.
The general idea of the method for reducing the fluorescence half-peak width of the core-shell type indium phosphide quantum dot provided by the invention is as follows: in the intermediate step of the reaction for preparing the core-shell type indium phosphide by the two-pot method, namely the temperature rise step after purifying the indium phosphide core and before coating the shell layer (ZnSeS/ZnS), a certain amount of ligand zinc halide is introduced. On one hand, the ligand zinc halide is added, so that the condition that the ligand on the surface of the indium phosphide quantum dot continuously falls off in the heating process can be relieved; on the other hand, ligand zinc halide is combined with indium and phosphorus which are not completely combined on the surface, ostwald ripening in the heating process is inhibited, the particle size distribution is more uniform, and the spectrum shows that the full width at half maximum (FWHM) of the fluorescence peak is smaller.
On the basis of the technical scheme, in the step S1, the raw material zinc halide is selected from one or more of zinc chloride, zinc bromide and zinc iodide; the phosphorus source is one or more of tri (trimethylsilyl) phosphine, tri (dimethylamino) phosphine and tri (diethylamino) phosphine; the indium source is selected from one or more of indium chloride, indium bromide, indium iodide and indium acetate.
Preferably, the phosphorus source is selected from tris (dimethylamino) phosphine or tris (diethylamino) phosphine, which have the advantages of low cost and low toxicity.
On the basis of the technical scheme, in the step S1, the reaction temperature is 100-250 ℃ and the reaction time is 1 min-1 h.
On the basis of the above technical solution, in the step S1, the purifying and dissolving the indium phosphide core includes: the indium phosphide nucleus is firstly placed in a poor solvent and centrifuged at high speed until the indium phosphide nucleus is completely precipitated, the supernatant is removed, and then the good solvent is added into the precipitate to be completely dissolved.
Further, the poor solvent is selected from one or more of absolute ethyl alcohol, acetone and methanol; the good solvent is selected from one or more of n-hexane, toluene and chloroform.
On the basis of the above technical solution, in the step S2, the ligand zinc halide is selected from one or a combination of zinc chloride, zinc bromide and zinc iodide.
Preferably, the ratio of the addition amount of the ligand zinc halide to the amount of the indium iodide substance is 1; within the range of the addition amount, the fluorescent peak of the indium phosphide quantum dot is obviously improved. More preferably, the ratio of the added amount of the ligand zinc halide to the amount of the indium iodide material is 1:3.6. in this case, the effect of improving the fluorescence peak of the indium phosphide quantum dot was most significant.
Further, the ligand zinc halide is added to the first product in the step S1 together with oleylamine and octadecene. Wherein, octadecene is used as a reaction solvent, and oleylamine has the functions of both the solvent and the ligand.
Furthermore, the adding temperature of the ligand zinc halide can be 20-120 ℃, and the heating rate is 20-50 ℃/min. Preferably, the adding temperature of the ligand zinc halide is 20-30 ℃, and the heating rate is 30 ℃/min. By controlling the heating rate, the heating time is shortened as much as possible, and the adverse effect on the particle size distribution of the quantum dots caused by the quantum dots always in the curing stage is avoided.
On the basis of the technical scheme, in the step S3, the zinc source is selected from one or more of zinc acetate dihydrate, zinc stearate and anhydrous zinc acetate; the sulfur source is selected from one or more of sulfur powder, 1-dodecanethiol and octanethiol; the selenium source is selected from selenium powder and/or selenium oxide.
Further, in the step S3, the temperature of the shell coating is 180-320 ℃, and the reaction time of the shell coating is 20 min-2 h.
Compared with the prior art, the invention has the beneficial effects that: according to the method for reducing the fluorescence half-peak width of the core-shell type indium phosphide quantum dot, ligand zinc halide is doped in a certain proportion in the intermediate step of indium phosphide nucleation and shell coating, and the zinc halide is absorbed on the surface of the quantum dot as a ligand, so that Ostwald ripening can be well relieved. And then coating ZnSeS and ZnS shells, and obviously reducing the half-peak width of the obtained quantum dots, which shows that the quantum dots are more uniform in size, and the TEM also more visually proves the improvement of the size polydispersity. In addition, the indium phosphide quantum dot prepared by the method has the advantages of no heavy metal element, environmental friendliness and the like, and is suitable for popularization and application.
