CN111019649A - Carbon quantum dot with ultrahigh fluorescence quantum yield, carbon quantum dot/PVA fluorescent film, and preparation method and application thereof - Google Patents
Carbon quantum dot with ultrahigh fluorescence quantum yield, carbon quantum dot/PVA fluorescent film, and preparation method and application thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 11
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 229910021642 ultra pure water Inorganic materials 0.000 claims description 13
- 239000012498 ultrapure water Substances 0.000 claims description 13
- 238000000502 dialysis Methods 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
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- 238000004806 packaging method and process Methods 0.000 abstract description 3
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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Abstract
The invention belongs to the technical field of luminescent materials, and particularly relates to a carbon quantum dot, a carbon quantum dot/PVA fluorescent film, and a preparation method and application thereof. The carbon quantum dot is prepared by taking rhodamine B as a carbon source. The preparation method of the carbon quantum dot with ultrahigh fluorescence quantum yield comprises the following steps: dissolving rhodamine B in the reaction solution, mixing, placing in a reaction kettle, reacting at 180-200 ℃ for 8-12 h, cooling to room temperature, and taking out the reactant; and adjusting the pH value of the reactant to be neutral, dialyzing, performing rotary evaporation, and freeze-drying to obtain the solid powder of the carbon quantum dots. The invention has the beneficial effects that: the carbon quantum dot with the ultrahigh fluorescence quantum yield is green light emitting, has good water dispersibility and ultrahigh fluorescence quantum yield, is 84.96-85.37% in water with the pH of 6.7, and is 95.84-96.55% when the pH is 9.0. The carbon quantum dot can be used for preparing environment-friendly packaging materials for packaging white light LEDs.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a carbon quantum dot, a carbon quantum dot/PVA fluorescent film, and a preparation method and application thereof.
Background
The carbon quantum dots are zero-dimensional carbon-based fluorescent materials with the particle size of less than 10nm, have the advantages of good water solubility, light stability, excellent biocompatibility, wide raw material source, low cost, environmental friendliness and the like, and have wide application prospects in the fields of analysis sensing, photocatalysis, solar cells, light-emitting diodes, fluorescence imaging and tracing, tumor targeting and treatment and the like. However, most of the carbon quantum dots synthesized at present are short wavelength emitting, and few of the carbon quantum dots emitting long wavelength have low quantum yield and poor water solubility.
The traditional materials for packaging the LED often contain heavy metal ions and rare earth elements, and the packaging materials are complex in preparation method, complex in operation, high in cost and capable of causing serious pollution to the environment; therefore, the preparation of a luminescent material with low cost, good luminescent performance and environmental friendliness is urgently needed to replace the traditional LED packaging material.
Therefore, based on the defects of the currently synthesized carbon quantum dots and the defects of the traditional encapsulated LED materials, it is necessary to synthesize an environment-friendly carbon quantum dot with good water solubility, long wavelength emission and high fluorescence quantum yield, and then prepare a solid luminescent phosphor or composite material from the carbon quantum dot to replace the traditional encapsulated materials of heavy metals or rare earth elements to prepare an environment-friendly white LED.
Disclosure of Invention
The invention provides a carbon quantum dot with ultrahigh fluorescence quantum yield, a carbon quantum dot/PVA fluorescent film, and a preparation method and application thereof, aiming at the defects in the background technology.
The first technical scheme adopted by the invention for solving the technical problems is as follows: the carbon quantum dot is prepared by taking rhodamine B as a carbon source.
The second technical scheme provided by the invention is as follows: a preparation method of carbon quantum dots with ultrahigh fluorescence quantum yield comprises the following steps:
dissolving rhodamine B in the reaction solution, mixing, placing in a reaction kettle, reacting at 180-200 ℃ for 8-12 h, cooling to room temperature, and taking out the reactant;
and adjusting the pH value of the reactant to be neutral, dialyzing, performing rotary evaporation, and freeze-drying to obtain the solid powder of the carbon quantum dots.
As a preferred mode of the present invention, the reaction solution is polyethylene glycol and an alkaline ultrapure aqueous solution; the mass/volume ratio of rhodamine B to the reaction solution is not more than 2.
