CN114989549B - Near-infrared carbon nano-dot light conversion film and preparation method and application thereof - Google Patents
Near-infrared carbon nano-dot light conversion film and preparation method and application thereof Download PDFInfo
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- CN114989549B CN114989549B CN202210644298.4A CN202210644298A CN114989549B CN 114989549 B CN114989549 B CN 114989549B CN 202210644298 A CN202210644298 A CN 202210644298A CN 114989549 B CN114989549 B CN 114989549B
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- ascorbic acid
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- C08J5/18—Manufacture of films or sheets
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
- A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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Abstract
The invention discloses a near-infrared carbon nano-dot light conversion film and a preparation method and application thereof, and belongs to the technical field of high polymer functional materials. The near-infrared nano carbon point light conversion film comprises near-infrared nano fluorescent carbon points, ascorbic acid and polyvinyl alcohol, wherein the near-infrared nano fluorescent carbon points, the ascorbic acid and the polyvinyl alcohol are in a mass ratio of (0.001-0.005): (0.0001-0.0005): 0.5. the near-infrared carbon nano-dot light conversion film is prepared without adding any toxic or expensive modifier, has the characteristics of environmental protection, stable performance, simple synthesis process and high light energy utilization rate, can convert ultraviolet light and yellow-green light in sunlight into red light which can be efficiently utilized by plants, and improves the light energy utilization rate.
Description
Technical Field
The invention relates to the technical field of high molecular functional materials, in particular to a near infrared carbon nano-dot light conversion film and a preparation method and application thereof.
Background
Sunlight is a source of energy for photosynthesis of plants, and the range of wavelengths of light utilized by plant photosynthesis is limited. Blue-violet light with the wavelength of 400-480 nm in sunlight can be strongly absorbed by chlorophyll and carotenoid, so that the growth of stems and leaves of plants is promoted; red orange light with the wavelength of 600-700 nm is absorbed by chlorophyll, so that the fruit growth of plants can be promoted; yellow-green light with the wavelength of 500-600 nm almost does not contribute to photosynthesis; ultraviolet rays with a wavelength of 290-315 nm are harmful to most plants.
The light conversion film can absorb part of ultraviolet light in sunlight and yellow-green light with low plant utilization rate, and convert the light into blue-violet light and red-orange light for plant photosynthesis. The ideal light conversion film can convert light which is harmful to plant growth and can not be absorbed into blue-violet light and red-orange light which can be absorbed and utilized by chlorophyll in photosynthesis. The agricultural light conversion film is a film which can more efficiently utilize sunlight than a common film for a common plant greenhouse without light conversion material addition by taking the film as an entry point. In addition, the large amount of data also suggests: the light conversion material can effectively improve the comprehensive utilization rate of light energy, is beneficial to the growth of plants and promotes the early ripening and yield increase of the plants.
Most rare earth inorganic light conversion agents are rare earth ion doped alkaline earth aluminates, oxysulfide, tungstate, silicate and the like, are rare earth functional materials with obvious light conversion effect, and are widely applied to light conversion agricultural films. However, the rare earth inorganic light conversion material is easy to hydrolyze in a wet environment, so that the luminous performance is reduced; and the rare earth inorganic light conversion material has poor compatibility with a high polymer matrix, and uneven stirring in the preparation process of the high polymer film can lead to poor dispersibility, so that the formed film has poor fluorescence uniformity, thereby affecting film forming, causing fluorescence quenching phenomenon and reducing the light conversion efficiency of the film. The light conversion agent with better solubility is synthesized and applied to a film, so that the problems of larger granularity and overlarge film forming thickness caused by material surface modification are solved.
Therefore, there is a need for improvements in the preparation of rare earth inorganic light conversion agents, micronizing or even nanocrystallizing the particles, since the ultrafine powder can enhance the dispersibility and fluorescence of the powder. Secondly, the research on compatibility of the light conversion agent with other functional assistants and polymers is increased, so that the light transmittance reduction and fluorescence quenching caused by rare earth agglomeration are effectively avoided.
At present, the red fluorescent carbon dots are synthesized by dopamine hydrochloride, o-phenylenediamine and acid, compared with the prior rare earth inorganic light conversion agent, the novel red fluorescent light conversion material solves the problems of larger granularity and overlarge film forming thickness caused by material surface modification, and has the advantages of high ultraviolet light conversion function, slow light conversion attenuation, low preparation cost and strong binding force with a polymer film material. However, raw materials of dopamine hydrochloride, o-phenylenediamine and acid for synthesizing carbon points are not friendly to the environment, and the raw materials are contrary to the current carbon neutralization environment-friendly concept.
