CN110878205A - Carbon dot-based fluorescent powder, and preparation method and application thereof - Google Patents
Carbon dot-based fluorescent powder, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a preparation method of carbon dot-based fluorescent powder, which comprises the following steps: s1) mixing the first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product; s2) mixing the intermediate product with a second amino-containing organic compound in water, and carrying out microwave heating for reaction to obtain the carbon dot-based fluorescent powder. Compared with the prior art, the carbon dots are formed by the organic acid and the first amino-containing organic compound in the first step, the second amino-containing organic compound added in the second step forms graphite-phase carbon nitride, the carbon dots can be uniformly distributed in the second amino-containing organic compound solution on one hand, so that the carbon dots are uniformly coated in the second amino-containing organic compound solution or bonded on the surface while the graphite-phase carbon nitride is formed, the aggregation-induced fluorescence quenching of the carbon dots is prevented, the solid-state luminescence of the carbon dots is realized, the luminous efficiency is high, and the luminous color of the carbon dot-based fluorescent powder can be adjusted by changing the content of the carbon dots on the other hand.
Description
Technical Field
The invention belongs to the technical field of carbon dots, and particularly relates to carbon dot-based fluorescent powder, and a preparation method and application thereof.
Background
Carbon dots, namely CDs, one of the most promising carbon-based materials, can impart a light emitting property to the carbon material when the carbon is tailored in a certain nanometer range based on quantum size effect. Recently, carbon dots have received much attention due to their environmentally friendly chemical composition, excellent optical properties, high water solubility, excellent biocompatibility, low toxicity and ease of preparation, and have demonstrated their potential applications in the fields of bio-imaging, biosensors and photoelectric devices, etc.
The photoluminescence effect of the carbon dots makes the carbon dots have the potential to become a light conversion layer of the LED and prepare a white light LED device. But the main reason that hinders its application is that the carbon spots in the aggregated state are quenched by the induced luminescence, so the illumination application in WLEDs progresses very slowly.
At present, a common way to overcome the luminescence quenching of solid carbon dots in white LED applications is to disperse the carbon dots on a substrate such as inorganic salt, but the introduction of the substrate in a physical adsorption manner is often not conducive to efficient luminescence of the carbon dots.
Chinese patent publication No. CN105647529 discloses a method for preparing carbon dot-based solid-state phosphor, wherein the method for preparing carbon dot-based solid-state phosphor is to electrostatically adsorb carbon dots in a carbon dot solution on the surface of starch by adding starch into the carbon dot solution. However, the experimental process of this method is complicated and time-consuming, and the light emitting efficiency of the WLED prepared thereby is relatively low.
Chinese patent publication No. CN107519907 discloses a carbon dot and graphite phase carbon nitride composite photocatalyst, wherein the carbon dot and graphite phase carbon nitride composite photocatalyst is obtained by calcining urea or dicyandiamide at a carbon dot temperature of 450-550 ℃.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a carbon dot-based phosphor with adjustable luminous efficiency and color, and a preparation method and an application thereof.
The invention provides a preparation method of carbon dot-based fluorescent powder, which comprises the following steps:
s1) mixing the first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product;
s2) mixing the intermediate product with a second amino-containing organic compound in water, and carrying out microwave heating for reaction to obtain the carbon dot-based fluorescent powder.
Preferably, the first and second amino group-containing organic compounds are each independently selected from one or more of urea, ammonium oxalate, tyrosine, glycine and ethylenediaminetetraacetic acid; the organic acid is selected from one or more of ascorbic acid, tartaric acid, malic acid and citric acid.
Preferably, the mass ratio of the total mass of the first amino group-containing organic compound and the second amino group-containing organic compound to the organic acid is (1000 to 40): 1.
preferably, the mass ratio of the first amino group-containing organic compound to the second amino group-containing organic compound is 1: (500-20).
Preferably, the power of microwave heating in the step S1) is 500-1000W; the reaction time is 3-5 min; the power of microwave heating in the step S2) is 500-1000W; the reaction time is 3-5 min.
Preferably, in the step S1), the mass-to-volume ratio of the organic acid to the water is (0.1-10) mg: 1 ml.
Preferably, the carbon dot-based phosphor is a blue light emitting carbon dot-based phosphor, a green light emitting carbon dot-based phosphor, or a yellow light emitting carbon dot-based phosphor.
The invention also provides the carbon dot-based fluorescent powder prepared by the method, and the carbon dot-based fluorescent powder is a compound of carbon dots and graphite-phase carbon nitride.
The invention also provides an LED which comprises the carbon dot-based fluorescent powder.