Further preferably, the alkaline ultrapure water solution is a sodium hydroxide ultrapure water solution with the concentration of more than or equal to 0.67M.
Further preferably, the volume ratio of the polyethylene glycol to the alkaline ultrapure water solution is 1: 14-3: 12.
Further preferably, the polyethylene glycol is polyethylene glycol 400.
More preferably, the interception amount of the dialysis bag is 500-1000 Da, and the dialysis time is 48-96 h.
The invention also provides a carbon quantum dot/PVA fluorescent film, which is prepared by adopting the carbon quantum dot prepared by the method.
The invention also provides a preparation method of the carbon quantum dot/PVA fluorescent film, which comprises the following steps:
(1) preparing a solution with the concentration of 0.05mg/mL by using the carbon quantum dots, weighing 0.4-1.5 g of PVA, putting the PVA into a beaker, transferring 1mL of the carbon quantum dot solution into the beaker, and adding a solvent to a constant volume of 10 mL;
(2) heating the mixture to 90-110 ℃, and continuously stirring until PVA is completely dissolved to form a uniform compound solution;
(3) and pouring the compound solution onto a 75cm culture dish, and placing the culture dish in a drying oven at 40-60 ℃ until water is completely evaporated to obtain the carbon quantum dot/PVA fluorescent film.
Further preferably, in the step (1), the solvent is ultrapure water with a pH of 6.7 or a buffer solution with a pH of 7-12.
The invention also provides application of the carbon quantum dot/PVA fluorescent film, and the carbon quantum dot/PVA fluorescent film is used as an encapsulating material for encapsulating the white light LED.
The invention has the beneficial effects that: the carbon quantum dot with the ultrahigh fluorescence quantum yield, the synthesis method of the carbon quantum dot, the carbon quantum dot/PVA fluorescent film, the preparation method and the application of the carbon quantum dot/PVA fluorescent film have the advantages that the carbon quantum dot is green light emitting, has good water dispersibility, and is ultrahigh in absolute fluorescence quantum yield, 84.96-85.37% in an ultrapure water solution with the pH of 6.7, and 95.84-96.55% when the pH is 9.0. The environment-friendly carbon quantum dot/PVA fluorescent film is prepared based on the carbon quantum dot, the PVA fluorescent film prepared by dissolving PVA by taking ultrapure water with pH of 6.7 as a solvent, and the absolute quantum yield is 72.81%. The buffer solution with the pH value of 9.0 is used as a solvent to dissolve the PVA to prepare the carbon quantum dot/PVA fluorescent film, and the absolute fluorescence quantum yield can reach 83.76%. And packaging the white light LED by using the carbon quantum dot/PVA fluorescent film as a packaging material.
Drawings
FIG. 1 is a TEM image of ultra-high fluorescence quantum yield carbon quantum dots prepared in example 1;
FIG. 2 is a UV-Vis spectrum of ultra-high fluorescence quantum yield carbon quantum dots prepared in example 1;
FIG. 3 is an XRD pattern of ultra-high fluorescence quantum yield carbon quantum dots prepared in example 1;
FIG. 4 is an infrared spectrum of ultra-high fluorescence quantum yield carbon quantum dots prepared in example 1;
FIG. 5 is a fluorescence spectrum of a carbon quantum dot with ultra-high fluorescence quantum yield prepared in example 1;
FIG. 6 is a diagram of a carbon quantum dot/PVA fluorescent film prepared in example 2;
FIG. 7 is a fluorescence spectrum of the carbon quantum dot/PVA fluorescent film prepared in example 2;
FIG. 8 is a spectrum of an LED encapsulated by the carbon quantum dot/PVA fluorescent film prepared in example 2;
fig. 9 is a chromaticity coordinate diagram of a packaged LED of example 2.