Disclosure of Invention
Aiming at the problems, the invention provides the near-infrared carbon nano-dot light conversion film, the preparation method and the application thereof, and the preparation of the near-infrared carbon nano-dot light conversion film does not add any toxic or expensive modifier, has the characteristics of environmental protection, stable performance, simple synthesis process and high light energy utilization rate, can convert ultraviolet light and yellow-green light in sunlight into red light which can be efficiently utilized by plants, and improves the light energy utilization rate.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the near-infrared nano carbon dot light conversion film comprises near-infrared nano fluorescent carbon dots, ascorbic acid and polyvinyl alcohol, wherein the near-infrared nano fluorescent carbon dots, the ascorbic acid and the polyvinyl alcohol are in a mass ratio of (0.001-0.005): (0.0001-0.0005): 0.5.
the near-infrared nano carbon dot light conversion film of the invention takes near-infrared nano fluorescent carbon dots as light conversion materials, ascorbic acid as an antioxidant and polyvinyl alcohol as a carrier, and the near-infrared nano carbon dot light conversion agricultural film is formed by compounding. The near infrared nanometer fluorescent carbon point is synthesized by a one-step solvothermal method of white magnolia leaf powder and an organic solvent, and has a nanometer light conversion material which has strong absorption in ultraviolet light and yellow-green light areas and emits red fluorescence, and the particle size of the nanometer light conversion material is smaller than 10 nm; the ascorbic acid is a carbohydrate compound containing rich oxidation states, has excellent strong oxidation resistance, is easily oxidized into dehydrovitamin C, but has reversible reaction, and has the same physiological function as dehydroascorbic acid, but if dehydroascorbic acid is further hydrolyzed to generate diketone gulonic acid, the reaction is irreversible and completely loses physiological efficacy, the quenching of near infrared nano fluorescent carbon dots caused by oxidation of strong physical factors can be prevented, and the service life of the near infrared nano carbon dot light conversion film is effectively prolonged; polyvinyl alcohol is a low-cost, nontoxic, non-corrosive, high-molecular material with good film-forming property, cohesiveness, biological affinity and environmental friendliness, is the only vinyl polymer which can be used as a carbon source and an energy source by bacteria, can be degraded by 75% in 46 days under the action of bacteria and enzymes, and belongs to a biodegradable high-molecular material. The invention is an important change of the existing agricultural light conversion film polymer material film and light conversion material, combines the novel carbon-based nanomaterial carbon dots with the polymer, fully utilizes the existing renewable green resources, avoids the environmental pollution problem caused by polymer synthesis, increases the optical performance on the basis of the traditional film, and enhances the oxidation resistance and prolongs the service life compared with the existing agricultural film. The near infrared carbon nano-dot light conversion film has strong absorption on ultraviolet light (380-420 nm) and yellow-green light (492-585 nm), emits red fluorescence with the wavelength range of 600-700 nm, can convert ultraviolet light and yellow-green light with lower utilization rate of ultraviolet light and plants into red light useful for plant growth, improves the utilization rate of light energy, can be used as an agricultural greenhouse film and a mulching film, is applied to the aspects of crop planting, seedling raising and the like, and can achieve the effects of increasing yield and improving quality.
Preferably, the near infrared nano fluorescent carbon dots are synthesized by a one-step solvothermal method by using white magnolia leaf powder and an organic solvent.
Preferably, the mass volume ratio of the white magnolia leaf powder to the organic solvent is 1g: 10-30 mL.
Preferably, the organic solvent is an acetone solution, absolute ethanol or methanol.
Preferably, the ultraviolet absorption wavelength and the excitation wavelength of the near infrared fluorescence nanometer carbon point are respectively 380-420 nm and 380-410 nm, and the emission peak wavelength range is 600-700 nm.
