CN113201331B - Dual-mode excited room temperature phosphorescent carbon dot - Google Patents
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Abstract
The invention discloses a dual-mode excited room-temperature phosphorescent carbon dot, which is prepared by forming a reaction system by using acrylic acid as a carbon source, ammonium oxalate as a nitrogen source and water as a solvent through a hydrothermal synthesis reaction. The invention does not need matrix, can generate the phosphorescence property through self-crosslinking in the synthesis process, has the ultraviolet and visible light double-mode excitation property, greatly strengthens the information protection function, and has great potential application prospect in the aspect of safety protection.
Description
Technical Field
The invention relates to the technical field of phosphorescent material production, in particular to a dual-mode excited room-temperature phosphorescent carbon dot.
Background
Room temperature phosphorescent materials have significant advantages over fluorescent materials, such as longer stokes shift and longer lifetime. Up to now, there are room temperature phosphorescent materials such as organometallic complexes, metal-free pure organic compounds, carbon dots, and the like. Among the room temperature phosphorescent materials, the carbon dots have the remarkable advantages of simple preparation, relatively low manufacturing cost, low toxicity, high luminous efficiency and the like.
Room temperature phosphorescent carbon dot-based materials are typically prepared by embedding carbon dots in a suitable matrix such as boric acid, polyvinyl alcohol, melamine, urea/biuret, amorphous silica and inorganic materials that provide strong rigid, dense hydrogen bonding sites to stabilize their triplet states and prevent their triplet quenching.
For example, ZHao et al (Y. Deng, D. ZHao, X. Chen, F. Wang, H. Song, D. Shen,Chem. Commun. 2013, 495751.) a room temperature phosphorescent material for carbon dots was first created by incorporating the polymer polyvinyl alcohol as a protective matrix and successfully used to protect documents.
Li et al (Li, Q.; zhou, M.; yang, Q.; wu, Q.; shi, J.; gong, A.; yang, M.chem. Mater. 2016, 28, 8221-8227.) report that nitrogen-doped CDs exhibit room temperature phosphorescence in the data encryption field after mixing with a matrix.
Lu et al (L.Q. Bai, N. Xue, X.R. Wang, W.Y. Shi and C. Lu, nanoscale, 2017, 9, 6658-6664.) embed carbon dots in Layered Double Hydroxides (LDHs) to obtain a carbon dot composite with a phosphorescent lifetime of 0.387 s.
Many room temperature phosphorescent carbon dot-based materials currently require a proper solid matrix or the introduction of heavy atoms to promote the cross-linking between systems and inhibit the vibration dissipation between singlet and triplet states, resulting in phosphorescent properties. Carbon dots, which are inherently non-phosphorescent, require the reliance on a substrate to produce phosphorescent properties, and have certain limitations.
The carbon dots can generate phosphorescence by themselves due to certain properties, and although the carbon dots are separated from the matrix, the phosphorescence can be generated only under the excitation of ultraviolet light, and the excitation spectrum of the carbon dots in the ultraviolet light region is not favorable for certain applications. Visible light is ubiquitous and safer than ultraviolet light. In contrast to ultraviolet light, visible light is safer to use and allows for deeper bioanalysis and imaging; and thus is easy to use in practical applications. However, the synthesis of room temperature phosphorescent carbon dots by excitation with visible light is a great challenge. Designing and fabricating room temperature phosphorescent carbon dots with matrix-free, dual-mode (uv, visible) excitation properties is therefore a great challenge.
Disclosure of Invention
The invention aims to provide a room-temperature phosphorescent carbon dot excited in a dual mode, which does not need a matrix, can generate a phosphorescent property through self-crosslinking in a synthesis process, has an ultraviolet and visible light dual-mode excitation property, greatly enhances the function of information protection, and has a great potential application prospect in the aspect of safety protection.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the room-temperature phosphorescence carbon dot excited by double modes is prepared by forming a reaction system by taking acrylic acid as a carbon source, ammonium oxalate as a nitrogen source and water as a solvent through a hydrothermal synthesis reaction.
The room temperature phosphorescent carbon dot without the matrix and with the dual-mode excitation property shows room temperature phosphorescent characteristics under the excitation of ultraviolet light, and can also show room temperature phosphorescent characteristics under the excitation of visible light. The development way of the visible light excited room temperature phosphorescent material and the application thereof is widened.