The invention provides a preparation method of carbon dot-based fluorescent powder, which comprises the following steps: s1) mixing the first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product; s2) mixing the intermediate product with a second amino-containing organic compound in water, and carrying out microwave heating for reaction to obtain the carbon dot-based fluorescent powder. Compared with the prior art, the carbon dots are formed by the organic acid and the first amino-containing organic compound in the first step, the second amino-containing organic compound added in the second step forms graphite-phase carbon nitride, the carbon dots can be uniformly distributed in the second amino-containing organic compound solution on one hand, so that the carbon dots are uniformly coated in the second amino-containing organic compound solution or bonded on the surface while the graphite-phase carbon nitride is formed, the aggregation-induced fluorescence quenching of the carbon dots is prevented, the solid-state luminescence of the carbon dots is realized, the luminous efficiency is high, and the luminous color of the carbon dot-based fluorescent powder can be adjusted by changing the content of the carbon dots on the other hand.
Drawings
FIG. 1 is an excitation and emission spectrum of a carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 2 is a scanning tunneling electron micrograph of the carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 3 is a TEM image of carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of the carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 5 is a three-dimensional fluorescence spectrum of the carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 6 is a fluorescent micrograph of a carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 7 is a graph showing the results of the fluorescence quantum efficiency test of the carbon dot-based phosphor obtained in example 1 of the present invention;
FIG. 8 is a steady state spectrum of a carbon dot-based phosphor obtained in example 2 of the present invention;
FIG. 9 is a photograph of a white LED obtained in example 3 of the present invention and its emission spectrum during operation;
FIG. 10 is a steady state spectrum of the carbon dot-based phosphor obtained in example 4 of the present invention under excitation of a 360nm light source;
FIG. 11 is a photograph under ultraviolet light of the carbon dot-based phosphor obtained in example 4 of the present invention;
FIG. 12 is an absorption and emission spectrum of a green fluorescent carbon dot solution obtained in comparative example 1 of the present invention;
FIG. 13 is a graph showing a steady state spectrum of a blue-emitting graphite-phase carbonitride phosphor obtained in comparative example 1 of the present invention;
FIG. 14 is a graph comparing the spectra of the carbon dot-based phosphor obtained in example 1 and the P-carbon dot-based phosphor obtained in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of carbon dot-based fluorescent powder, which comprises the following steps: s1) mixing the first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product; s2) mixing the intermediate product with a second amino-containing organic compound in water, and carrying out microwave heating for reaction to obtain the carbon dot-based fluorescent powder.
In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available.
Mixing a first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product; the first amino-containing organic compound is preferably one or more of urea, ammonium oxalate, tyrosine, glycine and ethylenediamine tetraacetic acid, and is more preferably urea; the organic acid is preferably one or more of ascorbic acid, tartaric acid, malic acid and citric acid, and is more preferably citric acid; the mass ratio of the organic acid to the first amino group-containing organic compound is preferably 1: (1 to 4), more preferably 1: (2-4), and more preferably 1: (2-3); the mass-volume ratio of the organic acid to the water is preferably (0.1-10) mg: 1ml, more preferably (0.5-8) mg: 1ml, more preferably (0.6-7.2) mg: 1 ml; the mixing is preferably to complete dissolution; the power of the microwave heating is preferably 500-1000W, more preferably 600-900W, still more preferably 700-800W, and most preferably 750W; the reaction time of the microwave heating is preferably 3-5 min, and more preferably 3-4 min.
Mixing the intermediate product and a second amino-containing organic compound in water, and carrying out microwave heating for reaction; the second amino-containing organic compound is preferably one or more of urea, ammonium oxalate, tyrosine, glycine and ethylenediamine tetraacetic acid, and is more preferably urea; the mass ratio of the total mass of the first amino group-containing organic compound and the second amino group-containing organic compound to the organic acid is preferably (1000 to 40): 1, more preferably (750-45): 1, and preferably (558-48): 1; the mass ratio of the first amino group-containing organic compound to the second amino group-containing organic compound is preferably 1: (500-20), more preferably 1: (300-20), and more preferably 1: (277-23); the mass volume ratio of the second amino group-containing organic compound to water is preferably (0.1-1) g: 1ml, more preferably (0.2 to 0.8) g: 1ml, more preferably (0.2 to 0.5) g: 1ml, more preferably (0.3 to 0.4) g: 1ml, most preferably 1 g: 3 ml; the mixing is preferably to complete dissolution; the power of the microwave heating is preferably 500-1000W, more preferably 600-900W, still more preferably 700-800W, and most preferably 750W; the reaction time of the microwave heating is preferably 3-5 min, and more preferably 3-4 min.
