CN110697766A - Preparation method of zinc-doped lead sulfide quantum dots - Google Patents
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Abstract
The invention provides a preparation method of zinc-doped lead sulfide quantum dots, which comprises the following steps: step 1, introducing protective gas into a zinc source, a lead source, organic acid and/or organic amine under the condition of stirring, and heating until the protective gas is dissolved to obtain a mixed precursor solution of zinc and lead; step 2, heating the solution to 120-150 ℃, and then injecting a sulfur source into the solution within 10 seconds; and 3, preserving the heat at 100-120 ℃, then adding a terminator, cooling to room temperature, and separating and purifying to obtain the zinc-doped lead sulfide quantum dots. The preparation method is safe, simple and controllable to operate, low in cost and easy to repeat and amplify; the prepared quantum dots are uniform and controllable in size and shape, good in monodispersity and high in fluorescence quantum yield, and have good stability under the conditions of high temperature, washing, water-soluble modification and the like. Can be widely applied to the fields of photoelectric devices, solar cells, biomedical detection, fluorescence living body imaging and the like.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a simple, convenient and quick method for preparing zinc-doped lead sulfide quantum dots by a thermal injection method.
Background
The quantum dot is an important low-dimensional semiconductor material, the size of three dimensions of the quantum dot is not more than twice of the exciton Bohr radius of the corresponding semiconductor material, and the quantum dot has extremely wide application prospect in aspects of nonlinear optics, magnetic media, catalysis, medicines, functional materials and the like due to unique excellent physicochemical properties, and can deeply influence the continuous development of life science and information technology and the basic research of the material field.
Although there are many reports on the synthesis of high-quality quantum dots, the problems of high raw material cost, complex synthesis process, difficult control of physical and chemical properties, long reaction period, poor particle size uniformity and the like are still not solved; on the other hand, the quantum dots synthesized by the simple process method are not high enough in quality, so that it is still necessary to develop a more green and simple synthesis method to prepare quantum dots with higher quality.
Considering that the fluorescence property of the quantum dot is one of the most important properties, the fluorescence of the quantum dot is mainly generated by radiative recombination of excitons, and the exciton recombination comprises two processes of radiative recombination and non-radiative recombination (Auger recombination and phonon recombination), if the non-radiative recombination process can be effectively reduced, the radiative recombination rate of the excitons can be greatly improved, namely, the fluorescence quantum yield of the quantum dot can be greatly improved; nonradiative recombination is largely caused by defects in and on the quantum dots, and these defects also affect the stability of the quantum dots, and it is therefore necessary to eliminate these defects.
Lead sulfide has a small energy band gap, so that the stability of the pure lead sulfide quantum dots is poor, and the problem of oxidation of the lead sulfide quantum dots under air and illumination conditions is difficult to avoid. The zinc sulfide has relatively good oxidation resistance due to large energy band gap; on the other hand, a proper amount of zinc can effectively reduce the crystal defects of lead sulfide, thereby improving the optical performance of the doped product. The temperature in the synthesis process is mild, and separation and purification are not carried out, so that the process operation can be greatly simplified, the generation and growth of crystal nuclei are facilitated, and the quality of the quantum dots is further improved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for simply, rapidly and controllably preparing zinc-doped lead sulfide quantum dots, and the obtained quantum dots have adjustable fluorescence emission, high fluorescence quantum yield, uniform particle size morphology and good stability.
The technical scheme adopted for solving the problems in the prior art is as follows:
a preparation method of zinc-doped lead sulfide quantum dots is characterized by comprising the following steps:
step 1, introducing protective gas into a zinc source, a lead source, organic acid and/or organic amine under the condition of stirring, and heating until the protective gas is dissolved to obtain a mixed precursor solution of zinc and lead;
step 2, heating the solution to 120-150 ℃, and then injecting a sulfur source into the solution within 10 seconds;
and 3, preserving the heat at 100-120 ℃, then adding a terminator, cooling to room temperature, and separating and purifying to obtain the zinc-doped lead sulfide quantum dots.
In the step 1, the zinc source is one of zinc powder, zinc chloride, zinc carbonate, zinc oxide, zinc oxalate, zinc acetate, zinc stearate, zinc undecylenate and zinc diethyldithiocarbamate.