Through research, the invention discovers that matrix-free and dual-mode (ultraviolet and visible light) excitation can be realized by combining specific molecular precursor acrylic acid and ammonium oxalate. The room temperature phosphorescent carbon dots with the double-mode (ultraviolet and visible light) excitation property and without the matrix are synthesized, and the method has a great potential application prospect in the aspect of safety protection.
The room temperature phosphorescent carbon dots synthesized by the method have the advantages that the room temperature phosphorescent carbon dots without matrixes and with the dual-mode (ultraviolet and visible light) excitation property can be generated without matrixes through self-crosslinking in the synthesis process, and have the dual-mode ultraviolet and visible light excitation property, namely phosphorescence can be generated under the excitation of ultraviolet light and phosphorescence can be generated under the excitation of visible light, so that the information protection function is greatly enhanced, and the room temperature phosphorescent carbon dots have great potential application prospects in the aspect of safety protection.
Preferably, the content of the ammonium oxalate in the reaction system is 0.42-3.51 wt%.
Preferably, the volume ratio of the acrylic acid to the water is: v Acrylic acid ：V Water (W) =1～5：3~8。
Preferably, the reaction conditions of the hydrothermal synthesis reaction are as follows: reacting for 2-18 hours at 140-300 ℃.
Preferably, the preparation method comprises the following specific steps:
(1) Dissolving ammonium oxalate and acrylic acid in water, and fully stirring to obtain a mixed solution;
(2) Reacting the mixed solution obtained in the step (1) at 140-300 ℃ for 2-18 hours to obtain an initial solution;
(3) And (3) carrying out ultrasonic dissolution, filtration and centrifugation on the initial solution obtained in the step (2), taking supernatant, dialyzing, and freeze-drying to obtain the dual-mode excited room-temperature phosphorescent carbon dot.
Preferably, in step (3), the centrifugation parameters are: rotating speed of 4000-10000 rpm, and centrifuging for 5-30 minutes.
Preferably, the centrifugation parameters are: rotating speed is 6000-10000 r/min, and centrifuging is carried out for 10-15 min.
Preferably, in the step (3), the dialysis bag has a specification of 500Da to 3500Da, and the dialysis is carried out in ultrapure water for 12 to 96 hours.
Preferably, the dialysis bag has a specification of 500Da-3500Da, and is dialyzed in ultrapure water for 48-72 hours.
Preferably, in step (3), the freeze-drying is carried out for 12 to 96 hours. The freeze-drying is preferably carried out for 36 to 48 hours.
The invention has the advantages that:
1. the room temperature phosphorescent carbon dot with dual-mode excitation prepared by the invention adopts acrylic acid as a carbon source and ammonium oxalate as a nitrogen source, and is prepared by a hydrothermal synthesis method under the condition that a solvent is water.
2. The room temperature phosphorescent carbon dot with the dual-mode excitation, which is prepared by the invention, utilizes self-crosslinking of the carbon dot in the preparation process, promotes the conversion from a singlet state to a triplet state, and inhibits the consumption of the triplet state, so that the carbon dot prepared from acrylic acid and ammonium oxalate has a phosphorescent property.
3. The room-temperature phosphorescent carbon dot prepared by the invention has a dual-mode excitation, has a phosphorescent property, can generate green afterglow under the excitation of an ultraviolet lamp and visible light (such as a flashlight), has a phosphorescent service life of more than 410ms, and can be observed by naked eyes for more than 10 s.
4. The room temperature phosphorescent carbon dot with dual-mode excitation prepared by the invention has the fluorescence property, is a light yellow solid under sunlight, shows white emission under an ultraviolet lamp, and shows blue luminescence after being dissolved in water.
5. The room temperature phosphorescent carbon dot with the dual-mode excitation prepared by the invention does not need to introduce a proper solid matrix or introduce heavy atoms to promote the crossing between systems and inhibit the vibration dissipation between the singlet state and the triplet state, and the room temperature phosphorescence can be generated by utilizing the self-crosslinking capability of the room temperature phosphorescent carbon dot with the dual-mode excitation prepared by the invention.
Drawings
FIG. 1 is a photograph of bi-mode excited room temperature phosphorescent carbon dots prepared in accordance with the present invention under UV lamp (a) and off (b) conditions, respectively.
FIG. 2 is a photograph of a dual mode excited room temperature phosphorescent carbon dot prepared in accordance with the present invention under visible light (e.g., flashlight) excitation (a) and off (b) conditions.
FIG. 3 shows HRTEM spectra (a) and particle size distribution (b) of dual-mode excited room temperature phosphorescent carbon dots prepared according to the present invention.