The invention also provides a preparation method of the near infrared carbon nano-dot light conversion film, which comprises the following steps:
(1) Uniformly mixing white magnolia leaf powder and an organic solvent, transferring the mixture into a stainless steel reaction kettle, heating the mixture at a constant temperature of between 100 and 200 ℃ for 3 to 8 hours in a reactor, naturally cooling the mixture after the reaction is finished, centrifuging the obtained reactant, filtering the obtained supernatant by using a filter membrane, purifying the obtained filtrate by using a silica gel column chromatography, dynamically eluting the purified filtrate by using petroleum ether and ethyl acetate eluents with different volume ratios, collecting a dark green solution, and evaporating the solution under reduced pressure to obtain a dark green colloid product near infrared nanometer fluorescent carbon point;
(2) The near infrared nanometer fluorescent carbon dot colloid is added into the mixed solution of ethanol and deionized water, and ultrasonic treatment is carried out until the colloid is dissolved, thus obtaining near infrared nanometer fluorescent carbon dot alcohol solution;
(3) Adding ascorbic acid into deionized water, and performing ultrasonic treatment until solid is dissolved to obtain an ascorbic acid solution;
(4) Adding polyvinyl alcohol into deionized water, heating at constant temperature of 280r/min and 95 ℃ in a reactor for 10 minutes until solid is melted, heating the solution to evaporate water until the whole solution is sticky, and obtaining a polyvinyl alcohol solution;
(5) Adding an ascorbic acid solution and a near infrared nano fluorescent carbon dot alcohol solution into a polyvinyl alcohol solution, continuously stirring, reacting for 5 minutes at constant temperature to uniformly disperse the ascorbic acid solution and the near infrared nano fluorescent carbon dot alcohol solution in the polyvinyl alcohol solution, removing bubbles to obtain a uniform composite solution, wherein the mass ratio of the near infrared nano fluorescent carbon dot to the ascorbic acid to the polyvinyl alcohol in the composite solution is (0.001-0.005): (0.0001-0.0005): 0.5;
(6) And a curing film forming step, namely casting the composite solution into a film, and air-drying, curing and forming to obtain the near infrared nano carbon point light conversion film.
Preferably, in the dissolving step of the near infrared nano fluorescent carbon dot colloid, the dosage ratio of the near infrared nano fluorescent carbon dot colloid to the ethanol to the deionized water is 4 mg:1-5 mL:0-4 mL.
Preferably, in the ascorbic acid dissolving step, the dosage ratio of the ascorbic acid to deionized water is 10mg:5mL.
Preferably, the volume ratio of the petroleum ether to the ethyl acetate in the petroleum ether and ethyl acetate eluent is 3:1-1:1.
The invention also provides application of the near-infrared nano carbon dot light conversion film, and the near-infrared nano carbon dot light conversion film is used for crop planting or crop seedling.
By adopting the technical scheme, the invention has the beneficial effects that:
the near-infrared nano carbon dot light conversion film of the invention takes near-infrared nano fluorescent carbon dots as light conversion material, ascorbic acid as antioxidant, polyvinyl alcohol as carrier, and the near-infrared nano carbon dot light conversion agricultural film is formed by compounding, wherein:
(1) The near infrared nano fluorescent carbon dots are synthesized by a one-step solvothermal method of the white magnolia leaf powder and the organic solvent, the synthesis process is simple, the utilization ratio of light energy is high, and the nano light conversion material which has strong absorption in ultraviolet light and yellow-green light areas and emits red fluorescence and has the particle size smaller than 10 nm: if the ultraviolet light (250-300 nm) and the yellow-green light (492-585 nm) with low plant utilization rate are strongly absorbed, the ultraviolet light can be excited by the light of the two areas, and red fluorescence with the wavelength range of 600-700 nm can be emitted and can be efficiently utilized by plants, so that the light conversion effect is realized, and the effect of promoting plant growth is achieved; the near infrared carbon dot shows stable near infrared emission, the peak value is about 678nm, the near infrared nano fluorescent carbon dot has narrow half-peak width, small particle size (particle diameter is less than 10 nm), stable light-transmitting property, low toxicity and good biocompatibility;
(2) The invention selects the ascorbic acid as the antioxidant, is environment-friendly, safe and nontoxic, has excellent strong oxidation resistance, can prevent the near infrared nano fluorescent carbon dots from being quenched due to oxidation of strong physical factors, and effectively prolongs the service life of the near infrared nano carbon dot light conversion film.
(3) The synthetic material and the preparation process of the near-infrared carbon nano-dot light conversion film follow the concept of green and environment protection, and the whole process has almost no pollution to the environment.
In conclusion, the near-infrared carbon nano-dot light conversion film is prepared without adding any toxic or expensive modifier, has the characteristics of environmental protection, stable performance, simple synthesis process and high light energy utilization rate, can convert ultraviolet light and yellow-green light in sunlight into red light which can be efficiently utilized by plants, and improves the light energy utilization rate.