Detailed Description
In order to facilitate an understanding of the invention, the invention is described in more detail below with reference to the accompanying drawings and specific examples. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
(1) firstly, 1mL of prepared 10M sodium hydroxide solution and 1mL of polyethylene glycol 400 are transferred, the mixed solution is subjected to constant volume to 15mL by using ultrapure water, then 30mg of rhodamine B is weighed and dissolved in the mixed solution, the mixed solution is transferred to a polytetrafluoroethylene reaction kettle after being uniformly stirred, the polytetrafluoroethylene reaction kettle is placed in an oven, and the reaction is continued for 12 hours after the heating to 180 ℃.
(2) Cooling to room temperature, pouring out the solution in the reaction kettle, adjusting the solution to be neutral by using hydrochloric acid, subpackaging the solution into dialysis bags of 1000Da, and dialyzing for 72h by using water frequently to remove impurities.
(3) And (3) collecting the solution after dialysis, performing rotary evaporation concentration at 65 ℃, and then performing freeze drying to obtain the carbon quantum dots with ultrahigh fluorescence quantum yield. The absolute fluorescence quantum yield of the carbon quantum dot in water is 85.19%, and the absolute fluorescence quantum yield is 96.12% when the pH value is 9.0.
The carbon quantum dots synthesized by the method of this example are characterized as follows:
(1) the synthesized carbon quantum dots were first subjected to transmission electron microscopy scanning, and the results are shown in fig. 1.
As can be seen from FIG. 1, the carbon quantum dots prepared in this example have good dispersibility in water, and the morphology is spheroidal.
In order to obtain the particle size of the carbon quantum dots, the particle size of the carbon quantum dots prepared in the embodiment is 1-2.8 nm and the average particle size is 1.96nm by statistically calculating 150 prepared carbon quantum dots.
(2) The carbon quantum dots prepared in this example were prepared as solutions of a certain concentration, and the ultraviolet-visible spectrum was scanned, and the results are shown in fig. 2.
As can be seen from FIG. 2, the carbon quantum dot prepared in this example has an absorption peak at 240nm in the ultraviolet region, which is caused by pi-pi transition of C-C, C-N bonds contained in the carbon quantum dot. Has a strong absorption peak at 491nm in a visible light region, belongs to sp2Caused by a conjugated structure. The carbon quantum dots prepared in the embodiment emit strong green fluorescence under the excitation of 365nm ultraviolet light.
(3) The carbon quantum dots prepared in this example were subjected to X-ray polycrystalline diffraction scanning, and the results are shown in fig. 3.
As can be seen from fig. 3, the carbon quantum dot prepared in this example has a distinct characteristic peak at 2 θ =23.7 °, which indicates that the carbon quantum dot prepared in this example is an amorphous structure, similar to the (002) plane of graphene.
(4) The infrared spectrum characterization of the synthesized carbon quantum dots is carried out, and the result is shown in figure 4.
As can be seen from FIG. 4, the carbon quantum dot prepared in this example is 3500-3050 cm-1Has strong peak, which indicates that the carbon quantum dot has more O-H bonds and is 1750--1Has a peak, belongs to the stretching vibration of C = C and C = N, and is at 1450--1The characteristic peak of (A) belongs to the stretching vibration of an aromatic ring framework.
(5) The prepared carbon quantum dots were prepared into a solution with water, and the fluorescence spectrum was scanned, with the results shown in fig. 5.
As can be seen from FIG. 5, the carbon quantum dot prepared by the present example has an emission peak wavelength of about 520nm, no excitation dependency, green emission, fluorescence intensity, and an absolute fluorescence quantum yield of 85.19%.
(1) firstly, 1mL of prepared 10M sodium hydroxide solution and 1mL of polyethylene glycol 400 are transferred, the mixed solution is subjected to constant volume to 15mL by using ultrapure water, then 28mg of rhodamine B is weighed and dissolved in the mixed solution, the mixed solution is transferred to a polytetrafluoroethylene reaction kettle after being uniformly stirred, the polytetrafluoroethylene reaction kettle is placed in an oven, and the reaction is continued for 8 hours after the heating to 200 ℃.
(2) Cooling to room temperature, pouring out the solution in the reaction kettle, adjusting the solution to be neutral by using hydrochloric acid, subpackaging the solution into 800Da dialysis bags, and dialyzing for 92h by using water in a common way to remove impurities.