Drawings
FIG. 1 is a graph showing an ultraviolet absorption spectrum and a fluorescence spectrum of a core-shell type InP quantum dot obtained in example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of a core-shell type InP quantum dot prepared in example 1 of the present invention;
FIG. 3 is a graph of the ultraviolet absorption spectrum and the fluorescence spectrum of the core-shell type indium phosphide quantum dot prepared in example 2 of the present invention;
FIG. 4 is a transmission electron microscope image of the core-shell type InP quantum dot prepared in example 2 of the present invention;
FIG. 5 is a graph showing the UV absorption spectrum and the fluorescence spectrum of a core-shell type InP quantum dot obtained in example 3 of the present invention;
FIG. 6 is a transmission electron microscope image of core-shell type InP quantum dots prepared in example 3 of the present invention;
FIG. 7 is a graph showing an ultraviolet absorption spectrum and a fluorescence spectrum of an undoped core-shell type InP quantum dot prepared according to a comparative example of the present invention;
FIG. 8 is a transmission electron microscope image of an undoped core-shell type InP quantum dot prepared by the comparative example of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, shall fall within the scope of protection of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1
Preparation of core-shell type indium phosphide quantum dot by doping zinc iodide with indium source molar weight of 1/3.6
Step 1: 1.7839g indium triiodide and 1.2g zinc chloride were taken and dissolved in a four-necked flask with 24mL oleylamine, evacuated for 1h, warmed to 180 ℃ under nitrogen, 2.6mL tri-n-octylphosphine (TOP) solution containing 7.7mmol tris (dimethylamino) phosphine was added and reacted at 180 ℃ for 2min, during which time the solution changed color from colorless to orange to brown. After 2min, the solution was immediately cooled to room temperature, and the obtained indium phosphide nuclei were mixed with excess absolute ethanol, and the mixture was centrifuged at high speed (9000 rpm,5 min) to obtain precipitates, and then the indium phosphide nuclei were completely dissolved in n-hexane.
And 2, step: the indium phosphide nucleus dissolved in n-hexane in step 1 was mixed with 3mL of oleylamine, 3mL of octadecene and zinc iodide (1 mmol) in an indium source molar amount of 1/3.6 in a 50mL four-necked flask, evacuated at room temperature and then heated to 160 ℃ under an atmosphere of argon (the whole apparatus was placed in an anhydrous oxygen-free atmosphere). When the temperature reached 70 ℃, the formed n-hexane vapor was collected by a condensation reflux apparatus to further raise the temperature of the reaction system.
And step 3: when the reaction temperature of the step 2 is increased to 160 ℃, rapidly injecting a zinc precursor (0.8 mmol of anhydrous zinc acetate dissolved in 0.5mL of oleic acid and 2mL of octadecene) and a Se + S precursor (0.4 mmol of Se powder and 0.45mmol of S powder dissolved in 1mL of tri-n-octylphosphine) into a reaction bottle, rapidly increasing the temperature to 270 ℃, and reacting at 270 ℃ for 30min; injecting zinc precursor (0.8 mmol of anhydrous zinc acetate dissolved in 0.5mL of oleic acid and 2mL of octadecene) and Se + S precursor (0.3 mmol of Se powder and 0.9mmol of S powder dissolved in 1mL of tri-n-octylphosphine) for the second time, and reacting at 280 ℃ for 30min; injecting zinc precursor (0.8 mmol of anhydrous zinc acetate dissolved in 0.5mL of oleic acid and 2mL of octadecene) and Se + S precursor (0.2 mmol of Se powder and 1.35mmol of S powder dissolved in 1mL of tri-n-octylphosphine) for the third time, and reacting at 290 ℃ for 30min; injecting a zinc precursor (0.8 mmol of anhydrous zinc acetate dissolved in 0.5mL of oleic acid and 2mL of octadecene) and a Se + S precursor (0.1 mmol of Se powder and 1.8mmol of S powder dissolved in 1mL of tri-n-octylphosphine) for the fourth time, reacting at 300 ℃ for 30min, rapidly cooling to 230 ℃, adding 0.75mL of octanethiol, reacting at 230 ℃ for 30min, cooling to 190 ℃, adding 1mmol of zinc acetate dihydrate, reacting at 190 ℃ for 1h, and cooling to room temperature to obtain the core-shell type indium phosphide quantum dots. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, centrifuging, precipitating, purifying, and dispersing in n-hexane again.