Drawings
FIG. 1 is a graph of absolute fluorescence quantum yields of near infrared nano-fluorescent carbon dots (NIR-CDs) in the present invention under (a) acetone and (b) DMSO, respectively;
FIG. 2 shows (a) ultraviolet absorption spectra and (b) fluorescence emission spectra of near infrared nano fluorescent carbon dots (NIR-CDs) of the present invention at different excitation wavelengths; (c) fluorescence emission spectra under different solvents; (d) Fluorescence emission spectra of NIR-CDs at different water/ethanol mixing ratios; (e) Fluorescence emission spectra of NIR-CDs in DMSO solution at different excitation wavelengths; (f) Fluorescence emission spectra of NIR-CDs in DMSO solutions at various water contents (NIR-CDs concentration of 50 mg.L -1 )；
FIG. 3 is a graph showing fluorescence of NIR-CDs of the invention prepared by different solvothermal methods, wherein solvents from left to right are respectively prepared by water, DMSO, DMF, glacial acetic acid and acetone;
FIG. 4 is a graph showing fluorescence of near infrared nano fluorescent carbon dots according to the present invention at different water/ethanol mixing ratios;
FIG. 5 is a photograph of the near infrared nanocarbon dot light conversion film of the present invention under ultraviolet irradiation;
FIG. 6 is a photograph of the near infrared nanocarbon dot light conversion film of the present invention under white light; (1) a film of polyvinyl alcohol and ethanol; (2) Films of polyvinyl alcohol and near infrared fluorescent nanocarbon dots; (3) Films of polyvinyl alcohol, near infrared fluorescent nanocarbon sites and ascorbic acid;
fig. 7 is a photograph of the near infrared nano light conversion film of the present invention under ultraviolet irradiation: (a) Is a film of polyvinyl alcohol and ethanol under ultraviolet irradiation; (b) Is a film of polyvinyl alcohol and near infrared fluorescent nano carbon dots under ultraviolet irradiation; (c) Is a film under the irradiation of polyvinyl alcohol, near infrared fluorescent nano carbon points and ascorbic acid ultraviolet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The near-infrared nano carbon dot light conversion film comprises near-infrared nano fluorescent carbon dots, ascorbic acid and polyvinyl alcohol, wherein the near-infrared nano fluorescent carbon dots, the ascorbic acid and the polyvinyl alcohol are in a mass ratio of (0.001-0.005): (0.0001-0.0005): 0.5. the near infrared fluorescent nano carbon dots are synthesized by a white magnolia leaf powder and an organic solvent solvothermal method. Wherein the mass volume ratio of the white magnolia leaf powder to the organic solvent is 1g: 10-30 mL. The organic solvent is acetone, absolute ethyl alcohol or methanol. The ultraviolet absorption wavelength and the excitation wavelength of the near infrared fluorescence nanometer carbon point are respectively 380-420 nm and 380-410 nm, and the emission peak wavelength range is 600-700 nm. The polyvinyl alcohol is polyvinyl alcohol-1799.
The preparation method of the near-infrared nano carbon dot light conversion film comprises the following steps:
the near infrared nanometer fluorescent carbon dot synthesis step comprises selecting fresh white yulan leaves, cleaning, oven drying, and pulverizing into powder; adding the obtained powder into an organic solvent, and fully and uniformly stirring; transferring the uniformly stirred solution into a stainless steel reaction kettle, and heating at a constant temperature in a reactor at 100-200 ℃ for 3-8 hours to obtain a reactant; cooling to room temperature, centrifuging the obtained reactant, filtering the obtained supernatant with a filter membrane, and purifying the obtained filtrate with silica gel column chromatography; dynamically eluting with petroleum ether and ethyl acetate eluents in different volume ratios; finally, collecting the dark green solution, and evaporating under reduced pressure to obtain a dark green colloid product near-infrared carbon point;
a step of dissolving polyvinyl alcohol, which is to add the polyvinyl alcohol into deionized water, heat the powder to melt in a water bath kettle of 280r at 95 ℃, and change the white solution into transparent solution to obtain a polyvinyl alcohol solution;
the near infrared fluorescent nano carbon dot colloid dissolving step: adding the near infrared nanometer fluorescent carbon dot colloid into a mixed solution of ethanol and deionized water, and performing ultrasonic treatment until the colloid is dissolved to obtain a near infrared fluorescent nanometer carbon dot solution;
an ascorbic acid dissolving step: adding ascorbic acid powder into deionized water for dissolution to obtain ascorbic acid solution;
adding a near infrared fluorescent nano carbon dot solution and an ascorbic acid solution into a polyvinyl alcohol solution, continuously stirring to uniformly disperse the near infrared fluorescent nano carbon dot solution and the ascorbic acid solution in the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution, wherein the mass ratio of the red fluorescent carbon dot to the ascorbic acid to the polyvinyl alcohol in the composite solution is (0.001-0.005): (0.0001-0.0005): 0.5;
and a curing film forming step, namely casting the composite solution into a film, and air-drying, curing and forming to obtain the near infrared nano light conversion film.