After the reaction is finished, the mixture is preferably ground into fine powder to obtain the carbon dot-based fluorescent powder.
The prepared carbon dot-based fluorescent powder can adjust the luminescent color of the carbon dot-based fluorescent powder by adjusting the mass ratio of the total mass of the first amino-containing organic compound and the second amino-containing organic compound to the mass of the organic acid; the carbon dot-based phosphor is preferably a blue light emitting carbon dot-based phosphor, a green light emitting carbon dot-based phosphor or a yellow light emitting carbon dot-based phosphor; when the mass ratio of the total mass of the first amino group-containing organic compound and the second amino group-containing organic compound to the organic acid is (1000 to 50): 1, preferably (1000 to 100): the carbon dot-based phosphor obtained in step 1 is a green light emitting carbon dot-based phosphor, and the ratio is 557.56: when 1, the green light emitting carbon dot-based fluorescent powder has the highest luminous intensity; as the carbon dot loading is increased, i.e., the proportion of the amino group-containing organic compound is further decreased, the composite emits light in a red shift, and the intensity of light emission decreases in a red shift, when the mass ratio of the total mass of the first amino group-containing organic compound and the second amino group-containing organic compound to the organic acid is decreased to 48.3:1, the obtained carbon dot-based fluorescent powder is yellow light emitting carbon dot-based fluorescent powder.
According to the invention, the carbon dots are formed by the organic acid and the first amino-containing organic compound in the first step, and the second amino-containing organic compound added in the second step forms graphite-phase carbon nitride, so that the carbon dots can be uniformly distributed in the second amino-containing organic compound solution on one hand, and the carbon dots are uniformly coated in the second amino-containing organic compound solution or bonded on the surface while the graphite-phase carbon nitride is formed, thereby preventing aggregation-induced fluorescence quenching of the carbon dots, realizing solid-state luminescence of the carbon dots, and having high luminous efficiency, and the luminous color of the carbon dot-based fluorescent powder can be adjusted by changing the content of the carbon dots on the other hand.
The invention also provides the carbon dot-based fluorescent powder prepared by the method, which is a compound of carbon dots and graphite-phase carbon nitride.
The invention also provides an LED which comprises the carbon dot-based fluorescent powder; the LED is preferably a WLED.
In the present invention, the LED is preferably prepared as follows: and dispersing the carbon dot-based fluorescent powder in the polydimethylsilane, and coating the dispersed carbon dot-based fluorescent powder on an indium gallium nitride blue LED chip to obtain the white LED taking the carbon dot-based fluorescent powder as a conversion layer.
The white light LED prepared by the invention has higher luminous efficiency than that of a white light LED using other carbon dot-based materials as conversion layers.
In order to further illustrate the present invention, the following will describe in detail a carbon dot-based phosphor, a preparation method thereof and an application thereof in conjunction with examples.
The reagents used in the following examples are all commercially available.
Example 1
The green luminous carbon dot-based fluorescent powder is prepared from citric acid and urea serving as raw materials by a two-step microwave method.
The preparation method of the green luminescent carbon dot-based fluorescent powder comprises the following steps:
s1, stirring 18 mg of citric acid and 36 mg of urea in 30ml of deionized water for a period of time until the citric acid and the urea are completely dissolved, and then transferring the solution into a 750W microwave reactor and heating for 3-4 minutes.
S2, 10g of urea is added into the solid in the S1, and the mixture is stirred in 30ml of deionized water for a period of time until the urea is completely dissolved. And then transferring the materials into a 750W microwave reactor and heating for 3-4 minutes to finally obtain a compound of carbon dots and graphite phase carbon nitride, and then grinding the powder to obtain the green luminous carbon dot-based fluorescent powder.
The carbon dot-based phosphor obtained in example 1 was analyzed by a fluorescence spectrophotometer to obtain an excitation and emission spectrum thereof, as shown in fig. 1. As can be seen from fig. 1, the excitation peak is around 400nm, and the excitation at 400nm has bright green light (λ 510 nm).
The carbon dot-based phosphor obtained in example 1 was analyzed by a scanning tunnel electron microscope to obtain a scanning tunnel electron micrograph, which is shown in fig. 2. Fig. 2 shows that the graphite phase carbon nitride is in a nanosheet layer.
The carbon dot-based phosphor obtained in example 1 was analyzed by a field emission transmission electron microscope to obtain a field emission transmission electron microscope photograph thereof, as shown in fig. 3. FIG. 3 shows that the particle size of the carbon dots is 2-8 nm and the lattice spacing is 0.21 nm.