Example 2
Preparation of core-shell type indium phosphide quantum dot by doping zinc bromide with indium source molar weight of 1/3.6
In addition to example 1, zinc iodide in an indium source molar amount of 1/3.6 in step 2 was replaced with zinc bromide (1 mmol) in an equivalent amount, and other steps and conditions were not changed to prepare core-shell type indium phosphide quantum dots. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, centrifuging, precipitating, purifying, and dispersing in n-hexane again.
Example 3
Preparation of core-shell type indium phosphide quantum dot by doping zinc chloride with indium source molar weight of 1/3.6
In addition to example 1, zinc iodide in an indium source molar amount of 1/3.6 in step 2 was replaced with zinc chloride (1 mmol) in an equivalent amount, and other steps and conditions were not changed to prepare core-shell type indium phosphide quantum dots. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, centrifuging, precipitating, purifying, and dispersing in n-hexane again.
Example 4
Preparation of core-shell type indium phosphide quantum dot by doping zinc iodide with indium source molar weight of 5/36
On the basis of example 1, zinc iodide with an indium source molar amount of 1/3.6 in step 2 was replaced with zinc iodide (0.5 mmol) with an indium source molar amount of 5/36, and other steps and conditions were not changed to prepare core-shell type indium phosphide quantum dots. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, centrifuging, precipitating, purifying, and dispersing in n-hexane again.
Example 5
Preparation of core-shell type indium phosphide quantum dot by doping zinc iodide with indium source molar weight of 3/3.6
On the basis of example 1, zinc iodide with the indium source molar quantity of 1/3.6 in step 2 is replaced by zinc iodide (3 mmol) with the indium source molar quantity of 3/3.6, and other steps and conditions are not changed, so that the core-shell type indium phosphide quantum dot is prepared. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, centrifuging, precipitating, purifying, and dispersing in n-hexane again.
Example 6
Preparation of core-shell type indium phosphide quantum dot by doping zinc iodide with indium source molar weight of 1/36
On the basis of example 1, zinc iodide with an indium source molar amount of 1/3.6 in step 2 was replaced with zinc iodide (0.1 mmol) with an indium source molar amount of 1/36, and other steps and conditions were not changed to prepare core-shell type indium phosphide quantum dots. And (3) mixing the obtained quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, purifying by centrifugal precipitation, and dispersing in n-hexane again.
Comparative example
Undoped preparation of core-shell type indium phosphide quantum dots
On the basis of the example 1, the step 2 is adjusted, the addition of zinc iodide with the indium source molar weight of 1/3.6 is removed, and other steps and conditions are not changed, so that the undoped core-shell type indium phosphide quantum dot is prepared.
And (2) mixing the obtained core-shell type indium phosphide quantum dots with absolute ethyl alcohol according to the volume ratio of 1:7, purifying by centrifugal precipitation, and dispersing in n-hexane again.
Characterization and Performance
Ultraviolet absorption and fluorescence spectrograms and projection electron micrographs of the ligand zinc halide doped core-shell type indium phosphide quantum dots prepared in examples 1-3 are shown in figures 1-6. It can be seen that the quantum dots prepared in examples 1-3 have better size uniformity than the undoped quantum dots prepared in the comparative example.