Example 1
A preparation method of a near-infrared carbon nano-dot light conversion film comprises the following steps:
firstly, the near infrared nanometer fluorescent carbon point synthesis step comprises the steps of selecting fresh magnolia leaves, cleaning, drying at 50 ℃ for 12 hours, and crushing into powder; weighing 4.0g of white magnolia leaf powder, adding the white magnolia leaf powder into 80ml of acetone solution, and fully and uniformly stirring; transferring the uniformly stirred solution into a polytetrafluoroethylene lining autoclave with the size of 100ml, and heating at the constant temperature of 120 ℃ for 5 hours to obtain a reactant; after heating is completed and cooling to room temperature, centrifuging the obtained reactant at 8000r/min for 10 minutes; filtering the supernatant with polyethersulfone membrane (0.22 μm), purifying the filtrate by silica gel column chromatography, and dynamically eluting with petroleum ether and ethyl acetate eluent at volume ratio of 3:1; finally, the dark green solution was collected and evaporated under reduced pressure to give a dark green colloid product with a yield of 2% near infrared carbon dots.
Next, 0.5g of polyvinyl alcohol was added to 495ml of deionized water, and the mixture was heated at a constant temperature of 95℃and 280r (water bath or oil bath) until the polyvinyl alcohol was melted, and the solution was changed from white to transparent, to obtain a polyvinyl alcohol solution. Then adding 10mg of ascorbic acid powder into 5ml of deionized water to prepare an ascorbic acid solution, taking 50 microliters of the ascorbic acid solution and 4mg of near infrared fluorescent nano carbon dot colloid, adding the near infrared fluorescent nano film carbon dot solution prepared by adding 5ml of ethanol into the polyvinyl alcohol solution, continuously stirring, uniformly dispersing the near infrared fluorescent nano film carbon dot solution and the ascorbic acid solution into the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution. And finally, casting the composite solution into a film, and air-drying, curing and forming to obtain the novel near infrared nanometer light conversion film.
Example 2
A preparation method of a near-infrared carbon nano-dot light conversion film comprises the following steps:
firstly, the near infrared nanometer fluorescent carbon point synthesis step comprises the steps of selecting fresh magnolia leaves, cleaning, drying at 50 ℃ for 12 hours, and crushing into powder; weighing 4.0g of white magnolia leaf powder, adding the white magnolia leaf powder into 80ml of acetone solution, and fully and uniformly stirring; transferring the uniformly stirred solution into a polytetrafluoroethylene lining autoclave with the size of 100ml, and heating at the constant temperature of 120 ℃ for 5 hours to obtain a reactant; after heating is completed and cooling to room temperature, centrifuging the obtained reactant at 8000r/min for 10 minutes; filtering the supernatant with polyethersulfone membrane (0.22 μm), purifying the filtrate by silica gel column chromatography, and dynamically eluting with petroleum ether and ethyl acetate eluent at volume ratio of 2:1; finally, the dark green solution was collected and evaporated under reduced pressure to give a dark green colloid product with a near infrared carbon dots (NIR-CDs) yield of 2%.
Next, 0.5g of polyvinyl alcohol was added to 495ml of deionized water, and the mixture was heated at a constant temperature of 95℃and 280r (water bath or oil bath) until the polyvinyl alcohol was melted, and the solution was changed from white to transparent, to obtain a polyvinyl alcohol solution. Then adding 10mg of ascorbic acid powder into 5ml of deionized water to prepare an ascorbic acid solution, adding 50 microliters of the ascorbic acid solution and 4mg of near infrared fluorescent nano carbon dot colloid into 4ml of ethanol and adding the near infrared fluorescent nano film carbon dot solution prepared into 1ml of deionized water into a polyvinyl alcohol solution, continuously stirring to uniformly disperse the near infrared fluorescent nano carbon dot solution and the ascorbic acid solution into the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution. And finally, casting the composite solution into a film, and air-drying, curing and forming to obtain the novel near infrared nanometer light conversion film.
Example 3
A preparation method of a near-infrared carbon nano-dot light conversion film comprises the following steps:
firstly, the near infrared nanometer fluorescent carbon point synthesis step comprises the steps of selecting fresh magnolia leaves, cleaning, drying at 50 ℃ for 12 hours, and crushing into powder; weighing 4.0g of white magnolia leaf powder, adding the white magnolia leaf powder into 80ml of acetone solution, and fully and uniformly stirring; transferring the uniformly stirred solution into a polytetrafluoroethylene lining autoclave with the size of 100ml, and heating at the constant temperature of 120 ℃ for 5 hours to obtain a reactant; after heating is completed and cooling to room temperature, centrifuging the obtained reactant at 8000r/min for 10 minutes; filtering the supernatant with polyethersulfone membrane (0.22 μm), purifying the filtrate by silica gel column chromatography, and dynamically eluting with petroleum ether and ethyl acetate eluent at volume ratio of 3:1; finally, the dark green solution was collected and evaporated under reduced pressure to give a dark green colloid product with a near infrared carbon dots (NIR-CDs) yield of 2%.
