CN114574197A - Carbon dot-organic silicon composite fluorescent material and preparation method and application thereof - Google Patents
Carbon dot-organic silicon composite fluorescent material and preparation method and application thereof Download PDFInfo
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- CN114574197A CN114574197A CN202210182587.7A CN202210182587A CN114574197A CN 114574197 A CN114574197 A CN 114574197A CN 202210182587 A CN202210182587 A CN 202210182587A CN 114574197 A CN114574197 A CN 114574197A
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
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- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 claims description 2
- VZFDRQUWHOVFCA-UHFFFAOYSA-L disodium;2-sulfanylbutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(S)C([O-])=O VZFDRQUWHOVFCA-UHFFFAOYSA-L 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
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- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- 235000019265 sodium DL-malate Nutrition 0.000 claims description 2
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- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- 239000001394 sodium malate Substances 0.000 claims description 2
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- 238000004519 manufacturing process Methods 0.000 claims 1
- XQGWAPPLBJZCEV-UHFFFAOYSA-N triethoxy(propyl)silane;urea Chemical compound NC(N)=O.CCC[Si](OCC)(OCC)OCC XQGWAPPLBJZCEV-UHFFFAOYSA-N 0.000 claims 1
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- 229910018540 Si C Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/054—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means
- H01L31/055—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means where light is absorbed and re-emitted at a different wavelength by the optical element directly associated or integrated with the PV cell, e.g. by using luminescent material, fluorescent concentrators or up-conversion arrangements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a carbon dot-organic silicon composite fluorescent material and a preparation method and application thereof, belonging to the technical field of optical functional materials. Adding a mixed reactant containing micromolecular organic acid and/or salt thereof, amino-containing organosilane and the like into a mixed solvent consisting of deionized water and absolute ethyl alcohol, uniformly mixing, carrying out solvothermal reaction on the obtained mixed reaction liquid, setting the reaction temperature to be 180-200 ℃, and the reaction time to be 4-12 h; and after the reaction is finished, centrifuging, washing and drying the obtained product to obtain the carbon dot-organic silicon composite fluorescent material. The invention realizes the regulation and control of the fluorescence of the composite fluorescent material from blue light to orange light, has stable solid fluorescence, and can be used for constructing a high-efficiency luminescent solar concentrator. The method has the advantages of easy preparation and purification, environmental protection, no toxicity and the like, and has good theoretical research and practical application values. The method for preparing the light collector is simple and convenient and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of optical functional materials, and particularly relates to a carbon dot-organic silicon composite fluorescent material as well as a preparation method and application thereof.
Background
The luminescent solar light collector is a novel sunlight collecting device, and can greatly reduce the use area of a monocrystalline silicon battery, thereby reducing the cost of solar power generation. The typical luminescent solar concentrator is composed of a fluorescent material and a waveguide material, and light absorbed and re-emitted by the fluorescent material reaches a silicon cell coupled at the edge through total internal reflection in the waveguide material, so that low-cost and high-efficiency conversion of solar energy into electric energy is realized.
Since the discovery of carbon dots as a novel fluorescent material, carbon dots are favored by researchers because of their advantages of non-toxicity, greenness, easy preparation, high chemical stability, excellent optical properties, etc., and have a very high application prospect in many fields such as illumination, probes, catalysis, energy, etc. The excellent properties of carbon dots have also attracted more and more researchers to apply them to luminescent solar concentrators in recent years. However, most of the carbon dots are affected by aggregation-induced quenching effect after being dried into thin film or powder, the fluorescence intensity is sharply reduced or even disappears, and the application of the carbon dots in solid-state devices is seriously hindered, so that the research on preparing the carbon dots with stable solid-state fluorescence is very practical.
Disclosure of Invention
In view of the problems or defects of the prior art, the present invention aims to provide a carbon dot-organosilicon composite fluorescent material, and a preparation method and an application thereof. The composite fluorescent material prepared by the method has stable solid fluorescence, can be used for constructing a high-efficiency luminescent solar concentrator, and solves or at least partially solves the technical defects in the prior art.