(3) And (3) collecting the solution after dialysis, performing rotary evaporation concentration at 65 ℃, and then performing freeze drying to prepare the carbon quantum dots with high fluorescence quantum yield. The absolute fluorescence quantum yield of the carbon quantum dots in water was 85.37%. The absolute fluorescence quantum yield was 95.84% at pH 9.0.
(1) firstly, 1mL of prepared 10M sodium hydroxide solution and 1mL of polyethylene glycol 400 are transferred, the mixed solution is subjected to constant volume to 14mL by using ultrapure water, then 20mg of rhodamine B is weighed and dissolved in the mixed solution, the mixed solution is transferred to a polytetrafluoroethylene reaction kettle after being uniformly stirred, the polytetrafluoroethylene reaction kettle is placed in an oven, and the reaction is continued for 10 hours after the temperature is 190 ℃.
(2) Cooling to room temperature, pouring out the solution in the reaction kettle, adjusting the solution to be neutral by using hydrochloric acid, subpackaging the solution into 900Da dialysis bags, and dialyzing for 80h by changing water to remove impurities.
(3) And (3) collecting the solution after dialysis, performing rotary evaporation concentration at 65 ℃, and then performing freeze drying to prepare the carbon quantum dots with high fluorescence quantum yield. The absolute fluorescence quantum yield of the carbon quantum dots in water was 84.96%. The absolute fluorescence quantum yield was 96.55% at pH 9.0.
Example 4 this example provides carbon quantum dots prepared by the method of the present invention for use in the preparation of carbon quantum dot/PVA fluorescent films.
(1) The carbon quantum dot prepared in example 1 was prepared into a solution having a concentration of 0.05mg/mL, 0.5g of PVA was weighed and placed in a beaker, 1mL of the carbon quantum dot solution was transferred to the beaker, and then ultrapure water having a pH of 6.7 was added to the beaker to bring the volume to 10 mL.
(2) The mixture was placed on an electric heating mantle, heated to 90 ℃ and stirred continuously until the PVA was completely dissolved to form a homogeneous complex solution.
(3) And pouring the compound solution into a 75cm culture dish, and placing the culture dish in a drying oven at 40 ℃ until the water is completely evaporated to obtain the carbon quantum dot/PVA fluorescent film. The absolute fluorescence quantum yield of the carbon quantum dot/PVA fluorescent film is 72.81%.
Example 5 this example provides carbon quantum dots prepared by the method of the present invention for use in the preparation of carbon quantum dot/PVA fluorescent films.
(1) The carbon quantum dot prepared in example 1 was prepared into a solution with a concentration of 0.05mg/mL, 0.5g of PVA was weighed into a beaker, 1mL of the carbon quantum dot solution was transferred into the beaker, and a buffer solution with a pH of 9.0 was added to the beaker to bring the volume to 10 mL.
(2) The mixture was placed on an electric heating mantle, heated to 90 ℃ and stirred continuously until the PVA was completely dissolved to form a homogeneous complex solution.
(3) And pouring the compound solution into a 75cm culture dish, and placing the culture dish in a drying oven at 40 ℃ until the water is completely evaporated to obtain the carbon quantum dot/PVA fluorescent film. The absolute fluorescence quantum yield of the carbon quantum dot/PVA fluorescent film is 83.76%.
Example application of six-carbon Quantum dot/PVA fluorescent film
1. A picture of carbon quantum dots/PVA phosphor film under UV lamp illumination, the results are shown in FIG. 6.
As can be seen from FIG. 6, the synthesized carbon quantum dot/PVA fluorescent film still has strong green emission under the irradiation of a 365nm ultraviolet lamp, and the carbon quantum dot loaded in the PVA film is ensured to have unchanged property.
2. The synthesized carbon quantum dot/PVA fluorescent film was scanned for fluorescence spectrum, and the result is shown in FIG. 7.
As can be seen from FIG. 7, the carbon quantum dot/PVA fluorescent film has a maximum excitation wavelength of 480nm and an emission wavelength of 527nm, is green light, and has a strong fluorescence intensity with an absolute quantum yield of 72.81%.