Statistics and calculations are performed on the ultraviolet absorption peak, the fluorescence emission peak, the half-peak width and the quantum yield of the quantum dots prepared in the above examples and comparative examples, and the results are shown in the following table 1:
wherein, a Cary Eclipse fluorescence spectrophotometer (Agilent technology) is adopted as a testing instrument of the half-peak width, and the concentration of the testing solution is 0.5mg/mL.
Table 1: optical Properties of Quantum dots
As can be seen from the above table, the fluorescent emission peak position of the indium phosphide quantum dots prepared by doping ligand zinc halide in the embodiments 1-6 of the invention is still kept near 527nm, and the dots emit green light. Compared with the comparative example 1, after the ligand zinc halide is added in a certain proportion in the examples 1-6, the half-peak width of the quantum dot is obviously narrowed from 50nm to 42-46 nm. This shows that the method provided by the invention can obviously improve the size uniformity of the core-shell type indium phosphide quantum dots, and the method can be more intuitively sensed from TEM.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method for reducing fluorescence half-peak width of core-shell type indium phosphide quantum dots comprises the following steps:
s1, mixing an indium source and a phosphorus source in the presence of a raw material zinc halide, and reacting to obtain an indium phosphide nucleus; cooling to room temperature to purify and dissolve the indium phosphide core to obtain a first product;
s2, adding ligand zinc halide into the first product, and then heating to a shell coating temperature;
and S3, adding a zinc source, a selenium source and a sulfur source into the product obtained in the step S2 for shell coating to obtain the core-shell type indium phosphide quantum dot.
2. The method according to claim 1, wherein in step S1, the raw material zinc halide is selected from one or more of zinc chloride, zinc bromide and zinc iodide; the phosphorus source is one or more of tri (trimethylsilyl) phosphine, tri (dimethylamino) phosphine and tri (diethylamino) phosphine; the indium source is selected from one or more of indium chloride, indium bromide, indium iodide and indium acetate.
3. The method according to claim 2, wherein in step S1, the reaction temperature is 100-250 ℃ and the reaction time is 1 min-1 h.
4. The method of claim 1, wherein the step S1 of purifying and dissolving the indium phosphide core comprises: the indium phosphide nucleus is firstly placed in a poor solvent and centrifuged at high speed until the indium phosphide nucleus is completely precipitated, the supernatant is removed, and then the good solvent is added into the precipitate to be completely dissolved.
5. The method according to claim 4, wherein the poor solvent is selected from one or more of absolute ethanol, acetone and methanol; the good solvent is selected from one or more of n-hexane, toluene and chloroform.
6. The method of claim 1, wherein in step S2, the ligand zinc halide is selected from one or more of zinc chloride, zinc bromide and zinc iodide.
7. The method according to claim 6, wherein the ratio of the addition amount of the ligand zinc halide to the amount of the indium source substance is 1.
8. The method according to claim 7, wherein the temperature increase rate in step S2 is 20 to 50 ℃/min.
9. The method according to claim 1, wherein in step S3, the zinc source is selected from one or more of zinc acetate dihydrate, zinc stearate, and anhydrous zinc acetate; the sulfur source is selected from one or more of sulfur powder, 1-dodecanethiol and octanethiol; the selenium source is selected from selenium powder and/or selenium oxide.
10. The method of claim 9, wherein the temperature of the shell coating is 180 to 320 ℃ and the reaction time of the shell coating is 20min to 2h.
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| CN118165730A (en) * | 2024-05-13 | 2024-06-11 | 北京北达聚邦科技有限公司 | Indium phosphide quantum dot and preparation method thereof |
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| CN113512416A (en) * | 2021-07-27 | 2021-10-19 | 福州大学 | Preparation method of Ga-doped water-soluble InP quantum dots |
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| CN112608752A (en) * | 2020-12-21 | 2021-04-06 | 深圳扑浪创新科技有限公司 | Core-shell InP/ZnSe/ZnS quantum dot and preparation method thereof |
| CN113512416A (en) * | 2021-07-27 | 2021-10-19 | 福州大学 | Preparation method of Ga-doped water-soluble InP quantum dots |
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