Next, 0.5g of polyvinyl alcohol was added to 495ml of deionized water, and the mixture was heated at a constant temperature of 95℃and 280r (water bath or oil bath) until the polyvinyl alcohol was melted, and the solution was changed from white to transparent, to obtain a polyvinyl alcohol solution. Then adding 10mg of ascorbic acid powder into 5ml of deionized water to prepare an ascorbic acid solution, adding 50 microliters of the ascorbic acid solution and 4mg of near infrared fluorescent nano carbon dot colloid into 3ml of ethanol and 2ml of near infrared fluorescent nano film carbon dot solution prepared into deionized water into a polyvinyl alcohol solution, continuously stirring to uniformly disperse the near infrared fluorescent nano carbon dot solution and the ascorbic acid solution into the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution. And finally, casting the composite solution into a film, and air-drying, curing and forming to obtain the novel near infrared nanometer light conversion film.
Example 4
A preparation method of a near-infrared carbon nano-dot light conversion film comprises the following steps:
firstly, the near infrared nanometer fluorescent carbon point synthesis step comprises the steps of selecting fresh magnolia leaves, cleaning, drying at 50 ℃ for 12 hours, and crushing into powder; weighing 4.0g of white magnolia leaf powder, adding the white magnolia leaf powder into 80ml of acetone solution, and fully and uniformly stirring; transferring the uniformly stirred solution into a polytetrafluoroethylene lining autoclave with the size of 100ml, and heating at the constant temperature of 120 ℃ for 5 hours to obtain a reactant; after heating is completed and cooling to room temperature, centrifuging the obtained reactant at 8000r/min for 10 minutes; filtering the supernatant with polyethersulfone membrane (0.22 μm), purifying the filtrate by silica gel column chromatography, and dynamically eluting with petroleum ether and ethyl acetate eluent at volume ratio of 1:1; finally, the dark green solution was collected and evaporated under reduced pressure to give a dark green colloid product with a near infrared carbon dots (NIR-CDs) yield of 2%.
Next, 0.5g of polyvinyl alcohol was added to 495ml of deionized water, and the mixture was heated at a constant temperature of 95℃and 280r (water bath or oil bath) until the polyvinyl alcohol was melted, and the solution was changed from white to transparent, to obtain a polyvinyl alcohol solution. Then adding 10mg of ascorbic acid powder into 5ml of deionized water to prepare an ascorbic acid solution, adding 50 microliters of the ascorbic acid solution and 4mg of near infrared fluorescent nano carbon dot colloid into 2ml of ethanol and 3ml of near infrared fluorescent nano film carbon dot solution prepared into deionized water into a polyvinyl alcohol solution, continuously stirring to uniformly disperse the near infrared fluorescent nano carbon dot solution and the ascorbic acid solution into the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution. And finally, casting the composite solution into a film, and air-drying, curing and forming to obtain the novel near infrared nanometer light conversion film.
Example 5
A preparation method of a near-infrared carbon nano-dot light conversion film comprises the following steps:
firstly, the near infrared nanometer fluorescent carbon point synthesis step comprises the steps of selecting fresh magnolia leaves, cleaning, drying at 50 ℃ for 12 hours, and crushing into powder; weighing 4.0g of white magnolia leaf powder, adding the white magnolia leaf powder into 80ml of acetone solution, and fully and uniformly stirring; transferring the uniformly stirred solution into a polytetrafluoroethylene lining autoclave with the size of 100ml, and heating at the constant temperature of 120 ℃ for 5 hours to obtain a reactant; after heating is completed and cooling to room temperature, centrifuging the obtained reactant at 8000r/min for 10 minutes; filtering the supernatant with polyethersulfone membrane (0.22 μm), purifying the filtrate by silica gel column chromatography, and dynamically eluting with petroleum ether and ethyl acetate eluent at volume ratio of 2:1; finally, the dark green solution was collected and evaporated under reduced pressure to give a dark green colloid product with a near infrared carbon dots (NIR-CDs) yield of 2%.