FIG. 4 is an XRD pattern of a bimodal excited room temperature phosphorescent carbon dot prepared in accordance with the present invention.
FIG. 5 is an infrared spectrum of a bi-modal excited room temperature phosphorescent carbon dot prepared in accordance with the present invention.
FIG. 6 shows XPS spectra (a) and its high resolution C1s spectra (b), N1s spectra (C) and O1s spectra (d) of dual-mode excited room temperature phosphorescent carbon dots prepared in accordance with the present invention.
FIG. 7 shows the excitation spectrum of the room temperature phosphorescent carbon dot prepared by the present invention under dual-mode excitation and the fluorescence spectrum under the optimal excitation.
FIG. 8 is the phosphorescence spectrum of the room temperature phosphorescent carbon dot excited at 365nm prepared by the present invention.
FIG. 9 is a phosphorescence spectrum of a dual-mode excited room temperature phosphorescent carbon dot prepared in accordance with the present invention under flashlight excitation.
FIG. 10 is a graph showing the decay of the fluorescence lifetime of a bi-mode excited room temperature phosphorescent carbon dot prepared in accordance with the present invention.
FIG. 11 is a graph showing the decay of the phosphorescence lifetime of a bi-mode excited room temperature phosphorescent carbon dot prepared in accordance with the present invention.
FIG. 12 shows the phosphorescent projection effect of the fabricated dual-mode excited room temperature phosphorescent carbon dots.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
In the present invention, the raw materials and equipment used are commercially available or commonly used in the art, unless otherwise specified. The methods in the following examples are conventional in the art unless otherwise specified.
General implementation: the room-temperature phosphorescent carbon dot excited in a dual mode is prepared by forming a reaction system by taking acrylic acid as a carbon source, ammonium oxalate as a nitrogen source and water as a solvent through a hydrothermal synthesis reaction. The content of the ammonium oxalate in the reaction system is 0.42 to 3.51 percent by weight. The volume ratio of the acrylic acid to the water is as follows: v Acrylic Acid (AA) ：V Water (W) =1 to 5:3 to 8. The reaction conditions of the hydrothermal synthesis reaction are as follows: reacting for 2-18 hours at 140-300 ℃.
The preparation method comprises the following specific steps:
(1) Dissolving ammonium oxalate and acrylic acid in water, and fully stirring to obtain a mixed solution;
(2) Reacting the mixed solution obtained in the step (1) at the temperature of 140-300 ℃ for 2-18 hours to obtain an initial solution;
(3) And (3) carrying out ultrasonic dissolution, filtration and centrifugation on the initial solution obtained in the step (2), taking supernatant, dialyzing, and freeze-drying to obtain the dual-mode excited room-temperature phosphorescent carbon dots.
The centrifugation parameters are as follows: the rotating speed is 4000 to 10000 r/min, and the centrifugation is 5 to 30 minutes. The centrifugation parameters are preferably: rotating speed is 6000-10000 r/min, and centrifuging is carried out for 10-15 min. The specification of the dialysis bag is 500Da to 3500Da, and the dialysis is carried out in ultrapure water for 12 to 96 hours. Dialysis in ultrapure water is preferably carried out for 48 to 72 hours. Freeze drying for 12-96 hr.
Example 1
This example 1 provides a method for preparing a dual-mode excited room temperature phosphorescent carbon dot, which includes the following steps:
(1) Dissolving 0.1g of ammonium oxalate and 1.5mL of acrylic acid in 6mL of distilled water to obtain a mixed solution;
(2) Placing the mixed solution obtained in the step (1) in a 25mL polytetrafluoroethylene high-pressure reaction kettle, and heating at 140 ℃ for 12 hours to obtain an initial solution of carbon dots;
(3) And (3) adding 10mL of distilled water into the initial solution obtained in the step (2), carrying out ultrasonic treatment for 15 minutes, filtering the solution, removing insoluble substances, centrifuging the obtained solution at the rotating speed of 6000 r/min for 15 minutes, washing with water for 3 times, taking the upper layer solution, dialyzing the upper layer solution for 48 hours, and carrying out freeze drying for 36 hours to obtain the dual-mode excited room-temperature phosphorescent carbon dot.
