CN113583275A - High-heat-dissipation carbon quantum dot fluorescent composite film and preparation method thereof - Google Patents
High-heat-dissipation carbon quantum dot fluorescent composite film and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2339/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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Abstract
The invention belongs to the technical field of inorganic luminescent materials, and particularly relates to a high-heat-dissipation carbon quantum dot fluorescent composite film and a preparation method thereof. The technical scheme is as follows: ultrasonically dispersing carbon quantum dots and boron nitride in a solvent, adding a polymer into a dispersion liquid, heating and stirring until the mixture forms pasty viscous liquid, removing bubbles, uniformly coating to form a film, drying in a vacuum oven, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material. The method has the advantages of simple and convenient synthesis process, environmental protection and low production cost, and the prepared fluorescent composite membrane has high luminous intensity, adjustable luminous color, excellent high temperature resistance and high heat dissipation performance, does not generate fluorescence quenching at higher temperature and can show strong fluorescence response to specific substances. Can be applied to the fields of fluorescent sensors, luminous display, anti-counterfeiting encryption and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic luminescent materials, and particularly relates to a high-heat-dissipation carbon quantum dot fluorescent composite film and a preparation method thereof.
Background
Carbon quantum dots are the most important type of carbon-based fluorescent nano materials, and due to the excellent optical performance of the carbon quantum dots, the carbon quantum dots are more and more concerned in the fields of fluorescence sensing, biological imaging, photoelectric devices, photocatalysis, anti-counterfeiting and the like.
The carbon quantum dots are carbon fluorescent materials with wide prospects in the next generation of white light illumination application. At present, people put a great deal of attention on material design, performance modulation, mechanism research and the like of carbon quantum dot fluorescent powder. However, the low thermal conductivity makes the heat dissipation of the carbon quantum dot phosphor a great challenge. It has been confirmed that the operating temperature of high power light emitting display devices easily exceeds 130 deg.c, and the problem of thermal quenching caused by high temperature operation severely limits the further development of carbon quantum dot phosphors.
The direct and effective way of solving the thermal quenching problem is to reduce the working temperature of the carbon quantum dots and enhance the thermal conductivity of the carbon quantum dot composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a high-heat-dissipation carbon quantum dot fluorescent composite film, which is used for preparing a novel fluorescent composite film functional material with good luminous performance by a simple method, and the obtained product has high luminous intensity, adjustable luminous color, excellent high-temperature resistance and high heat dissipation performance, does not generate fluorescence quenching at high temperature and can show strong fluorescence response to specific substances.
The technical scheme adopted by the invention to achieve the aim is as follows:
a preparation method of a high-heat-dissipation carbon quantum dot fluorescent composite film comprises the following steps:
(1) ultrasonically dispersing carbon quantum dots and boron nitride in a solvent to obtain a dispersion liquid;
(2) adding a polymer into the dispersion liquid, heating and stirring until the mixture becomes pasty viscous liquid;
(3) uniformly coating the viscous liquid on a clean and flat substrate;
(4) and (3) drying the base material in a vacuum oven, and naturally cooling to obtain the carbon quantum dot fluorescent composite film.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film comprises the step (1), wherein the carbon quantum dots comprise one or more carbon quantum dot combinations with emission wavelengths within the range of 400-700 nm.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film comprises the step (1) that the boron nitride is a boron nitride nanosheet, a hydroxyl boron nitride nanosheet or an amino boron nitride nanosheet.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite membrane comprises the step (1) of using water, methanol, ethanol, chloroform or acetone as a solvent.
In the preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite membrane, the polymer in the step (2) is at least one selected from polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polyethyleneimine, polyethylene oxide, polyvinylidene fluoride, polyamide, polyimide, polyaramide, polysulfone, polyester, polyether, polymethacrylate, polycarbonate, polyurethane, phenolic resin, epoxy resin, nano cellulose, sodium carboxymethylcellulose and silica gel.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film comprises the step (1) and the step (2), wherein the mass ratio of the carbon quantum dots to the boron nitride to the polymer is 0.005-0.01: 0.01-0.1: 0.3-3.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film comprises the step (2) of heating at the temperature of 40-130 ℃ and stirring for 30-300 min.
Before coating in the step (3), the uniformly mixed viscous liquid is placed in a vacuum defoaming machine for defoaming and vacuumizing for 5-10 min.
In the preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film, the substrate in the step (3) is glass, ceramic, a silicon wafer or a quartz wafer.
The preparation method of the high-heat-dissipation carbon quantum dot fluorescent composite film comprises the step (4) of drying at the temperature of 40-70 ℃ for 5-12 hours.