In order to achieve one of the above objects of the present invention, the present invention adopts the following technical solutions:
a preparation method of a carbon dot-organic silicon composite fluorescent material specifically comprises the following steps:
adding the mixed reactant into a mixed solvent consisting of deionized water and absolute ethyl alcohol, uniformly mixing, and carrying out solvothermal reaction on the obtained mixed reaction liquid, wherein the reaction temperature is set to be 180-200 ℃, and the reaction time is 4-12 hours; after the reaction is finished, centrifuging, washing and drying the obtained product to obtain the carbon dot-organic silicon composite fluorescent material; wherein:
the mixed reactant is composed of small molecular organic acid and/or salt thereof and organosilane containing amino; or the mixed reactant is composed of small-molecule organic acid and/or salt thereof, nitrogen-containing small molecules and amino-containing organosilane.
Further, in the above technical solution, the small molecule organic acid is at least one of citric acid, malic acid, tartaric acid, thiomalic acid, and the like.
In the above embodiment, the salt of the small molecule organic acid includes alkali metal salts of the small molecule organic acids, especially water-soluble salts such as sodium salts, potassium salts and/or ammonium salts thereof, and preferably the salt is at least one of sodium citrate, sodium malate, sodium tartrate, sodium thiomalate, and the like.
Furthermore, in the technical scheme, the organosilane containing the amino group is at least one of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, ureidopropyltriethoxysilane, 1- [3- (trimethoxysilyl) propyl ] urea, N- [3- (trimethoxysilyl) propyl ] ethylenediamine and the like.
Further, according to the technical scheme, the molar ratio of the amino-containing organosilane to the small-molecule organic acid and/or the salt thereof is 6: 1-1: 1.
Further, in the above technical scheme, the nitrogen-containing small molecule is at least one of urea, thiourea, dicyanodiamine and the like.
Further, in the above technical solution, the molar ratio of the nitrogen-containing small molecule to the small molecule organic acid and/or the salt thereof is m, wherein: m is more than 0:1 and less than or equal to 32: 1.
Further, according to the technical scheme, the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solvent is 15: 15-5: 25.
The second purpose of the invention is to provide the carbon dot-organic silicon composite fluorescent material prepared by the method.
The third purpose of the invention is to provide the application of the carbon dot-organic silicon composite fluorescent material prepared by the method in the preparation of Luminescent Solar Collectors (LSCs).
A luminescent solar concentrator comprising a glass or plastic waveguide forming a concentrator body, and a phosphor coating a surface of the body, wherein: the phosphor comprises the carbon dot-organic silicon composite fluorescent material.
Further, in the above technical solution, the body of the present invention is preferably a glass substrate.
Preferably, in the above technical solution, the size of the glass substrate is between 2.5 × 2.5 × 1mm and 5 × 5 × 1 mm.
The invention also provides a preparation method of the luminescent solar energy concentrator, which comprises the following steps:
mixing the carbon dot-organic silicon composite fluorescent material with polysiloxane, and uniformly stirring; and then adding a catalyst, continuously stirring uniformly, coating the obtained coating liquid on the surface of the body, and curing at room temperature to obtain the luminescent solar light collector.
Further, in the above technical solution, the polysiloxane is at least one of polydimethylsiloxane, silicone resin, and the like.
Further, in the above technical solution, the catalyst is a titanate catalyst (for example
722 titanate chelates) or tin-based catalysis (e.g., at least one of dibutyltin dilaurate, stannous octoate, etc.) for catalyzing alkoxy dealcoholization cross-linking polymerization of polysiloxanes.
Furthermore, according to the technical scheme, the dosage of the catalyst is 1/1000-10/1000 of the mass of polysiloxane, and 3/1000 is more preferable.
Further, in the technical scheme, the carbon dot-organic silicon composite fluorescent material accounts for 5-20 wt% of the coating liquid.
Further, in the above technical solution, the coating method includes, but is not limited to, any one of spin coating, drop coating, knife coating, spray coating, and solution shearing.