Example 2
This example 2 provides a method for preparing a room temperature phosphorescent carbon dot with a dual-mode excitation property, which includes the following steps:
(1) Dissolving 0.15g of ammonium oxalate and 3mL of acrylic acid in 9mL of distilled water to obtain a mixed solution;
(2) Placing the mixed solution obtained in the step (1) in a 25mL polytetrafluoroethylene high-pressure reaction kettle, and heating at 160 ℃ for 10 hours to obtain an initial solution of carbon dots;
and (3) adding 10mL of distilled water into the initial solution obtained in the step (2), carrying out ultrasonic treatment for 15 minutes, filtering the solution, removing insoluble substances, centrifuging the obtained solution at the rotating speed of 6000 rpm for 15 minutes, washing with water for 3 times, taking the upper layer solution, dialyzing the upper layer solution for 48 hours, and carrying out freeze drying for 36 hours to obtain the room-temperature phosphorescent carbon dot powder with the dual-mode excitation property.
Example 3
The embodiment provides a preparation method of a room temperature phosphorescent carbon dot with a dual-mode excitation property, which comprises the following steps of:
(1) Dissolving 0.12g of ammonium oxalate and 2.4mL of acrylic acid in 7.5mL of distilled water to obtain a mixed solution;
(2) Placing the mixed solution obtained in the step (1) in a 25mL polytetrafluoroethylene high-pressure reaction kettle, and heating for 8 hours at 180 ℃ to obtain an initial solution of carbon dots;
(3) And (3) adding 10mL of distilled water into the initial solution obtained in the step (2), carrying out ultrasonic treatment for 15 minutes, filtering the solution, removing insoluble substances, centrifuging the obtained solution at the rotation speed of 8000 rpm for 10 minutes, washing with water for 3 times, taking the upper solution, dialyzing the upper solution for 36 hours, and carrying out freeze drying for 36 hours to obtain the room-temperature phosphorescent carbon dot powder with the dual-mode excitation property.
Example 4
The embodiment provides a preparation method of a room temperature phosphorescent carbon dot with a dual-mode excitation property, which comprises the following steps:
(1) Dissolving 0.18g of ammonium oxalate and 4mL of acrylic acid in 10.5mL of distilled water to obtain a mixed solution;
(2) Placing the mixed solution obtained in the step (1) in a 25mL polytetrafluoroethylene high-pressure reaction kettle, and heating for 8 hours at 200 ℃ to obtain an initial solution of carbon dots;
(3) And (3) adding 10mL of distilled water into the initial solution obtained in the step (2), carrying out ultrasonic treatment for 15 minutes, filtering the solution, removing insoluble substances, centrifuging the obtained solution at the rotating speed of 6000 rpm for 15 minutes, washing with water for 3 times, taking the upper layer solution, dialyzing the upper layer solution for 36 hours, and carrying out freeze drying for 36 hours to obtain the room-temperature phosphorescent carbon dot powder with the dual-mode excitation property.
The room temperature phosphorescent carbon dot obtained by the invention has the following fluorescent and phosphorescent properties:
1. fluorescence properties:
(1) the room-temperature phosphorescent carbon dot excited by the dual-mode light source is a light yellow solid under sunlight and emits white fluorescence under the excitation of an ultraviolet lamp.
(2) The room-temperature phosphorescent carbon dots excited by the dual-mode are dissolved in ultrapure water and emit blue fluorescence under the excitation of an ultraviolet lamp.
And (3) phosphorescence property:
(1) the room-temperature phosphorescent carbon dot excited by the dual modes can emit green afterglow more than 10s to naked eyes under the excitation of an ultraviolet lamp, and the phosphorescent service life can reach more than 410 ms.
(2) The room-temperature phosphorescent carbon dot excited by the dual modes can emit green afterglow which can reach more than 10s to the naked eye under the excitation of visible light (such as a flashlight), and the phosphorescent service life can reach more than 410 ms.
FIG. 1 is a photograph of room temperature phosphorescent carbon dots of dual mode excitation nature prepared in example 1 under 365nm UV lamp illumination and after shut down. The photo shows that the room temperature phosphorescent carbon dots with the dual-mode excitation property prepared in the above way can emit white fluorescence under the irradiation of an ultraviolet lamp of 365 nm. After the ultraviolet lamp is turned off, the room temperature phosphorescent carbon dots with the dual-mode excitation property prepared above can still emit green phosphorescence.
FIG. 2 is a photograph of a room temperature phosphorescent carbon dot of dual mode excitation nature prepared in example 1 under visible light (e.g., a flashlight) and after shut down. The photographs show that the room temperature phosphorescent carbon dots with the dual-mode excitation property prepared above are light yellow solids under the irradiation of visible light (such as a flashlight). The room temperature phosphorescent carbon dots with dual-mode excitation property prepared above can still emit green phosphorescence after the visible light (such as a flashlight) is turned off.