Next, 0.5g of polyvinyl alcohol was added to 495ml of deionized water, and the mixture was heated at a constant temperature of 95℃and 280r (water bath or oil bath) until the polyvinyl alcohol was melted, and the solution was changed from white to transparent, to obtain a polyvinyl alcohol solution. Then adding 10mg of ascorbic acid powder into 5ml of deionized water to prepare an ascorbic acid solution, adding 50 microliters of near infrared fluorescent nano carbon dot colloid into 1ml of ethanol and 4ml of near infrared fluorescent nano film carbon dot solution prepared into deionized water to prepare a polyvinyl alcohol solution, continuously stirring to uniformly disperse the near infrared fluorescent nano carbon dot solution and the ascorbic acid solution into the polyvinyl alcohol solution, and heating for 5 minutes to obtain a uniform composite solution. And finally, casting the composite solution into a film, and air-drying, curing and forming to obtain the novel near infrared nanometer light conversion film.
Performance testing
FIG. 1 shows the absolute quantum yields of NIR-CDs in acetone and DMSO solutions of 19.80% and 22.66%, respectively, as measured by fluorescence steady state/transient state spectroscopy.
FIG. 2 is a graph of UV-Vis spectra and FL emission spectra recorded for NIR-CDs solutions to describe their spectral characteristics. As shown in FIG. 2a, the NIR-CDs solution showed broad absorption in the wavelength range of 350-470 nm with a maximum absorption peak around 413 nm. FIG. 2b shows FL emission of NIR-CDs in acetone solution at different excitation wavelengths, showing stable deep red emission with peak around 678nm and FWHM 25nm; when the polarity of the solvent was increased (FIG. 2 c), the NIR-CDs showed a weak shoulder emission at 720nm under excitation at 413 nm. However, the prepared NIR-CDs have poor solubility in water. In addition, FL emission spectra of NIR-CDs in ethanol solutions at different water contents were obtained under excitation at 413 nm. Solutions of NIR-CDs in pure ethanol are transparent and show pronounced near infrared fluorescence, whereas the fluorescence intensity gradually decreases with increasing water proportion due to the quenching effect (ACQ) caused by aggregation (FIG. 2 d). NIR-CDs in DMSO solutions exhibit similar fluorescence phenomena (panels e and f) compared to acetone or ethanol solutions, which provides the possibility for biological applications.
FIG. 3 is a graph of fluorescence luminescence of NIR-CDs prepared by different solvothermal methods at 120 ℃. In the orthogonal test design and analysis, the UV-Vis spectra of carbon points prepared by reaction under the same solvent are compared, and the fact that the absorbance of the carbon points prepared by different solvothermal reactions is continuously increased along with the continuous increase of the reaction temperature, and the absorption intensity is gradually reduced from a short wavelength to a long wavelength at 210 ℃, so that the maximum absorption peak is no longer generated in the middle; in particular, when water and glacial acetic acid are used as reaction solvents, the absorption intensity of the aqueous dispersion is gradually reduced from 350 to 800nm at 90 ℃.
FIG. 4 is a photograph of NIR-CDs (50 mg/L) in ethanol solution at different water contents (i.e., fluorescence emission patterns at different water/ethanol mixing ratios) under UV light, which intuitively shows that NIR-CDs' near infrared fluorescence in ethanol solution decreases significantly with the addition of water. This suggests that NIR-CDs have similar properties in DMSO.
Fig. 5 is a picture of the near infrared nano fluorescent carbon dot of the present invention irradiated by ultraviolet light, and it can be seen that red fluorescent light is uniformly distributed in an ethanol aqueous solution.
FIG. 6 is a photograph of three groups of films of the present invention under white light, (1) films with added polyvinyl alcohol and ethanol; (2) A film for adding polyvinyl alcohol and near infrared fluorescent nano carbon dots; (3) Is a film added with polyvinyl alcohol, near infrared fluorescent nano carbon dots and ascorbic acid. The film No. 1 is transparent and colorless, and the films No. 2 and No. 3 are green, which indicates that the color of the light conversion film is the same as the color of the near infrared nano carbon dot colloid.
FIG. 7 is a photograph of three sets of films of the present invention under ultraviolet irradiation, the three sets of films being (a) films of polyvinyl alcohol and ethanol, respectively, under ultraviolet irradiation; (b) Is a film of polyvinyl alcohol and near infrared fluorescent nano carbon dots under ultraviolet irradiation; (c) Is a film under the irradiation of polyvinyl alcohol, near infrared fluorescent nano carbon points and ascorbic acid ultraviolet. It can be observed that fig. 7 (a) does not have red fluorescence, fig. 7 (b) has red fluorescence, and fig. 7 (c) is deeper than the red fluorescence of fig. 7 (b), because fig. 7 (c) adds ascorbic acid, making the carbon point fluorescence less quenched.