Preferably, in the technical scheme, the coating method preferably adopts spin coating, the rotating speed of a spin coating machine is 1500 r/min-3000 r/min, and the spin coating time is 30-60 s.
Further, according to the technical scheme, the mixing and stirring time of the carbon dot-organic silicon composite fluorescent material and polysiloxane is any time between 1 and 4 hours.
Further, according to the technical scheme, the stirring time after the catalyst is added is 1-5 min.
Further, according to the technical scheme, the room temperature curing time is 36-72 hours, and preferably 48 hours.
The reaction principle of the invention and the functions of the raw materials are as follows:
under the condition of not adding urea, the small molecular organic acid and/or the salt thereof is used as a carbon source to form carbon points; in the case of adding a nitrogen-containing small molecule, a small molecule organic acid and/or a salt thereof serves as a carbon source, and a nitrogen-containing small molecule serves as a nitrogen source, and both together form a carbon site. The surface of the carbon dot generated by the invention contains a large amount of carboxyl, and the carboxyl can be connected with the amino in the amino-containing organosilane through amidation reaction, and simultaneously, siloxane in the amino-containing organosilane forms a 'Si-O-Si' network structure by taking the carbon dot as a hydrolysis and polycondensation center under the solvothermal condition, thereby wrapping the carbon dot.
Compared with the prior art, the invention has the following beneficial effects:
(1) the carbon dot-organic silicon composite fluorescent material prepared by the invention shows blue light emission under the condition that no small nitrogen-containing molecules are added, the molar ratio of the small nitrogen-containing molecules to the small molecular organic acid and/or the salt thereof in the reaction system is increased to 16:1, the composite fluorescent material shows green light emission, and the molar ratio of the small nitrogen-containing molecules to the small molecular organic acid and/or the salt thereof in the reaction system is further increased to 32:1, so that the composite material shows yellow light emission. On the basis of a yellow light emitting system, the ratio of the amino-containing organosilane to the small-molecule organic acid and/or the salt thereof is further reduced to 2:1, and the fluorescence of the composite fluorescent material can be regulated to orange light emission, so that the regulation of the fluorescence of the composite fluorescent material from blue light to orange light is realized. Yellow light and orange light emission belong to long wavelength emission, and the defect that carbon dot light wavelength is concentrated in blue-green light and other short wavelength emission in the prior art is overcome.
(2) The blue light, green light, yellow light and orange light carbon dot-organic silicon composite fluorescent materials prepared by the method have the fluorescence quantum yields of 54 percent, 43 percent, 33 percent and 21 percent respectively, and have the potential of preparing high-performance solid devices.
(3) The composite fluorescent material prepared by the invention belongs to a carbon dot fluorescent material coated by polysiloxane, and has good compatibility with most silicon-based materials. In the invention, after the polysiloxane is fully stirred, the mixing content can reach 20 wt%, and a transparent and uniform film can be formed after the polysiloxane is coated on a glass substrate in a spin mode, and obvious agglomeration or uneven dispersion is avoided.
(4) The invention preferably adopts a spin-coating method to prepare the light collector, has simple preparation method and mild curing conditions, and is suitable for industrial large-scale production.
(5) The carbon dot-organic silicon composite fluorescent material prepared by the invention is used for synthesizing a precursor, the solvent is cheap and non-toxic, and the product and the by-product are non-toxic and harmless; the preparation process of the method is suitable for green large-scale production; the obtained solid product can be purified by washing and centrifuging, and the purification step is simple and easy to implement; the obtained product has excellent optical performance and good theoretical research and practical application values.