FIG. 3 is a HRTEM image (a) and a particle size distribution (b) of a solution obtained by adding room temperature phosphorescent carbon dots of the dual mode excitation property prepared in example 1 to water. The morphology and the size of the prepared room-temperature phosphorescent carbon dots with the dual-mode excitation property are characterized by a high-resolution transmission electron microscope, an HRTEM image shows that the prepared room-temperature phosphorescent carbon dots with the dual-mode excitation property have obvious lattice stripes, and the average particle size of the room-temperature phosphorescent carbon dots with the dual-mode excitation property is 2.8nm according to a particle size distribution diagram.
Fig. 4 is an XRD spectrum of the room temperature phosphorescent carbon dot of the bimodal excitation property prepared in example 1, and it can be seen from the spectrum that the room temperature phosphorescent carbon dot of the bimodal excitation property prepared has a single peak at a 2 θ = 20.0 a and has a representative graphite structure.
FIG. 5 is a FT-IR spectrum of a room temperature phosphorescent carbon dot of dual mode excitation nature prepared in example 1. In the figure, 3270cm -1 The characteristic peak corresponds to the stretching vibration of O-H, 1760cm -1 Characteristic peak of (1) corresponding to C = O (from COOH) stretching vibration, 1440cm -1 The characteristic peak corresponds to C-N stretching vibration. It is known that functional groups such as-COOH and-OH exist on the surface of the prepared room-temperature phosphorescent carbon dot with the dual-mode excitation property, a large number of hydrogen bonds exist, the conversion from a singlet state to a triplet state is promoted, the consumption of the triplet state is inhibited, and the carbon dot prepared from acrylic acid and ammonium oxalate has the phosphorescent property.
Fig. 6 is an XPS spectrum of a room temperature phosphorescent carbon dot of the dual mode excitation property prepared in example 1. Fig. 6 (a) shows that the contents of C, N, and O elements in the room-temperature phosphorescent carbon dots having the dual-mode excitation property are 73.03%, 0.98%, and 25.99%, respectively. In the high-resolution C1s spectrum of fig. 6 (b), the three peak positions 284.63, 285.17 and 288.77eV correspond to C-C/C = C, COOH and C-N, respectively. From the high-resolution N1s spectrum of FIG. 6 (c), two peaks 400.18 and 401.57eV are present in the form of pyrrole N and graphite N, respectively. From the high-resolution O1s spectrum of fig. 6 (d), peaks at two peak positions 531.9 and 533.28eV correspond to C-OH and C = O, respectively. Wherein Raw represents: raw data line, fixed represents: fitting lines.
FIG. 7 shows the excitation spectrum of room temperature phosphorescent carbon dots with dual-mode excitation properties prepared in example 1 and the fluorescence spectrum under the optimal excitation. The room temperature phosphorescent carbon dot with the dual-mode excitation property prepared by the invention is dissolved in water for excitation, and the room temperature phosphorescent carbon dot with the dual-mode excitation property prepared by the invention is known to show blue emission in an emission wavelength range, and the optimal emission is 408nm.
FIG. 8 is the phosphorescence spectrum at 365nm excitation of the room temperature phosphorescent carbon dot of the dual mode excitation nature prepared in example 1. The room temperature phosphorescent carbon dot solid with the dual-mode excitation property prepared by the invention is excited by an excitation wavelength of 365nm, and the room temperature phosphorescent carbon dot with the dual-mode excitation property prepared by the invention is found to be green phosphorescence at 476nm and have afterglow phenomenon of more than 10s visible to naked eyes.
FIG. 9 shows the phosphorescence spectra of room temperature phosphorescent carbon dots of dual mode excitation nature prepared in example 1 under flashlight excitation. The room-temperature phosphorescent carbon dot solid with the dual-mode excitation property prepared by the invention is excited by a flashlight, and the room-temperature phosphorescent carbon dot with the dual-mode excitation property prepared by the invention is found to be green phosphorescence at 465nm and have afterglow over 10s visible to naked eyes.
FIG. 10 is a graph of the fluorescence lifetime of room temperature phosphorescent carbon dots with dual mode excitation properties prepared in example 1. The fluorescence lifetime of the room temperature phosphorescent carbon dot with the prepared dual-mode excitation property is 1.31ns calculated by a fluorescence attenuation curve and fitting data.