The invention has the beneficial effects that:
the synthesis process is easy to control, simple to operate, green and environment-friendly, low in production cost, and capable of quickly constructing the carbon quantum dot fluorescent composite film, overcoming the defects of the existing carbon quantum dot film, and effectively overcoming the problems of solid-state fluorescence quenching and thermal quenching of the carbon quantum dots. The prepared carbon quantum dot fluorescent composite membrane has high luminous intensity, adjustable luminous color, excellent high temperature resistance and high heat dissipation performance, does not generate fluorescence quenching at higher temperature, and can show strong fluorescence response to specific substances. Can be widely applied to the fields of fluorescent sensors, luminous display, anti-counterfeiting encryption and the like.
Drawings
Fig. 1 is a photograph of a carbon quantum dot fluorescent composite film prepared in example 1 of the present invention under sunlight and ultraviolet light.
Fig. 2 is an excitation spectrum of the carbon quantum dot fluorescent composite film prepared in example 1 of the present invention and the carbon quantum dot fluorescent thin film without boron nitride in the comparative experiment in example 8.
Fig. 3 is an emission spectrum of the carbon quantum dot fluorescent composite film prepared in example 1 of the present invention and the carbon quantum dot fluorescent thin film without boron nitride in the comparative experiment in example 8.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described below with reference to the following embodiments. The specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Example 1 high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.005g of carbon quantum dots with the emission wavelength of 550nm and 0.05g of boron nitride nanosheets in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinyl alcohol into the dispersion, and putting the dispersion into a water bath kettle at 70 ℃ for heating and stirring for 30min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on clean and flat glass;
(4) and (3) drying the glass in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite film has excellent heat dissipation capacity, and emits uniform yellow fluorescent light under the irradiation of 445nm exciting light.
Embodiment 2 high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.005g of carbon quantum dots with the emission wavelength of 450nm and 0.05g of boron nitride hydroxide nano-sheets in 20mL of ethanol to obtain a dispersion liquid;
(2) adding 1g of polyurethane into the dispersion, and putting the dispersion into a water bath kettle at 80 ℃ for heating and stirring for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on dry and clean ceramics;
(4) and (3) drying the ceramic in a vacuum oven at 60 ℃ for 10h, and naturally cooling to obtain the carbon quantum dot fluorescent composite membrane material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity, and emits uniform blue fluorescence under the irradiation of 380nm exciting light.
Example 3A high thermal dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.005g of carbon quantum dots with emission wavelength of 620nm and 0.05g of amino boron nitride nanosheets in 20mL of chloroform to obtain a dispersion liquid;
(2) adding 1g of sodium carboxymethylcellulose into the dispersion, placing into a water bath kettle at 90 ℃, heating and stirring for 90min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on a dry and clean silicon wafer;
(4) and (3) drying the silicon wafer in a vacuum oven at 70 ℃ for 8h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite film has excellent heat dissipation capacity, and emits uniform red fluorescence under the irradiation of exciting light of 550 nm.
Embodiment 4 a high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.004g of carbon quantum dots with the emission wavelength of 450nm, 0.002g of carbon quantum dots with the emission wavelength of 550nm, 0.003g of carbon quantum dots with the emission wavelength of 620nm and 0.05g of boron nitride nanosheets in 20mL of distilled water to obtain dispersion liquid;
(2) adding 1g of polyvinylpyrrolidone into the dispersion, and heating and stirring the mixture in a water bath kettle at 80 ℃ for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on clean and flat glass;
(4) and (3) drying the glass in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity and emits uniform white fluorescence under the irradiation of 380nm exciting light.
Example 5A high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.003g of carbon quantum dots with the emission wavelength of 450nm and 0.002g of emission wavelength of 570nm and 0.01g of boron nitride nanosheets in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinylpyrrolidone into the dispersion, and heating and stirring the mixture in a water bath kettle at 80 ℃ for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on a clean and flat quartz plate;
(4) and (3) drying the quartz plate in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity and emits uniform white fluorescence under the irradiation of 380nm exciting light.
Embodiment 6 high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.003g of carbon quantum dots with the emission wavelength of 450nm and 0.002g of emission wavelength of 570nm and 0.03g of boron nitride nanosheets in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinylpyrrolidone into the dispersion, and heating and stirring the mixture in a water bath kettle at 80 ℃ for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on a clean and flat quartz plate;
(4) and (3) drying the quartz plate in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity and emits uniform white fluorescence under the irradiation of 380nm exciting light.
Example 7A high thermal dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.003g of carbon quantum dots with the emission wavelength of 450nm and 0.002g of emission wavelength of 570nm and 0.08g of boron nitride nanosheets in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinylpyrrolidone into the dispersion, and heating and stirring the mixture in a water bath kettle at 80 ℃ for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on a clean and flat quartz plate;
(4) and (3) drying the quartz plate in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity and emits uniform white fluorescence under the irradiation of 380nm exciting light.