Drawings
The left graph in FIG. 1 is a comparison graph of the emission spectra of the carbon dot-organosilicon composite fluorescent materials prepared in examples 1-4; the right graph in FIG. 1 is a comparison graph of the emission spectra of the carbon dot-organosilicon composite fluorescent materials prepared in examples 5-8;
FIG. 2 is a photo of a carbon dot-organosilicon composite fluorescent material prepared in examples 1-4 of the present invention under a fluorescent lamp and a 365nm ultraviolet lamp, respectively; wherein: the first row is a real photograph of the fluorescent material prepared in example 1, example 2, example 3 and example 4 under a fluorescent lamp from left to right; the second row is a photo of the fluorescent material prepared in example 1, example 2, example 3, and example 4 under a 365nm ultraviolet lamp from left to right;
FIG. 3 is an HRTEM image of the carbon dot-organosilicon composite fluorescent material prepared in examples 1-4; wherein:
a) the method comprises the following steps Example 1; b) the method comprises the following steps Example 2; c) the method comprises the following steps Example 3; d) the method comprises the following steps Example 4;
FIG. 4 is an FESEM photograph of the carbon dot-organosilicon composite fluorescent materials prepared in examples 1-4; wherein:
a) the method comprises the following steps Example 1; b) the method comprises the following steps Example 2; c) the method comprises the following steps Example 3; d) the method comprises the following steps Example 4;
FIG. 5 is a comparison graph of IR spectra of the carbon dot-organosilicon composite fluorescent materials prepared in examples 1-4;
FIG. 6 is a fluorescence spectrum of the carbon dot-organosilicon composite fluorescent material prepared in examples 1-4 under different excitation wavelengths; wherein: a) the method comprises the following steps Example 1; b) the method comprises the following steps Example 2; c) the method comprises the following steps Example 3; d) the method comprises the following steps Example 4;
FIG. 7 is a graph comparing normalized absorption spectra of the carbon dot-organosilicon composite fluorescent materials prepared in examples 1-4;
FIG. 8 is a photograph comparison of luminescent solar collectors respectively prepared in application examples 1 to 4 under natural light and 365nm ultraviolet light;
FIG. 9 is a graph comparing the photocurrent curves of the light collectors prepared in examples 1-4.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
According to the invention, mixed reactants with different molar ratios are added into a mixed solvent consisting of deionized water and absolute ethyl alcohol for solvothermal reaction, and the obtained product is centrifuged, washed and dried to obtain solid powder with a specific fluorescence emission wavelength. The powder can be mixed with polysiloxane, and after a catalyst is added, a high-efficiency luminescent solar light collector can be obtained by spin coating on a glass substrate and curing at room temperature; wherein: the mixed reactant is composed of small molecular organic acid and/or salt thereof and organosilane containing amino; or the mixed reactant is composed of small-molecule organic acid and/or salt thereof, nitrogen-containing small molecules and amino-containing organosilane.
The equipment and raw materials used in the present invention are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid and 3.78mL of 3-aminopropyltriethoxysilane (Aladdin reagent Co., CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 10mL of deionized water and 20mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 200 ℃ for 12 hours. After the reaction product is centrifugally separated from solid and liquid, the solid is respectively washed by deionized water and absolute ethyl alcohol for three times, and is dried in an oven at 50 ℃ overnight to obtain white powder.
As can be seen from FIG. 1, the carbon dot-organosilicon composite fluorescent material prepared in this example emits blue light under a 365nm ultraviolet lamp.
Example 2
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 2.6g of urea and 3.78mL of 3-aminopropyltriethoxysilane (Aladdin reagent, CAS number: 919-30-2, density: 0.95 g/cm)3) DissolutionIn a mixed solvent composed of 10mL of deionized water and 20mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 200 ℃ for 12 hours. After the solid-liquid separation of the reaction product, the solid is washed three times by deionized water and absolute ethyl alcohol respectively, and is dried in an oven at 50 ℃ overnight to obtain light yellow powder.
As can be seen from FIG. 1, the carbon dot-organosilicon composite fluorescent material prepared in this example emits green light under a 365nm ultraviolet lamp.
Example 3
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 5.2g of urea and 3.78mL of 3-aminopropyltriethoxysilane (Aladdin reagent, CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent consisting of 10mL of deionized water and 20mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 200 ℃ for 12 hours. After the solid-liquid separation of the reaction product, the solid is washed three times by deionized water and absolute ethyl alcohol respectively, and is dried in an oven at 50 ℃ overnight to obtain yellow powder.