Fig. 11 is a phosphorescence lifetime map of a room temperature phosphorescent carbon dot of a dual mode excitation property prepared in example 1. The room temperature phosphorescent carbon dot phosphorescence lifetime of the prepared dual-mode excitation property is 412.03ms according to phosphorescence attenuation curve and fitting data calculation.
FIG. 12 shows the phosphorescent projection effect of room temperature phosphorescent carbon dots with dual mode excitation properties prepared in example 1. During the process of turning on and off the ultraviolet lamp, the sketch map can be clearly seen to be projected on the prepared room temperature phosphorescent carbon dot platform with the dual-mode excitation property.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. The dual-mode excited room-temperature phosphorescent carbon dot is characterized in that a reaction system is formed by taking acrylic acid as a carbon source, ammonium oxalate as a nitrogen source and water as a solvent, and the dual-mode excited room-temperature phosphorescent carbon dot is prepared by a hydrothermal synthesis reaction;
the content of ammonium oxalate in the reaction system is 0.42 to 3.51 percent by weight; the volume ratio of the acrylic acid to the water is as follows: v Acrylic acid ：V Water (I) =1～5：3~8。
2. The room temperature phosphorescent carbon dot excited in a dual-mode according to claim 1, wherein the reaction conditions of the hydrothermal synthesis reaction are as follows: reacting for 2-18 hours at 140-300 ℃.
3. The room temperature phosphorescent carbon dot with dual-mode excitation according to claim 1, which is prepared by the following steps:
(1) Dissolving ammonium oxalate and acrylic acid in water, and fully stirring to obtain a mixed solution;
(2) Reacting the mixed solution obtained in the step (1) at the temperature of 140-300 ℃ for 2-18 hours to obtain an initial solution;
(3) And (3) carrying out ultrasonic dissolution, filtration and centrifugation on the initial solution obtained in the step (2), taking supernatant, dialyzing, and freeze-drying to obtain the dual-mode excited room-temperature phosphorescent carbon dots.
4. A dual-mode excited room temperature phosphorescent carbon dot as claimed in claim 3, wherein in step (3), the centrifugal parameters are: the rotating speed is 4000 to 10000 r/min, and the centrifugation is 5 to 30 minutes.
5. A dual-mode excited room temperature phosphorescent carbon dot as claimed in claim 4, wherein the centrifugation parameters are: rotating speed is 6000-10000 r/min, and centrifuging is carried out for 10-15 min.
6. The dual-mode excited room temperature phosphorescent carbon dot as claimed in claim 3, wherein in the step (3), the dialysis bag has a specification of 500Da-3500Da, and is dialyzed in ultrapure water for 12-96 hours.
7. The dual-mode excited room temperature phosphorescent carbon dot as claimed in claim 6, wherein the dialysis bag has a specification of 500Da-3500Da, and is dialyzed in ultrapure water for 48-72 hours.
8. The dual-mode excited room temperature phosphorescent carbon dot as claimed in claim 1, wherein in the step (3), the mixture is freeze-dried for 12-96 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
| CN108128767A (en) * | 2018-01-03 | 2018-06-08 | 辽宁大学 | A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment |
| CN110205121A (en) * | 2019-05-24 | 2019-09-06 | 深圳大学 | Room temperature phosphorimetry carbon dots material and the preparation method and application thereof |
| CN111607394A (en) * | 2020-06-17 | 2020-09-01 | 太原理工大学 | Room temperature phosphorescent carbon dot compound and preparation method thereof |
| CN111704124A (en) * | 2020-07-24 | 2020-09-25 | 浙江工业大学 | Blue room-temperature phosphorescent carbon dot and preparation method thereof |
-
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- 2021-04-23 CN CN202110438883.4A patent/CN113201331B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
| CN108128767A (en) * | 2018-01-03 | 2018-06-08 | 辽宁大学 | A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment |
| CN110205121A (en) * | 2019-05-24 | 2019-09-06 | 深圳大学 | Room temperature phosphorimetry carbon dots material and the preparation method and application thereof |
| CN111607394A (en) * | 2020-06-17 | 2020-09-01 | 太原理工大学 | Room temperature phosphorescent carbon dot compound and preparation method thereof |
| CN111704124A (en) * | 2020-07-24 | 2020-09-25 | 浙江工业大学 | Blue room-temperature phosphorescent carbon dot and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Visible-Light-Excited Ultralong-Lifetime Room Temperature Phosphorescence Based on Nitrogen-Doped Carbon Dots for Double Anticounterfeiting;Yifang Gao et al，;《Adv. Optical Mater.》;20200212;第8卷;第1901557：1-7页 * |
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