3. The synthesized carbon quantum dot/PVA fluorescent film is coated on a blue LED lamp wick and packaged into a white LED, and the spectrum of the LED is scanned, and the result is shown in figure 8.
As can be seen from fig. 8, the spectrum of the white LED packaged mainly consists of a blue light wick and a carbon quantum dot/PVA film emitted by green light, and under the excitation of the blue light, the carbon quantum dot/PVA film emits the strongest green fluorescence, which is complementary to the blue light source to emit white light.
4. The spectral data of the white light LED is derived, and chromaticity coordinates are calculated, as shown in fig. 9. As can be seen from fig. 9, the chromaticity coordinates of the encapsulated white light LED are (0.3148, 0.3242), and the color temperature of the white light LED encapsulated by the carbon quantum dot/PVA fluorescent film prepared by the method of the present invention is 6406.78K, which is a cold white light.
Claims (11)
1. A carbon quantum dot with ultrahigh fluorescence quantum yield is characterized in that: the carbon quantum dot is prepared by taking rhodamine B as a carbon source.
2. The method for preparing the ultra-high fluorescence quantum yield carbon quantum dot according to claim 1, comprising:
dissolving rhodamine B in the reaction solution, mixing, placing in a reaction kettle, reacting at 180-200 ℃ for 8-12 h, cooling to room temperature, and taking out the reactant;
and adjusting the pH value of the reactant to be neutral, dialyzing, performing rotary evaporation, and freeze-drying to obtain the solid powder of the carbon quantum dots.
3. The method for preparing carbon quantum dots with ultrahigh fluorescence quantum yield according to claim 2, wherein the reaction solution is polyethylene glycol and an alkaline ultrapure water solution; the mass/volume ratio of the rhodamine B to the reaction solution is not more than 2.
4. The method for preparing carbon quantum dots with ultrahigh fluorescence quantum yield according to claim 3, wherein the volume ratio of the polyethylene glycol to the alkaline ultrapure water solution is 1: 14-3: 12.
5. The method for preparing carbon quantum dots with ultrahigh fluorescence quantum yield according to claim 3, wherein the alkaline ultrapure aqueous solution is sodium hydroxide ultrapure aqueous solution with concentration of not less than 0.67M.
6. The method for preparing carbon quantum dots with ultrahigh fluorescence quantum yield according to claim 3, wherein the polyethylene glycol is polyethylene glycol 400.
7. The method for preparing carbon quantum dots with ultrahigh fluorescence quantum yield according to claim 2, wherein the cut-off volume of the dialysis bag is 500-1000 Da, and the dialysis time is 48-96 h.
8. A carbon quantum dot/PVA fluorescent film, characterized in that it is prepared by using the carbon quantum dot prepared by the method of any one of claims 2 to 7.
9. The method for preparing a carbon quantum dot/PVA fluorescent film according to claim 8, comprising:
(1) preparing a solution with the concentration of 0.05mg/mL by using the carbon quantum dots, weighing 0.4-1.5 g of PVA, putting the PVA into a beaker, transferring 1mL of the carbon quantum dot solution into the beaker, and adding a solvent to a constant volume of 10 mL;
(2) heating the mixture to 90-110 ℃, and continuously stirring until PVA is completely dissolved to form a uniform compound solution;
(3) and pouring the compound solution onto a 75cm culture dish, and placing the culture dish in a drying oven at 40-60 ℃ until water is completely evaporated to obtain the carbon quantum dot/PVA fluorescent film.
10. The method for preparing a carbon quantum dot/PVA fluorescent film according to claim 9, wherein in the step (1), the solvent is ultrapure water having a pH of 6.7 or a buffer solution having a pH of 7 to 12.