As can be seen from FIG. 1, the carbon dot-organosilicon composite fluorescent material prepared in this example has yellow light emission under a 365nm ultraviolet lamp.
Example 4
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 5.2g of urea and 1.26mL of 3-aminopropyltriethoxysilane (Aladdin reagent, CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 10mL of deionized water and 20mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 200 ℃ for 12 hours. After the reaction product is centrifugally separated from solid and liquid, the solid is respectively washed three times by deionized water and absolute ethyl alcohol and is placed at 50 ℃ for dryingOven dried overnight to give an orange powder.
As can be seen from FIG. 1, the carbon dot-organosilicon composite fluorescent material prepared in this example emits orange light under a 365nm ultraviolet lamp.
Example 5
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid and 3.78mL of 3-aminopropyltriethoxysilane (Allantin reagent Co., CAS No.: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 15mL of deionized water and 15mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 180 ℃ for 12 hours. After the solid-liquid separation of the reaction product, the solid was washed three times with deionized water and absolute ethanol, and dried overnight in an oven at 50 ℃ to give a white powder.
The carbon dot-organic silicon composite fluorescent material prepared in the embodiment shows blue light emission under a 365nm ultraviolet lamp.
Example 6
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 2.6g of urea and 3.78mL of 3-aminopropyltriethoxysilane (Aladdin reagent, CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 15mL of deionized water and 15mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 180 ℃ for 12 hours. After the solid-liquid separation of the reaction product, the solid is washed three times by deionized water and absolute ethyl alcohol respectively, and is dried in an oven at 50 ℃ overnight to obtain light yellow powder.
The carbon dot-organic silicon composite fluorescent material prepared in the embodiment shows green light emission under a 365nm ultraviolet lamp.
Example 7
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 5.2g of urea and 3.78mL of 3-aminopropyltriethoxysilane (Allantin reagent Co., CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 15mL of deionized water and 15mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 180 ℃ for 12 hours. After the solid-liquid separation of the reaction product, the solid was washed three times with deionized water and absolute ethanol, respectively, and dried in an oven at 50 ℃ overnight to give a yellow powder.
The carbon dot-organosilicon composite fluorescent material prepared by the embodiment has yellow green light emission under a 365nm ultraviolet lamp.
Example 8
The preparation method of the carbon dot-organosilicon composite fluorescent material of the embodiment specifically comprises the following steps:
0.52g of citric acid, 5.2g of urea and 1.26mL of 3-aminopropyltriethoxysilane (Aladdin reagent, CAS number: 919-30-2, density: 0.95 g/cm)3) Dissolved in a mixed solvent composed of 10mL of deionized water and 20mL of absolute ethyl alcohol. The resulting mixed reaction solution was transferred to a teflon-lined stainless steel autoclave and kept in a forced air drying oven at 200 ℃ for 4 hours. After the solid-liquid separation of the reaction product, the solid was washed three times with water and absolute ethanol, respectively, and dried overnight in an oven at 50 ℃ to give a yellow powder.
The carbon dot-organic silicon composite fluorescent material prepared in the embodiment emits yellow light under a 365nm ultraviolet lamp.
The left image in FIG. 1 is an emission spectrum of the carbon dot-organosilicon composite fluorescent material prepared in examples 1-4, and emission peaks of the carbon dot-organosilicon composite fluorescent material are sequentially at 448nm, 518nm, 555nm and 585 nm. From example 1 to example 3, the reaction amount of urea is gradually increased, the fluorescence of the composite material is red-shifted from blue light to yellow light, and in example 4, the reaction amount of 3-aminopropyltriethoxysilane is further reduced on the basis of the reaction of example 3, and the fluorescence is further red-shifted to orange light, so that the regulation of the fluorescence from blue light to orange light is realized.