The lead source is one of lead powder, lead chloride, lead carbonate, lead oxide, lead oxalate, lead acetate, lead stearate, lead undecylenate and lead diethyldithiocarbamate.
The organic acid is one or more than two of saturated or unsaturated fatty acid with the carbon atom number more than or equal to 8; the shielding gas is one of nitrogen, argon, helium and neon.
The organic amine is one of saturated or unsaturated aliphatic amine with the carbon atom number more than or equal to 8.
The molar ratio of the total amount of the zinc source and the lead source to the total amount of the organic acid and/or the organic amine in the step 1 is 1: 10-1: 20.
In the step 2, the sulfur source is one of an organic solution of inorganic sulfur, an organic sulfur compound solution and an organic phosphine complex solution of sulfur; the organic solution of the inorganic sulfur comprises a 1-octadecene solution of sulfur powder, a liquid paraffin solution of the sulfur powder, a saturated or unsaturated fatty amine solution with the carbon atom number of the sulfur powder being more than or equal to 8, and a saturated or unsaturated fatty acid solution with the carbon atom number of the sulfur powder being more than or equal to 8; the organic sulfur comprises mercaptan, thioether, sulfur azole, thiourea, thioester, thioamide and the like; the organic phosphine complex of sulfur comprises tri-n-butyl phosphine sulfur, tri-n-octyl phosphine sulfur and diphenyl phosphine sulfur.
The concentration of the sulfur source in the step 2 is 0.01-10 mol/L.
And in the step 3, the heat preservation time is 0.01-2 h.
The invention has the following advantages:
the preparation method of the zinc-doped lead sulfide quantum dot is safe, simple and controllable in operation, low in cost and easy to repeat and amplify; the prepared quantum dots are uniform and controllable in size and shape, good in monodispersity and high in fluorescence quantum yield, and have good stability under the conditions of high temperature, washing, water-soluble modification and the like. Can be widely applied to the fields of photoelectric devices, solar cells, biomedical detection, fluorescence living body imaging and the like.
Drawings
FIG. 1 is a fluorescence spectrum of zinc-doped lead sulfide quantum dots provided by four embodiments of the present invention;
fig. 2 is a transmission electron microscope image of zinc-doped lead sulfide quantum dots provided in example 1 of the present invention;
fig. 3 is a transmission electron microscope image of zinc-doped lead sulfide quantum dots provided in example 2 of the present invention;
fig. 4 is a transmission electron microscope image of zinc-doped lead sulfide quantum dots provided in example 3 of the present invention;
fig. 5 is a transmission electron microscope image of zinc-doped lead sulfide quantum dots provided in example 4 of the present invention;
Detailed Description
The technical scheme of the invention is further described in detail by the following embodiments and the accompanying drawings:
example 1
Adding 0.05mmol of zinc acetate, 0.1mmol of lead chloride and 10ml of oleylamine into a flask with a condensing tube, introducing argon under the condition of stirring, heating to 80 ℃, vacuumizing for 30min, stopping vacuumizing, introducing argon, and heating to 120 ℃; after complete dissolution, cooling to 100 ℃, quickly injecting (within 10 s) 2ml of sulfur source, and keeping the temperature for 5 min; adding n-hexane to terminate the reaction, adding ethanol, centrifuging at 8000rpm/min for 5min, discarding supernatant to obtain precipitate, and sequentially washing with n-hexane and oleic acid twice. And finally, dissolving the product in n-hexane, measuring a fluorescence spectrum by using a fluorescence spectrophotometer, and positioning an emission peak at 1210 nm.
The sulfur source described in this example was prepared using the following method: adding 8mg of sulfur powder and 4mL of oleylamine into a three-neck flask, introducing argon, heating to 120 ℃, preserving heat for 10 minutes, and cooling to 80 ℃ to obtain a 0.06mol/L sulfur source solution.
