CN111849465A - Method for preparing high-performance quantum dot powder - Google Patents
Method for preparing high-performance quantum dot powder Download PDFInfo
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- CN111849465A CN111849465A CN202010800110.1A CN202010800110A CN111849465A CN 111849465 A CN111849465 A CN 111849465A CN 202010800110 A CN202010800110 A CN 202010800110A CN 111849465 A CN111849465 A CN 111849465A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0237—Converting into particles, e.g. by granulation, milling
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/10—Finely divided sulfur, e.g. sublimed sulfur, flowers of sulfur
Abstract
The invention provides a method for preparing high-performance quantum dot powder, belonging to the field of luminescent materials, wherein the method for preparing the quantum dot powder comprises the following steps: (1) mixing and stirring the sublimed sulfur powder, sodium hydroxide and polyethylene glycol (PEG-400) in a metal bath, and heating to obtain a precursor of the sulfur point dispersion solution. (2) And naturally cooling the sulfur dot dispersion solution to room temperature, and slowly adding hydrogen peroxide dropwise under the condition of ice bath stirring (-3-0 ℃) to obtain a crude product of the sulfur quantum dots. (3) And centrifuging and dispersing in ethanol to obtain the pure colloidal quantum dots. (4) And adding acetone and ethyl acetate in a quantitative ratio into the solution, mixing and stirring, precipitating, centrifuging, and freeze-drying to obtain the sulfur quantum dot fluorescent powder. The invention has good luminous efficiency, high color purity and simple preparation process, and can be widely applied to biomedical markers, quantum dot light emitting diodes (QLEDs) and displays.
Description
Technical Field
The invention belongs to the field of luminescent materials, and provides a method for preparing high-performance quantum dot powder.
Background
Quantum dots, also known as nanocrystals, are composed of a finite number of atoms, all in the order of nanometers in size in 3 dimensions. The quantum dots are generally spherical or spheroidal, and are nanoparticles which are made of semiconductor materials and have stable diameters of 2-20 nm. As a novel semiconductor nano material, quantum dots have many unique optical properties such as high luminous efficiency, narrow emission spectrum, tunable emission spectrum, etc., which are important prerequisites for the application of quantum dots in display devices. Among these optical properties, quantum dots attract the eyeball of a skilled person with their very narrow half-peak width, and are considered as "the best historically luminescent materials". The quantum dot luminescent materials are various, CdSe is the earliest and the technology is the most mature in research of II-VI family quantum dots represented by the quantum dots, and the quantum dots are the most used materials in the backlight technology at present, however, with the gradual enhancement of the concept of 'green' synthesis of people, the market prospect of the metal element fluorescent quantum dots of cadmium-containing materials is gradually reduced, a plurality of countries clearly declare and limit the use of Cd-containing electronic products at present, in the 'method for limiting the use and management of harmful substances of electric and electronic products' issued in 2016, 1 month and China, the content of Cd is required to be lower than 100 ppm, so that the non-toxic quantum dot materials are regarded by people. Although a plurality of metal element-free fluorescent quantum dots such as silicon quantum dots, carbon quantum dots, sulfur-doped carbon quantum dots, nitrogen carbide quantum dots and the like are synthesized at present, a novel non-toxic sulfur quantum dot material is rarely reported, and the action of preparing the fluorescent sulfur quantum dots at a low temperature by using a water bath method is not reported.
Sulfur is widely distributed in nature, and the content of sulfur in the crust of the earth is 0.048 percent (by mass). Sulfur exists in nature in free and combined forms. Elemental sulfur is mainly present in the ground surrounding volcanoes, and most of the sulfur present in a combined state is a mineral and can be divided into sulfide minerals and sulfate minerals. But has the problems of low utilization rate and serious waste. Therefore, the method for preparing the sulfur quantum dots with high efficiency, green safety, environmental protection, high performance and high quantum yield has profound theoretical significance and application value. One side is used for promoting the development and application of the fluorescent quantum dot material; on the other hand, the development and utilization of elemental sulfur resources can be promoted, and the additional value is improved.
Disclosure of Invention
The technical purpose of the invention is to provide a preparation method of a sulfur quantum dot powder material with high efficiency, large-scale preparation and high quantum yield aiming at the current situation of the sulfur quantum dot preparation technology, and the technical scheme is as follows.