The right graph in FIG. 1 shows the emission spectra of the carbon dot-organosilicon composite fluorescent materials prepared in examples 5-8, and the emission peaks are sequentially located at 486nm, 510nm, 529nm and 551 nm. Examples 5 to 8 show that fluorescence emitted at a specific wavelength can be obtained by changing the reaction solvent ratio, the reaction temperature, and the reaction time. Since the fluorescence modulation of examples 1-4 is more regular with the change of reaction conditions, the following four examples are representative for further discussion.
FIG. 2 is a photograph of the carbon dot-organosilicon composite fluorescent material of examples 1-4 under the irradiation of a fluorescent lamp and a 365nm ultraviolet lamp. The fluorescence of the products prepared in examples 1-4 under ultraviolet light is blue, green, yellow and orange respectively.
The particle size and the crystal lattice of the carbon dots in the carbon dot-organic silicon composite fluorescent material prepared in examples 1 to 4 are observed under a high-power transmission electron microscope in fig. 3, and it can be seen from the HRTEM photograph in fig. 3 that the carbon dots are uniformly dispersed and do not agglomerate. The lattice spacing of the carbon dots in the composite fluorescent material of the embodiments 1 to 4 is 0.21nm, which corresponds to the (001) crystal face of graphene. The particle sizes of the carbon dots in the composite fluorescent material in the embodiments 1 to 4 are 3.13nm, 3.21nm, 3.37nm and 4.19nm in sequence.
When the morphology of the carbon dot-organosilicon composite fluorescent material described in examples 1-4 is observed under a Field Emission Scanning Electron Microscope (FESEM), as can be seen from an FESEM photograph in fig. 4, the samples in examples 1 and 2 show a cross-linked irregular structure, because the content of citric acid or citric acid and urea in the systems of examples 1 and 2 is less than that of 3-aminopropyltriethoxysilane, and after the carbon dots are wrapped by silane, the excessive silane can still react with silane which is not completely condensed and is wrapped outside the carbon dots, so that a cross-linked structure is formed by condensation polymerization. The sample in example 3 has a spheroidal structure, but there is still some cross-linking between the "spheres" and "spheres" due to the increased urea content in the system compared to example 2, resulting in increased carbon sites being formed and consequently increased silane used to encapsulate the carbon sites, which results in a relative reduction in free silane. Finally, the sample of example 3 exhibited a relatively larger size and a relatively smaller degree of crosslinking than those of examples 1 and 2. In example 4, the amount of silane reaction was further reduced, and the carbon dots tended to form spheres under the encapsulation of the silane without significant crosslinking.
FIG. 5 is an infrared spectrum of the carbon dot-organosilicon composite fluorescent material according to examples 1-4. It can be seen that the infrared spectra of the 4 composite fluorescent materials are basically consistent, wherein the infrared spectra are 947-1171 cm-1Stretching vibrations attributed to Si-O-Si and Si-C bonds indicate that 3-aminopropyltriethoxysilane forms polysiloxane during hydrothermal processing. At 1654cm-1The vibration of (A) indicates that-OH on the surface of the carbon dots and-NH of 3-aminopropyltriethoxysilane2An amide bond (C ═ ONHR) is formed during the reaction. The above results in combination with FESEM can confirm that the carbon dots are combined with 3-aminopropyltriethoxysilane in the form of cross-linking dots, and the ethoxy group is hydrolyzed and condensed to form a polysiloxane-coated carbon dot-organosilicon composite material.
FIG. 6 shows fluorescence spectra of the carbon dot-organosilicon composite fluorescent materials of examples 1-4 under different excitation wavelengths. As can be seen from fig. 6, 4 kinds of composite fluorescent materials all exhibit excitation-independent emission, wherein the optimal excitation wavelength of the composite fluorescent materials described in examples 1 and 2 is 400nm, and the corresponding maximum emission is 448nm and 518nm, respectively, which are blue light and green light emission. The optimal excitation wavelength of the composite fluorescent materials described in examples 3 and 4 is 470nm, and the corresponding maximum emission is 555nm and 585nm, respectively, which belong to yellow light emission and orange light emission. The fluorescence quantum yields of the carbon dot-organic silicon composite fluorescent materials of examples 1 to 4 are 54%, 43%, 33% and 21%, respectively. The fluorescence quantum yield was measured by placing the powder on a four-way quartz cuvette on a PicoQuant Fluo Time 300, measuring with an integrator, and calculating by software, with excitation light sources of 420nm for examples 1 and 2, and 485nm for examples 3 and 4.