The carbon dot-based phosphor obtained in example 1 was analyzed by X-ray diffraction, and its X-ray diffraction pattern was obtained as shown in fig. 4. From FIG. 4, it can be seen that the diffraction angle is 27.8 degrees.
The carbon dot-based phosphor obtained in example 1 was analyzed using a spectrofluorometer to obtain a three-dimensional fluorescence spectrum, as shown in fig. 5. FIG. 5 shows that the green emitting carbon dot-based phosphor has a luminescent center with an optimal emission at 510 nm.
The carbon dot-based phosphor obtained in example 1 was analyzed by a fluorescence microscope to obtain a microscopic fluorescence photograph thereof, as shown in fig. 6. FIG. 6 shows that the carbon dot-based phosphor emits light uniformly.
The fluorescence quantum efficiency of the carbon dot-based phosphor obtained in example 1 was measured by a fluorescence spectrophotometer, and a fluorescence quantum efficiency measurement result graph thereof was obtained as shown in fig. 7. FIG. 7 shows that the fluorescence quantum efficiency is as high as 62%.
Example 2
The yellow luminous carbon point-based fluorescent powder is obtained by mixing citric acid and urea in proportion.
The preparation method of the carbon dot-based fluorescent powder comprises the following steps:
s1, stirring 216 mg of citric acid and 432 mg of urea in 30ml of deionized water for a period of time until the citric acid and urea are completely dissolved, and then transferring the solution into a 750W microwave reactor and heating for 3-4 minutes.
S2, 10g of urea is added to the solid in S1, and the mixture is stirred in 30ml of deionized water for a period of time until the urea is completely dissolved. And then transferring the materials into a 750W microwave reactor and heating for 3-4 minutes to finally obtain a compound of carbon dots and graphite phase carbon nitride, and then grinding the powder to obtain the yellow luminous carbon dot-based fluorescent powder.
The carbon dot-based phosphor obtained in example 2 was analyzed by a fluorescence photometer to obtain a steady-state spectrum thereof, as shown in fig. 8. Fig. 8 shows that the phosphor emits yellow light (λ 530nm) under 365nm excitation.
Example 3
And mixing the carbon dot-based fluorescent powder prepared in the example 1 with dimethyl silane according to the mass ratio of 1:2, coating the mixture on a 450nm indium gallium nitride blue light LED chip with the coating thickness of 2mm, and drying to obtain the white light LED.
FIG. 9 shows a white LED photo and an emission spectrum during operation, wherein the emission peak is 540nm, the color temperature is 7557K, the luminous efficiency is 42lm/W, and the color coordinates (0.29,0.33) show that white light illumination can be realized by the white LED photo and the emission spectrum during operation, as shown in FIG. 9.
Example 4
The preparation method is as in example 1, the adding amount of urea in the step S2 is not changed, only the adding amount of citric acid and urea in the step S1 is changed, and the mass ratio of citric acid to urea in the step S1 is ensured to be 1:2, so that a series of carbon dot-based phosphors with different carbon dot contents are prepared.
Analyzing the carbon dot-based phosphor obtained in example 4 by using a fluorescence spectrophotometer to obtain a steady state spectrum of the phosphor under excitation of a light source with a wavelength of 360nm, as shown in fig. 10; and obtaining a photo under ultraviolet light, as shown in fig. 11, wherein from left to right in fig. 11, the mass ratio of urea to citric acid is 1000:1, 557.56:1, 280:1, 187: 1. 94.6: 1 and 48.3:1 carbon dot based phosphors.
Comparative example 1
The original solid luminescence quenched carbon nanodots are green light emitting carbon nanodots, and the preparation method thereof is the prior art, for example, see the chinese patent (application No.: CN201210312844.0), and mainly comprises the following steps:
dissolving 3g of citric acid and 6g of urea in 20ml of deionized water to obtain a transparent solution;
and (3) placing the obtained solution in a microwave oven, heating for 3-5 minutes by microwave with power of 750W, wherein the surface temperature of reactants can reach 255 ℃ after the reaction is finished, and obtaining a brownish black solid, namely the green fluorescent carbon dots.
The blue luminescent graphite-phase carbon nitride fluorescent powder is prepared by using urea as a raw material through a one-step microwave method.
The preparation method of the graphite phase carbon nitride fluorescent powder comprises the following steps:
stirring 10g of urea in 20ml of deionized water for a period of time until the urea is completely dissolved, transferring the solution into a 750W microwave reactor, and heating for 3-4 minutes to obtain graphite-phase carbon nitride. And grinding the powder to obtain the blue luminescent graphite-phase carbon nitride fluorescent powder.