Embodiment 8 high heat dissipation carbon quantum dot fluorescent composite film
The method comprises the following steps:
(1) ultrasonically dispersing 0.003g of carbon quantum dots with the emission wavelength of 450nm and 0.002g of emission wavelength of 570nm and 0.10g of boron nitride nanosheets in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinylpyrrolidone into the dispersion, and heating and stirring the mixture in a water bath kettle at 80 ℃ for 60min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on a clean and flat quartz plate;
(4) and (3) drying the quartz plate in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared fluorescent composite membrane has excellent heat dissipation capacity and emits uniform white fluorescence under the irradiation of 380nm exciting light.
Influence of boron nitride content on the carbon quantum dot fluorescent composite film: from examples 4 to 8, it can be seen that when the content of boron nitride is less, the heat dissipation performance of the fluorescent composite film is not greatly improved, and as the content of boron nitride gradually increases, the heat dissipation performance of the fluorescent composite film is obviously improved, but the boron nitride with too high content affects the light emitting performance of the carbon quantum dots.
Example 9 comparative experiment
The method comprises the following steps:
(1) ultrasonically dispersing 0.005g of carbon quantum dots with the emission wavelength of 550nm in 20mL of distilled water to obtain a dispersion liquid;
(2) adding 1g of polyvinyl alcohol into the dispersion, and putting the dispersion into a water bath kettle at 70 ℃ for heating and stirring for 30min until the mixture forms pasty viscous liquid;
(3) placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 10min, and then uniformly coating the viscous liquid on clean and flat glass;
(4) and (3) drying the glass in a vacuum oven at 50 ℃ for 12h, and naturally cooling to obtain the carbon quantum dot fluorescent composite film material.
The prepared carbon quantum dot fluorescent film emits uniform yellow fluorescence under the irradiation of 445nm exciting light.
Fig. 1 is a photograph of a carbon quantum dot fluorescent composite film under sunlight (a) and ultraviolet light (b), and the carbon quantum dot fluorescent composite film emits uniform yellow fluorescence under the irradiation of the ultraviolet light.
FIG. 2 is an excitation spectrum of a carbon quantum dot fluorescent thin film (a) and a carbon quantum dot fluorescent composite film (b) without boron nitride under monitoring at an emission wavelength of 541nm, with the strongest excitation peak at 446 nm.
Fig. 3 is a graph of the emission spectra of the carbon quantum dot fluorescent thin film (a) and the carbon quantum dot fluorescent composite film (b) without boron nitride, monitored at an excitation wavelength of 446nm, with the strongest emission peak at 541nm, the associated emission and lattice defect states attributed to surface defects of the carbon quantum dots, and the band gap transition of excitons. It can be seen that the addition of a proper amount of boron nitride can effectively improve the heat dissipation capability of the carbon quantum dot fluorescent composite film, and the luminescence level of the composite film is hardly influenced.
Claims (10)
1. A high heat dissipation carbon quantum dot fluorescent composite film is characterized in that the preparation method comprises the following steps:
(1) ultrasonically dispersing carbon quantum dots and boron nitride in a solvent to obtain a dispersion liquid;
(2) adding a polymer into the dispersion liquid, heating and stirring until the mixture becomes pasty viscous liquid;
(3) uniformly coating the viscous liquid on a clean and flat substrate;
(4) and (3) drying the base material in a vacuum oven, and naturally cooling to obtain the carbon quantum dot fluorescent composite film.
2. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 1, characterized in that: the carbon quantum dots in the step (1) comprise one or a combination of several carbon quantum dots with emission wavelengths of 400-700 nm.
3. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 2, characterized in that: the boron nitride in the step (1) is a boron nitride nanosheet, a hydroxyl boron nitride nanosheet or an amino boron nitride nanosheet.
4. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 3, characterized in that: the solvent in the step (1) is water, methanol, ethanol, chloroform or acetone.
5. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 4, wherein: the polymer in the step (2) is at least one selected from polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polyethyleneimine, polyethylene oxide, polyvinylidene fluoride, polyamide, polyimide, polyaramide, polysulfone, polyester, polyether, polymethacrylate, polycarbonate, polyurethane, phenolic resin, epoxy resin, nano cellulose, sodium carboxymethyl cellulose and silica gel.
6. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 5, characterized in that: the mass ratio of the carbon quantum dots, the boron nitride and the polymer in the step (1) and the step (2) is 0.005-0.01: 0.01-0.1: 0.3-3.
7. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 6, characterized in that: the heating temperature in the step (2) is 40-130 ℃, and the stirring time is 30-300 min.
8. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 7, characterized in that: and (4) before coating in the step (3), placing the uniformly mixed viscous liquid in a vacuum defoaming machine for defoaming and vacuumizing for 5-10 min.
9. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 8, characterized in that: the base material in the step (3) is glass, ceramic, a silicon wafer or a quartz wafer.
10. The high-heat-dissipation carbon quantum dot fluorescent composite film according to claim 9, characterized in that: and (4) drying at the temperature of 40-70 ℃ for 5-12 h.
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