FIG. 7 is a normalized absorption spectrum of the carbon dot-organosilicon composite fluorescent material of examples 1-4. It can be seen that the absorption peak between 300nm and 350nm can be attributed to pi-pi of the C ═ C and C ═ O bonds*And (4) transition.The absorption of the composite phosphor gradually increases from blue to orange, probably due to the n-pi increase caused by the increase of the nitrogen content*Enhancement of the transition. The absorption enhancement in the long wavelength range is advantageous for the efficient absorption and utilization of sunlight by the luminescent solar concentrator.
Application example 1
The luminescent solar concentrator of the application embodiment is prepared by the following method:
0.25g of the carbon dot-organosilicon composite fluorescent material prepared in example 1 was added to 1g of polydimethylsiloxane (mixing ratio: 20 wt%), and stirred for 4 hours. After stirring thoroughly, 0.003g of
722 and stirring is continued for 5 min. Subsequently, the resulting mixture was dropped onto a 2.5X 1mm glass substrate, and spin-coated at a rotation speed of 2500r/min to form a film. The resulting sample was cured at room temperature for 48 hours to yield a transparent, blue-fluorescent luminescent solar concentrator.
Application example 2
The luminescent solar concentrator of the application embodiment is prepared by the following method:
0.18g of the carbon dot-organosilicon composite fluorescent material prepared in example 2 was added to 1g of polydimethylsiloxane (mixing ratio: 15 wt%), and stirred for 4 hours. After stirring thoroughly, 0.003g of
722 and stirring is continued for 5 min. Subsequently, the resulting mixture was dropped onto a 2.5X 1mm glass substrate, and spin-coated at a rotation speed of 2500r/min to form a film. The obtained sample is cured for 48 hours at room temperature to obtain the transparent luminescent solar light collector with green fluorescence.
Application example 3
The luminescent solar concentrator of the application embodiment is prepared by the following method:
0.18g of the carbon dot-organosilicon composite fluorescent material prepared in example 3 was added to 1g of polydimethylsiloxane (mixing ratio: 15 wt%)) And stirring for 4 hours. After stirring thoroughly, 0.003g of
722 and stirring is continued for 5 min. Subsequently, the resulting mixture was dropped onto a 2.5X 1mm glass substrate, and spin-coated at a rotation speed of 2500r/min to form a film. The obtained sample is solidified for 48 hours at room temperature to obtain the transparent luminescent solar light collector with yellow fluorescence.
Application example 4
The luminescent solar concentrator of the application embodiment is prepared by the following method:
0.18g of the carbon dot-organosilicon composite fluorescent material prepared in example 4 was added to 1g of polydimethylsiloxane (mixing ratio: 15 wt%), and stirred for 4 hours. After stirring thoroughly, 0.003g of
722 and stirring is continued for 5 min. Subsequently, the resulting mixture was dropped onto a 2.5X 1mm glass substrate, and spin-coated at a rotation speed of 2500r/min to form a film. The resulting sample was cured at room temperature for 48 hours to yield a transparent, orange fluorescent luminescent solar concentrator.
Fig. 8 is a photograph comparison of the luminescent solar collectors prepared in application examples 1 to 4 under natural light and 365nm ultraviolet light, respectively. As can be seen from the figure, the prepared light collector has good transparency under natural light, and characters at the bottom of the light collector can be clearly seen. Under the ultraviolet light, the fluorescence of the light collector is consistent with the fluorescence of the corresponding composite fluorescent material, and strong fluorescence is emitted.