The P-carbon dot-based fluorescent powder (carbon dot-based fluorescent powder obtained by stirring and physically adsorbing carbon dots and graphite-phase carbon nitride) is prepared by taking the carbon dots and the graphite-phase carbon nitride as raw materials and mechanically stirring the raw materials;
the preparation method of the carbon dot-based fluorescent powder is characterized by comprising the following steps of:
the prepared 10mg of green fluorescent carbon dots and the prepared 1g of graphite-phase carbon nitride were mixed and added to 30ml of deionized water and stirred for 2 hours, and then placed in a freeze-dryer for vacuum freeze-drying. And then grinding the powder to obtain the P-carbon dot-based fluorescent powder.
The absorption and emission spectra of the green fluorescent carbon dot solution obtained in comparative example 1 were measured by a fluorescence spectrophotometer, as shown in fig. 12. As can be seen from fig. 12, the absorption peak is around 400nm, and the excitation at 400nm shows bright green light (λ 550 nm).
The blue luminescent graphite-phase carbon nitride phosphor obtained in comparative example 1 was analyzed by a fluorescence spectrophotometer to obtain a steady-state spectrum thereof, as shown in fig. 13. Fig. 13 shows that the phosphor emits blue light when excited at 365nm (λ ═ 410 nm).
The green light-emitting carbon dot-based phosphor obtained in example 1 was recorded as an M-carbon dot-based phosphor, and fig. 14 shows a spectral comparison of a P-carbon dot-based phosphor and an M-carbon dot-based phosphor, indicating that the light-emitting intensity of the M-carbon dot-based phosphor is superior to that of the P-carbon dot-based phosphor.
Claims (9)
1. A preparation method of carbon dot-based fluorescent powder is characterized by comprising the following steps:
s1) mixing the first amino-containing organic compound with organic acid in water, and carrying out microwave heating for reaction to obtain an intermediate product;
s2) mixing the intermediate product with a second amino-containing organic compound in water, and carrying out microwave heating for reaction to obtain the carbon dot-based fluorescent powder.
2. The method according to claim 1, wherein the first and second amino group-containing organic compounds are each independently selected from one or more of urea, ammonium oxalate, tyrosine, glycine and ethylenediaminetetraacetic acid; the organic acid is selected from one or more of ascorbic acid, tartaric acid, malic acid and citric acid.
3. The production method according to claim 1, wherein the mass ratio of the total mass of the first amino group-containing organic compound and the second amino group-containing organic compound to the organic acid is (1000 to 40): 1.
4. the method according to claim 1, wherein the mass ratio of the first amino group-containing organic compound to the second amino group-containing organic compound is 1: (500-20).
5. The preparation method according to claim 1, wherein the microwave heating power in step S1) is 500 to 1000W; the reaction time is 3-5 min; the power of microwave heating in the step S2) is 500-1000W; the reaction time is 3-5 min.
6. The preparation method according to claim 1, wherein the mass-to-volume ratio of the organic acid to the water in the step S1) is (0.1-10) mg: 1 ml.
7. The method of claim 1, wherein the carbon dot-based phosphor is a blue-emitting carbon dot-based phosphor, a green-emitting carbon dot-based phosphor, or a yellow-emitting carbon dot-based phosphor.
8. The carbon dot-based phosphor of claim 1, wherein the carbon dot-based phosphor is a composite of carbon dots and graphite-phase carbon nitride.
9. An LED comprising the carbon dot-based phosphor according to any one of claims 1 to 7 or the carbon dot-based phosphor according to claim 8.
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| CN109825290A (en) * | 2019-03-29 | 2019-05-31 | 广西师范大学 | A kind of aggregation-induced emission type carbon quantum dot and preparation method thereof |
| US11760928B2 (en) * | 2021-07-06 | 2023-09-19 | Jiangnan University | Enhanced yellow-emitting carbon dots and its preparation method and application |
| CN117025216A (en) * | 2023-08-09 | 2023-11-10 | 陕西科技大学 | Multicolor carbon quantum dot-based fluorescent powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109825290A (en) * | 2019-03-29 | 2019-05-31 | 广西师范大学 | A kind of aggregation-induced emission type carbon quantum dot and preparation method thereof |
| US11760928B2 (en) * | 2021-07-06 | 2023-09-19 | Jiangnan University | Enhanced yellow-emitting carbon dots and its preparation method and application |
| CN117025216A (en) * | 2023-08-09 | 2023-11-10 | 陕西科技大学 | Multicolor carbon quantum dot-based fluorescent powder and preparation method thereof |
| CN117025216B (en) * | 2023-08-09 | 2024-03-22 | 陕西科技大学 | Multicolor carbon quantum dot-based fluorescent powder and preparation method thereof |
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