The foregoing description is directed to the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the invention, and all equivalent changes or modifications made under the technical spirit of the present invention should be construed to fall within the scope of the present invention.
Claims (6)
1. The near-infrared nano carbon dot light conversion film is characterized by comprising near-infrared nano fluorescent carbon dots, ascorbic acid and polyvinyl alcohol, wherein the near-infrared nano fluorescent carbon dots, the ascorbic acid and the polyvinyl alcohol are in a mass ratio of (0.001-0.005): (0.0001-0.0005): 0.5;
the near infrared nanometer fluorescent carbon dots are synthesized by a one-step solvothermal method by using white magnolia leaf powder and an organic solvent, wherein the mass volume ratio of the white magnolia leaf powder to the organic solvent is 1g: 10-30 mL; the ultraviolet absorption wavelength and the excitation wavelength of the near infrared fluorescence nanometer carbon point are respectively 380-420 and 380-410 nm, and the emission peak wavelength range is 600-700 nm;
the preparation method of the near-infrared carbon nano-dot light conversion film comprises the following steps:
(1) Uniformly mixing white magnolia leaf powder and an organic solvent, transferring the mixture into a stainless steel reaction kettle, heating the mixture at a constant temperature of between 100 and 200 ℃ for 3 to 8 hours in a reactor, naturally cooling the mixture after the reaction is finished, centrifuging the obtained reactant, filtering the obtained supernatant by using a filter membrane, purifying the obtained filtrate by using a silica gel column chromatography, dynamically eluting the purified filtrate by using petroleum ether and ethyl acetate eluents with different volume ratios, collecting a dark green solution, and evaporating the solution under reduced pressure to obtain a dark green colloid product near infrared nanometer fluorescent carbon point;
(2) The near infrared nanometer fluorescent carbon dot colloid is added into the mixed solution of ethanol and deionized water, and ultrasonic treatment is carried out until the colloid is dissolved, thus obtaining near infrared nanometer fluorescent carbon dot alcohol solution;
(3) Adding ascorbic acid into deionized water, and performing ultrasonic treatment until solid is dissolved to obtain an ascorbic acid solution;
(4) Adding polyvinyl alcohol into deionized water, heating the solution at a constant temperature in a reactor until the solid is melted, and heating the solution to evaporate water until the whole solution is sticky to obtain a polyvinyl alcohol solution;
(5) Adding an ascorbic acid solution and a near infrared nano fluorescent carbon dot alcohol solution into a polyvinyl alcohol solution, continuously stirring, reacting for 5 minutes at constant temperature to uniformly disperse the ascorbic acid solution and the near infrared nano fluorescent carbon dot alcohol solution in the polyvinyl alcohol solution, removing bubbles to obtain a uniform composite solution, wherein the mass ratio of the near infrared nano fluorescent carbon dot to the ascorbic acid to the polyvinyl alcohol in the composite solution is (0.001-0.005): (0.0001-0.0005): 0.5;
(6) And a curing film forming step, namely casting the composite solution into a film, and air-drying, curing and forming to obtain the near infrared nano carbon point light conversion film.
2. The near infrared nanocarbon point light conversion film according to claim 1, wherein the organic solvent is an acetone solution, absolute ethanol or methanol.
3. The near infrared nanocarbon spot light conversion film according to claim 1, wherein in the near infrared nanocarbon spot colloid dissolution step, the dosage ratio of near infrared nanocarbon spot colloid, ethanol and deionized water is 4mg:1 to 5ml:0 to 4mL.
4. The near infrared nanocarbon spot light-converting film according to claim 3, wherein in the ascorbic acid dissolving step, the ratio of the ascorbic acid to deionized water is 10mg:5mL.
5. The near infrared nanocarbon point light conversion film according to claim 3, wherein the volume ratio of petroleum ether to ethyl acetate in the petroleum ether and ethyl acetate eluent is 3:1-1:1.
6. The use of the near infrared nanocarbon dot light conversion film of claim 1, wherein the near infrared nanocarbon dot light conversion film is used in crop planting or crop seedling.
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| CN111662524A (en) * | 2020-05-26 | 2020-09-15 | 华南农业大学 | Red fluorescent carbon dot light conversion film and preparation method and application thereof |
| CN112067587A (en) * | 2020-08-06 | 2020-12-11 | 福建医科大学 | Preparation of sulfur quantum dots with high quantum yield and method for measuring ascorbic acid by using sulfur quantum dots |
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