The collectors prepared in application examples 1 to 4 were coupled to the edge of a commercial solar silicon cell (cell parameter: V)oc,JscPCE, and EQE are 0.48V,41.28mA/cm, respectively214% and 16%, the effective area of the cell being 25X 1mm) under simulated sunlight (AM 1.5G, 100mW/cm2) The photocurrent parameters of the concentrator-cell systems were determined using a source meter and their external optical efficiency was calculated. FIG. 9 is a graph of photocurrent for light collectors prepared using examples 1-4. The assemblies prepared in application examples 1 to 4J of optical devicescRespectively at 13.15, 9.58, 10.99 and 7.30mA/cm2. Calculating the external optical efficiency (η) of the collector using the following formulaopt)：
Where G is the geometric gain, defined as the ratio of the area of the top of the collector to the area of the edge. I.C. ASCIs the short-circuit current of the silicon cell under the simulated sunlight. I isLSCIs the short circuit current of the silicon cell under simulated sunlight when the light collector is coupled with the silicon cell.
Eta calculated for the collectors prepared in application examples 1-4opt5.10%, 3.71%, 4.26% and 2.83%, respectively.
Claims (10)
1. A preparation method of a carbon dot-organic silicon composite fluorescent material is characterized by comprising the following steps: the method specifically comprises the following steps:
adding the mixed reactant into a mixed solvent consisting of deionized water and absolute ethyl alcohol, uniformly mixing, and carrying out solvothermal reaction on the obtained mixed reaction liquid, wherein the reaction temperature is set to be 180-200 ℃, and the reaction time is 4-12 hours; after the reaction is finished, centrifuging, washing and drying the obtained product to obtain the carbon dot-organic silicon composite fluorescent material; wherein:
the mixed reactant is composed of small molecular organic acid and/or salt thereof and organosilane containing amino; or the mixed reactant is composed of small-molecule organic acid and/or salt thereof, nitrogen-containing small molecules and amino-containing organosilane.
2. The method for preparing the carbon dot-organosilicon composite fluorescent material according to claim 1, wherein: the small molecular organic acid is at least one of citric acid, malic acid, tartaric acid and thiomalic acid; the salt of the small molecular organic acid is at least one of sodium citrate, sodium malate, sodium tartrate and sodium thiomalate.
3. The method for preparing the carbon dot-organosilicon composite fluorescent material according to claim 1, wherein: the organosilane containing amino is at least one of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, urea propyl triethoxysilane, 1- [3- (trimethoxysilyl) propyl ] urea and N- [3- (trimethoxysilyl) propyl ] ethylenediamine.
4. The method for preparing the carbon dot-organosilicon composite fluorescent material according to claim 1, wherein: the nitrogen-containing micromolecules are at least one of urea, thiourea and dicyanodiamine.
5. The method for preparing the carbon dot-organosilicon composite fluorescent material according to claim 1, wherein: the mol ratio of the amino-containing organosilane to the small-molecule organic acid and/or the salt thereof is 6: 1-1: 1.
6. The method for preparing the carbon dot-organosilicon composite fluorescent material according to claim 1, wherein: the mole ratio of the nitrogen-containing micromolecules to the micromolecule organic acid and/or the salt thereof is m, wherein: m is more than 0:1 and less than or equal to 32: 1.
7. The carbon dot-organosilicon composite fluorescent material prepared by the method for preparing the carbon dot-organosilicon composite fluorescent material according to any one of claims 1 to 6.
8. The application of the carbon dot-organic silicon composite fluorescent material prepared by the method of any one of claims 1 to 6 in preparing a luminescent solar concentrator.
9. A luminescent solar concentrator, characterized by: comprising a glass or plastic waveguide forming a light collector body, and a phosphor coated on a surface of the body, wherein: the phosphor comprises the carbon dot-organic silicon composite fluorescent material prepared by the method of any one of claims 1 to 6.
10. The method of making a luminescent solar concentrator as defined in claim 9, wherein: the method comprises the following steps:
mixing the carbon dot-organic silicon composite fluorescent material with polysiloxane, and uniformly stirring; and then adding a catalyst, continuously stirring uniformly, coating the obtained coating liquid on the surface of the body, and curing at room temperature to obtain the luminescent solar light collector.
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