(1) And (4) preparing a sulfur dispersion solution.
Dispersing sublimed sulfur into a sodium hydroxide solution to prepare a dispersion liquid with the concentration of 2-5 g/L, adding 1-5 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 20-40 min; and (3) carrying out ultrasonic treatment to obtain a uniformly dispersed mixed solution, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring and continuously heating for reaction for 4-72 h at 50-150 ℃ to obtain a precursor sulfur dispersion liquid A.
(2) And preparing the sulfur quantum dots.
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 30-70% into the product A in a low-temperature environment under the condition of mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide, so that the crude product of the sulfur quantum dots with the fluorescent characteristic is prepared.
(3) And washing and purifying the colloidal sulfur quantum dots.
And (3) diluting the product B with deionized water, standing for 12 h to obtain a sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH =7 of the solution, wherein the product is the colloidal quantum dot C.
(4) And (3) preparing sulfur quantum dot powder.
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 3-7 times (rotating speed: 9000 r/m, centrifuging time: 5 min), removing the upper layer liquid, and retaining the precipitate. And transferring the obtained precipitate to a freeze drying box for low-temperature drying at the temperature of-60 to-30 ℃ for 12 to 24 hours. Finally, white sulfur quantum dot powder is obtained.
In the preparation method, in the step (1), the sulfur powder is one of sublimed sulfur, precipitated sulfur, inclined sulfur and elastic sulfur.
In the preparation method, in the step (1), the synthesis method is a metal bath reaction, the reaction temperature is 4-72 h and is 50-150 ℃.
In the preparation method, in the step (4), the anti-solvent is one of acetone, ethyl acetate and a mixed solvent of acetone and ethyl acetate. In the preparation method, in the step (4), low-temperature drying is carried out in a freeze drying box to obtain the sulfur quantum dot powder, and the drying temperature is-60 to-30 ℃ and the drying time is 12 to 24 hours.
The size of the sulfur quantum dot obtained by the method is 1-10 nm, and the sulfur quantum dot shows blue fluorescence under the excitation of ultraviolet light with the wavelength of 365 nm.
The invention has the beneficial effects.
(1) The invention uses sulfur powder as a sulfur source, sodium hydroxide provides an alkaline environment, and polyethylene glycol colloid as a dispersion stabilizer, so that the raw materials are cheap and easy to obtain.
(2) The preparation process is simple and controllable, has high yield and can be used for large-scale preparation.
(3) The preparation method provided by the invention does not need subsequent surface modification, and the prepared sulfur quantum dots have bright blue fluorescence.
(4) The sulfur quantum dots prepared by the method can be used for preparing composite materials, and can also be used for biomedical markers, quantum dot light emitting diodes (QLEDs), displays and the like.
Drawings
FIG. 1 is a picture of sulfur quantum dot powder obtained after the practice of the present invention.
FIG. 2 is a photograph of sulfur quantum dot powder obtained after practice of the invention under a 365 nm UV lamp.
Detailed Description
Example 1:
the embodiment provides a method for preparing high-performance quantum dot powder, and the specific preparation method is as follows.
(1) And (4) preparing a sulfur dispersion solution.
Dispersing sublimed sulfur into a sodium hydroxide solution to prepare a dispersion solution with the concentration of 2 g/L, adding 2 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 40 min; and (3) obtaining a uniformly dispersed mixed solution after ultrasonic treatment, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring and continuously heating for reaction for 7 hours at 70 ℃ to obtain a precursor sulfur dispersion liquid A.
(2) And preparing the sulfur quantum dots.
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 40% into the product A under the conditions of low-temperature environment and mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide, thus obtaining the crude product of the sulfur quantum dots with the fluorescent characteristic.
(3) And washing and purifying the colloidal sulfur quantum dots.
And (3) diluting the product B with deionized water, standing for 12 h to obtain a sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH =7 of the solution, wherein the product is the colloidal quantum dot C.
(4) And (3) preparing sulfur quantum dot powder.
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 4 times (rotating speed: 9000 r/m, centrifuging time: 5 min), removing the upper layer liquid, and retaining the precipitate. Transferring the obtained precipitate to a freeze drying oven for low temperature drying at-50 deg.C for 12 hr. Finally, white sulfur quantum dot powder is obtained.