11. The application of the carbon quantum dot/PVA fluorescent film prepared by the method as claimed in claim 9, wherein the carbon quantum dot/PVA fluorescent film is used as an encapsulating material for encapsulating white light LEDs.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111808602A (en) * | 2020-06-12 | 2020-10-23 | 苏州星烁纳米科技有限公司 | Carbon quantum dot, method for synthesizing same, thin film, and electronic device |
| CN112961669A (en) * | 2021-02-01 | 2021-06-15 | 苏州星烁纳米科技有限公司 | Preparation method of solid-phase carbon quantum dot, solid-phase carbon quantum dot prepared by same and light-emitting device |
| CN113265114A (en) * | 2021-04-30 | 2021-08-17 | 上海大学 | Preparation method of carbon quantum dot-based blue light filtering film |
| CN116948640A (en) * | 2023-07-27 | 2023-10-27 | 云南大学 | Method for preparing green light carbon quantum dots with ultrahigh fluorescence quantum yield by one-step hydrothermal method and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528691A (en) * | 2015-01-22 | 2015-04-22 | 广西师范学院 | Method for synthesizing high-quantum-yield fluorescent carbon point |
| CN104592993A (en) * | 2015-01-22 | 2015-05-06 | 电子科技大学 | Preparation method of carbon quantum dot and application thereof |
| CN106701069A (en) * | 2016-11-22 | 2017-05-24 | 福州大学 | Preparation method of wavelength-controllable long wavelength emitting fluorescent carbon-based nanodots |
| CN107841307A (en) * | 2016-08-04 | 2018-03-27 | 南京工业大学 | A kind of large-scale preparation method of fluorescent carbon quantum dot |
| CN109233821A (en) * | 2018-11-05 | 2019-01-18 | 华南师范大学 | A kind of multicolor luminous carbon quantum dot and the preparation method and application thereof |
| CN109913211A (en) * | 2019-04-08 | 2019-06-21 | 东北林业大学 | Carbon quantum dot and preparation method thereof, membrane material of carbon containing quantum dot and its preparation method and application |
-
2019
- 2019-12-12 CN CN201911271586.4A patent/CN111019649B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528691A (en) * | 2015-01-22 | 2015-04-22 | 广西师范学院 | Method for synthesizing high-quantum-yield fluorescent carbon point |
| CN104592993A (en) * | 2015-01-22 | 2015-05-06 | 电子科技大学 | Preparation method of carbon quantum dot and application thereof |
| CN107841307A (en) * | 2016-08-04 | 2018-03-27 | 南京工业大学 | A kind of large-scale preparation method of fluorescent carbon quantum dot |
| CN106701069A (en) * | 2016-11-22 | 2017-05-24 | 福州大学 | Preparation method of wavelength-controllable long wavelength emitting fluorescent carbon-based nanodots |
| CN109233821A (en) * | 2018-11-05 | 2019-01-18 | 华南师范大学 | A kind of multicolor luminous carbon quantum dot and the preparation method and application thereof |
| CN109913211A (en) * | 2019-04-08 | 2019-06-21 | 东北林业大学 | Carbon quantum dot and preparation method thereof, membrane material of carbon containing quantum dot and its preparation method and application |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111808602A (en) * | 2020-06-12 | 2020-10-23 | 苏州星烁纳米科技有限公司 | Carbon quantum dot, method for synthesizing same, thin film, and electronic device |
| WO2021248830A1 (en) * | 2020-06-12 | 2021-12-16 | 苏州星烁纳米科技有限公司 | Carbon quantum dot and synthesis method therefor, thin film and electronic device |
| CN111808602B (en) * | 2020-06-12 | 2024-01-02 | 苏州星烁纳米科技有限公司 | Carbon quantum dot, synthesis method thereof, film and electronic equipment |
| CN112961669A (en) * | 2021-02-01 | 2021-06-15 | 苏州星烁纳米科技有限公司 | Preparation method of solid-phase carbon quantum dot, solid-phase carbon quantum dot prepared by same and light-emitting device |
| CN113265114A (en) * | 2021-04-30 | 2021-08-17 | 上海大学 | Preparation method of carbon quantum dot-based blue light filtering film |
| CN116948640A (en) * | 2023-07-27 | 2023-10-27 | 云南大学 | Method for preparing green light carbon quantum dots with ultrahigh fluorescence quantum yield by one-step hydrothermal method and application |
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