Example 2
Adding 0.05mmol of zinc acetate, 0.1mmol of lead chloride and 10ml of oleylamine into a flask with a condensing tube, introducing argon under the condition of stirring, heating to 80 ℃, vacuumizing for 30min, stopping vacuumizing, introducing argon, and heating to 120 ℃; after complete dissolution, cooling to 100 ℃, quickly injecting (within 10 s) 2ml of sulfur source, and keeping the temperature for 10 min; adding n-hexane to terminate the reaction, adding ethanol, centrifuging at 8000rpm/min for 5min, discarding supernatant to obtain precipitate, and sequentially washing with n-hexane and oleic acid twice. And finally dissolving the product in n-hexane, measuring a fluorescence spectrum by using a fluorescence spectrophotometer, and positioning an emission peak at 1420 nm.
The sulfur source described in this example was prepared using the following method: adding 8mg of sulfur powder and 4mL of oleylamine into a three-neck flask, introducing argon, heating to 120 ℃, preserving heat for 10 minutes, and cooling to 80 ℃ to obtain a 0.06mol/L sulfur source solution.
Example 3
Adding 0.05mmol of zinc acetate, 0.1mmol of lead chloride and 10ml of oleylamine into a flask with a condensing tube, introducing argon under the condition of stirring, heating to 80 ℃, vacuumizing for 30min, stopping vacuumizing, introducing argon, and heating to 120 ℃; after complete dissolution, cooling to 100 ℃, quickly injecting (within 10 s) 2ml of sulfur source, and keeping the temperature for 15 min; adding n-hexane to terminate the reaction, adding ethanol, centrifuging at 8000rpm/min for 5min, discarding supernatant to obtain precipitate, and sequentially washing with n-hexane and oleic acid twice. And finally dissolving the product in n-hexane, measuring a fluorescence spectrum by using a fluorescence spectrophotometer, and positioning an emission peak at 1520 nm.
The sulfur source in this example was prepared by the following method: adding 8mg of sulfur powder and 4mL of oleylamine into a two-neck flask, introducing argon, heating to 120 ℃, preserving heat for 10 minutes, and cooling to 80 ℃ to obtain a 0.06mol/L sulfur source solution.
Example 4
Adding 0.05mmol of zinc acetate, 0.1mmol of lead chloride and 10ml of oleylamine into a flask with a condensing tube, introducing argon under the condition of stirring, heating to 80 ℃, vacuumizing for 30min, stopping vacuumizing, introducing argon, and heating to 120 ℃; after complete dissolution, cooling to 100 ℃, quickly injecting (within 10 s) 2ml of sulfur source, and keeping the temperature for 20 min; adding n-hexane to terminate the reaction, adding ethanol, centrifuging at 8000rpm/min for 5min, discarding supernatant to obtain precipitate, and sequentially washing with n-hexane and oleic acid twice. And finally, dissolving the product in n-hexane, and measuring a fluorescence spectrum by using a fluorescence spectrophotometer, wherein an emission peak is 1630 nm.
The sulfur source in this example was prepared by the following method: adding 8mg of sulfur powder and 4mL of oleylamine into a two-neck flask, introducing argon, heating to 120 ℃, preserving heat for 10 minutes, and cooling to 80 ℃ to obtain a 0.06mol/L sulfur source solution.
The fluorescence spectra of the products prepared in the above four groups of examples are shown in FIG. 1, the emission peak of the product obtained in example 1 is at 1210nm, the emission peak of the product obtained in example 2 is at 1420nm, the emission peak of the product obtained in example 3 is at 1520nm, and the emission peak of the product obtained in example 4 is at 1630 nm.
The transmission electron microscope images of the products prepared in the above embodiments 1, 2, 3 and 4 of the present invention are shown in fig. 2-5, and it can be seen from fig. 2-5 that the prepared quantum dots have uniform size and morphology and good monodispersity.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (9)
1. A preparation method of zinc-doped lead sulfide quantum dots is characterized by comprising the following steps:
step 1, introducing protective gas into a zinc source, a lead source, organic acid and/or organic amine under the condition of stirring, and heating until the protective gas is dissolved to obtain a mixed precursor solution of zinc and lead;
step 2, heating the solution to 120-150 ℃, and then injecting a sulfur source into the solution within 10 seconds;
and 3, preserving the heat at 100-120 ℃, then adding a terminator, cooling to room temperature, and separating and purifying to obtain the zinc-doped lead sulfide quantum dots.
2. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: in the step 1, the zinc source is one of zinc powder, zinc chloride, zinc carbonate, zinc oxide, zinc oxalate, zinc acetate, zinc stearate, zinc undecylenate and zinc diethyldithiocarbamate.
3. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: in the step 1, the lead source is one of lead powder, lead chloride, lead carbonate, lead oxide, lead oxalate, lead acetate, lead stearate, lead undecylenate and lead diethyldithiocarbamate.
4. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: in the step 1, the organic acid is one or more than two of saturated or unsaturated fatty acid with carbon atom number more than or equal to 8; the shielding gas is one of nitrogen, argon, helium and neon.
5. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: in the step 1, the organic amine is one of saturated or unsaturated aliphatic amine with carbon atom number more than or equal to 8.
6. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: the molar ratio of the total amount of the zinc source and the lead source to the total amount of the organic acid and/or the organic amine in the step 1 is 1: 10-1: 20.
7. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: in the step 2, the sulfur source is one of an organic solution of inorganic sulfur, an organic sulfur compound solution and an organic phosphine complex solution of sulfur; the organic solution of the inorganic sulfur comprises a 1-octadecene solution of sulfur powder, a liquid paraffin solution of the sulfur powder, a saturated or unsaturated fatty amine solution with the carbon atom number of the sulfur powder being more than or equal to 8, and a saturated or unsaturated fatty acid solution with the carbon atom number of the sulfur powder being more than or equal to 8; the organic sulfur comprises mercaptan, thioether, sulfur azole, thiourea, thioester, thioamide and the like; the organic phosphine complex of sulfur comprises tri-n-butyl phosphine sulfur, tri-n-octyl phosphine sulfur and diphenyl phosphine sulfur.
8. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: the concentration of the sulfur source in the step 2 is 0.01-10 mol/L.
9. The method for preparing zinc-doped lead sulfide quantum dots according to claim 1, wherein the method comprises the following steps: and in the step 3, the heat preservation time is 0.01-2 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111204809A (en) * | 2020-02-18 | 2020-05-29 | 黔南民族医学高等专科学校 | Preparation method of molybdenum disulfide quantum dots with high fluorescence intensity |
| CN114015442A (en) * | 2021-11-17 | 2022-02-08 | 北京工业大学 | Vacuum-assisted large-size lead sulfide quantum dot large-batch multi-injection synthesis method |
| CN114316988A (en) * | 2021-12-29 | 2022-04-12 | 武汉大学 | Preparation method and application of near-infrared IIb region metal ion (M = Zn, Mn) doped silver telluride quantum dot |
| CN114933898A (en) * | 2022-06-20 | 2022-08-23 | 南昌大学 | Preparation method of transition metal element doped lead sulfide quantum dots |
| CN115287057A (en) * | 2022-08-02 | 2022-11-04 | 华中科技大学 | Preparation method of lead sulfide quantum dots, near-infrared solar cell and photoelectric detector |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111204809A (en) * | 2020-02-18 | 2020-05-29 | 黔南民族医学高等专科学校 | Preparation method of molybdenum disulfide quantum dots with high fluorescence intensity |
| CN114015442A (en) * | 2021-11-17 | 2022-02-08 | 北京工业大学 | Vacuum-assisted large-size lead sulfide quantum dot large-batch multi-injection synthesis method |
| CN114316988A (en) * | 2021-12-29 | 2022-04-12 | 武汉大学 | Preparation method and application of near-infrared IIb region metal ion (M = Zn, Mn) doped silver telluride quantum dot |
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| CN114933898A (en) * | 2022-06-20 | 2022-08-23 | 南昌大学 | Preparation method of transition metal element doped lead sulfide quantum dots |
| CN114933898B (en) * | 2022-06-20 | 2023-10-31 | 南昌大学 | Preparation method of transition metal element doped lead sulfide quantum dot |
| CN115287057A (en) * | 2022-08-02 | 2022-11-04 | 华中科技大学 | Preparation method of lead sulfide quantum dots, near-infrared solar cell and photoelectric detector |
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