Example 2:
the embodiment provides a method for preparing high-performance quantum dot powder, and the specific preparation method is as follows.
(1) And (4) preparing a sulfur dispersion solution.
Dispersing the precipitated sulfur into a sodium hydroxide solution to prepare a dispersion solution with the concentration of 4 g/L, adding 2 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 40 min; and (3) obtaining a uniformly dispersed mixed solution after ultrasonic treatment, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring and continuously heating for reaction for 7 hours at 70 ℃ to obtain a precursor sulfur dispersion liquid A.
(2) And preparing the sulfur quantum dots.
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 40% into the product A under the conditions of low-temperature environment and mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide, thus obtaining the crude product of the sulfur quantum dots with the fluorescent characteristic.
(3) And washing and purifying the colloidal sulfur quantum dots.
And (3) diluting the product B with deionized water, standing for 12 h to obtain a sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH =7 of the solution, wherein the product is the colloidal quantum dot C.
(4) And (3) preparing sulfur quantum dot powder.
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 4 times (rotating speed: 9000 r/m, centrifuging time: 5 min), removing the upper layer liquid, and retaining the precipitate. Transferring the obtained precipitate to a vacuum drying oven for low-temperature drying at-50 deg.C for 24 hr. Finally, white sulfur quantum dot powder is obtained.
Example 3:
the embodiment provides a method for preparing high-performance quantum dot powder, and the specific preparation method is as follows.
(1) And (4) preparing a sulfur dispersion solution.
Dispersing elastic sulfur into a sodium hydroxide solution to prepare a dispersion solution with the concentration of 6 g/L, adding 5 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 40 min; and (3) obtaining a uniformly dispersed mixed solution after ultrasonic treatment, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring, continuously heating for reaction for 20 hours at 70 ℃, and obtaining a precursor sulfur dispersion liquid A.
(2) And preparing the sulfur quantum dots.
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 40% into the product A under the conditions of low-temperature environment and mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide, thus obtaining the crude product of the sulfur quantum dots with the fluorescent characteristic.
(3) And washing and purifying the colloidal sulfur quantum dots.
And (3) diluting the product B with deionized water, standing for 12 h to obtain a sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH =7 of the solution, wherein the product is the colloidal quantum dot C.
(4) And (3) preparing sulfur quantum dot powder.
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 4 times (rotating speed: 9000 r/m, centrifuging time: 5 min), removing the upper layer liquid, and retaining the precipitate. Transferring the obtained precipitate to a freeze drying oven for low-temperature drying at-50 deg.C for 24 hr. Finally, white sulfur quantum dot powder is obtained.
Example 4:
the embodiment provides a method for preparing high-performance quantum dot powder, and the specific preparation method is as follows.
(1) And (4) preparing a sulfur dispersion solution.
Dispersing sublimed sulfur into a sodium hydroxide solution to prepare a dispersion solution with the concentration of 6 g/L, adding 5 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 40 min; and (3) obtaining a uniformly dispersed mixed solution after ultrasonic treatment, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring, continuously heating for reaction for 20 hours at 90 ℃ to obtain a precursor sulfur dispersion liquid A.
(2) And preparing the sulfur quantum dots.
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 40% into the product A under the conditions of low-temperature environment and mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide, thus obtaining the crude product of the sulfur quantum dots with the fluorescent characteristic.
(3) And washing and purifying the colloidal sulfur quantum dots.
And (3) diluting the product B with deionized water, standing for 12 h to obtain a sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH =7 of the solution, wherein the product is the colloidal quantum dot C.
(4) And (3) preparing sulfur quantum dot powder.
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 4 times (rotating speed: 9000 r/m, centrifuging time: 5 min), removing the upper layer liquid, and retaining the precipitate. Transferring the obtained precipitate to a freeze drying oven for low-temperature drying at-50 deg.C for 24 hr. Finally, white sulfur quantum dot powder is obtained.
Claims (6)
1. A method for preparing high-performance quantum dot powder comprises the following steps:
(1) preparation of Sulfur Dispersion solution
Dispersing sublimed sulfur into a sodium hydroxide solution to prepare a dispersion liquid with the concentration of 2-5 g/L, adding 1-5 mL of polyethylene glycol (PEG-400), putting all the solutions into a clean beaker, and carrying out ultrasonic treatment for 20-40 min; carrying out ultrasonic treatment to obtain a uniformly dispersed mixed solution, placing the mixed solution into a three-neck flask water bath reaction, mechanically stirring and continuously heating for reaction for 4-72 h at 50-150 ℃ to obtain a precursor sulfur dispersion liquid A;
(2) preparation of sulfur quantum dot solution
Standing the product A, cooling to room temperature, transferring the product A into a beaker, and placing the beaker in an ice bath, wherein the temperature is-3-0 ℃; slowly dropwise adding hydrogen peroxide with the mass concentration of 30-70% into the product A under the conditions of low-temperature environment and mechanical stirring, dispersing the precursor A into small-particle sulfur quantum dots (product B) with uniform size under the etching action of the hydrogen peroxide by adjusting the concentration and the dosage of the hydrogen peroxide, and changing the product B from gray green to blue under the irradiation of a 365 nm ultraviolet lamp along with the change of the dropwise addition of the hydrogen peroxide to obtain a crude product of the sulfur quantum dots with the fluorescent characteristic;
(3) washing and purification of sulfur quantum dots
Diluting the product B with deionized water, standing for 12 h to obtain sodium hydroxide dispersion liquid of the sulfur quantum dots, and filtering and washing by using a porous filtering membrane with the pore diameter of 0.3 mu m until the pH of the solution is =7, wherein the product is colloidal quantum dot C;
(4) preparation of sulfur quantum dot powder
Adding a mixed solution of acetone and ethyl acetate in a certain proportion into the colloidal quantum dot C as an anti-solvent, centrifuging the precipitated sulfur quantum dot product for 3-7 times (the rotating speed is 9000 r/m, the centrifuging time is 5 min), removing the upper layer liquid, and retaining the precipitate; and transferring the obtained precipitate to a freeze drying box for low-temperature drying at the temperature of-60 to-30 ℃ for 12 to 24 hours to finally obtain white sulfur quantum dot powder.
2. The method for producing a sulfur dispersion according to claim 1, characterized in that: in the step (1), the sulfur powder is one of sublimed sulfur, precipitated sulfur, inclined sulfur and elastic sulfur.
3. The method for producing a sulfur dispersion according to claim 1, characterized in that: in the step (1), the synthesis method is a metal bath reaction, and the reaction temperature is 4-72 h and 50-150 ℃.
4. The method of claim 1, wherein: in the step (4), the anti-solvent is one of acetone, ethyl acetate and a mixed solvent of acetone and ethyl acetate.
5. The method of claim 1, wherein: and (4) drying at low temperature in a freeze drying box to obtain sulfur quantum dot powder, wherein the drying temperature is-60 to-30 ℃, and the drying time is 12 to 24 hours.
6. The method for producing a sulfur quantum dot powder according to claim 1, characterized in that: under the excitation of ultraviolet light with the wavelength of 365 nm, the sulfur quantum dot powder shows blue fluorescence.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| NL2033219A (en) * | 2022-09-09 | 2022-12-15 | Univ Sichuan Agricultural | Sulfur quantum dot with high fluorescence quantum yield and mimic oxidase activity, and preparation and application thereof |
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| CN110715912A (en) * | 2019-10-08 | 2020-01-21 | 河北大学 | Sulfur quantum dot/manganese dioxide nanosheet composite material and preparation method and application thereof |
| CN110734763A (en) * | 2019-11-08 | 2020-01-31 | 中国石油大学(北京) | sulfur quantum dots, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110715912A (en) * | 2019-10-08 | 2020-01-21 | 河北大学 | Sulfur quantum dot/manganese dioxide nanosheet composite material and preparation method and application thereof |
| CN110734763A (en) * | 2019-11-08 | 2020-01-31 | 中国石油大学(北京) | sulfur quantum dots, and preparation method and application thereof |
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| NL2033219A (en) * | 2022-09-09 | 2022-12-15 | Univ Sichuan Agricultural | Sulfur quantum dot with high fluorescence quantum yield and mimic oxidase activity, and preparation and application thereof |
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