CN113148988A - Preparation method of nitrogen atom doped graphene quantum dots - Google Patents
Preparation method of nitrogen atom doped graphene quantum dots Download PDFInfo
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- CN113148988A CN113148988A CN202110398317.5A CN202110398317A CN113148988A CN 113148988 A CN113148988 A CN 113148988A CN 202110398317 A CN202110398317 A CN 202110398317A CN 113148988 A CN113148988 A CN 113148988A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 29
- 125000004433 nitrogen atom Chemical group N* 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000002096 quantum dot Substances 0.000 claims abstract description 17
- 239000006260 foam Substances 0.000 claims abstract description 16
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 7
- 238000006862 quantum yield reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000012298 atmosphere Substances 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000000799 fluorescence microscopy Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The invention discloses a preparation method of nitrogen atom doped graphene quantum dots, which comprises the following steps: preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate as a precursor; placing the precursor in a double-electrode system taking 0.1-0.3 mol/L ammonia solution as electrolyte, wherein the current is 0.01A, the reaction time is 4-8 h, the precursor is used as a working electrode, and a platinum sheet is used as a counter electrode; and after the reaction is finished, filtering the reaction solution, and performing rotary evaporation to obtain the nitrogen atom doped graphene quantum dots. The nitrogen doping content of the graphene quantum dot prepared by the method is up to 18%, the high-content nitrogen doping can improve the chemical property and electron transport of the quantum dot, and in addition, the fluorescence quantum yield of the graphene quantum dot is up to 19.3%. The simple, green and economic synthesis method provides a new way for preparing the nitrogen atom-doped graphene quantum dots, and has wide application prospects in the aspects of biosensors, photocatalysis, supercapacitors and the like.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a preparation method of nitrogen atom doped graphene quantum dots.
Background
The graphene has excellent thermal conductivity, high carrier mobility, larger theoretical specific surface area and excellent mechanical properties, so that the graphene has wide application prospects in the fields of energy storage materials such as lithium ion batteries, super capacitors, lithium-sulfur batteries and the like. Although graphene shows quantum confinement effect as a zero-bandgap semiconductor with infinite exciton Bohr radius, the application of the zero-bandgap semiconductor in the fields of optics and optoelectronics is greatly limited due to the characteristic of the zero-bandgap. Through a great deal of research, researchers find that a novel carbon nanomaterial with good water solubility and a tunable band gap, namely Graphene Quantum Dots (GQDs), can be obtained after cutting two-dimensional graphene by using various synthesis methods, such as an electrochemical method, an acid oxidation method, a microwave method and the like.
Graphene Quantum Dots (GQDs) have high electron mobility, good chemical stability, and high biocompatibility, and thus are widely used in the fields of biology, medicine, energy, and the like. The unique quantum confinement effect and boundary effect make it have great potential in photoelectric devices and fluorescence imaging. The graphene quantum dots are doped, so that the performances of all aspects of the graphene quantum dots can be further improved. For example, the addition of nitrogen atoms helps to enhance the surface polarity of the graphene quantum dots, and may enhance the electrical conductivity thereof. However, how to prepare high-quality controllable graphene quantum dots with high fluorescence quantum yield is still a major issue of current research.
Disclosure of Invention
The invention aims to provide a preparation method of nitrogen atom doped graphene quantum dots, wherein nitrogen-doped carbon nanotubes/nitrogen-doped graphene three-dimensional hybrid materials with nickel foam as a substrate are used as precursors to obtain the nitrogen atom doped graphene quantum dots with high photoluminescence quantum yield.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of nitrogen atom doped graphene quantum dots comprises the following steps:
(1) preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate as a precursor;
(2) placing the precursor prepared in the step (1) in a double-electrode system with 0.1-0.3 mol/L ammonia solution as electrolyte, wherein the current is 0.01A, the reaction time is 4-8 h, the precursor is used as a working electrode, and a platinum sheet is used as a counter electrode;
(3) and after the reaction is finished, filtering the reaction solution, and performing rotary evaporation to obtain the nitrogen atom doped graphene quantum dots.
Preferably, the specific process of step (1) is as follows: nickel foam was mixed with melamine in a ratio of 1: 5, placing the quartz boat on the quartz boat after mixing, placing the quartz boat in a tube furnace, heating to 800 ℃ in a hydrogen atmosphere, maintaining the temperature at 800 ℃, annealing for 0.5h in a mixed gas atmosphere, and finally cooling to room temperature in an argon atmosphere, wherein the mixed gas comprises argon and hydrogen in a volume ratio of 5: 1.
Preferably, the voltage of the double-electrode system in the step (2) is 5-10V, and the distance between the working electrode and the counter electrode is 2-4 cm.
Preferably, the concentration of the ammonia solution in the step (2) is 0.2mol/L, the reaction time is 8h, and the area of the platinum sheet is 15mm2。
Preferably, the nickel foam is also washed and dried prior to mixing.
Preferably, the temperature of the tube furnace is increased to 600 ℃ according to a first temperature increasing rate, then is increased to 800 ℃ according to a second temperature increasing rate, the first temperature increasing rate is greater than the second temperature increasing rate, the first temperature increasing rate is 30 ℃/min, and the second temperature increasing rate is 20 ℃/min.
Preferably, when the temperature is raised to 800 ℃ in the hydrogen atmosphere, the flow rate of the hydrogen is 70 sccm; when annealing is carried out for 0.5h in the mixed gas atmosphere, the flow rate of the mixed gas is 60 sccm; when the temperature in the argon atmosphere is reduced to room temperature, the argon flow is 30 sccm.
The invention also provides the nitrogen atom-doped graphene quantum dot, the nitrogen doping amount of the obtained graphene quantum dot is 18%, the fluorescence quantum yield is 19.3%, the surface polarity and the conductivity of the graphene quantum dot are enhanced, and the graphene quantum dot can be applied to a micro supercapacitor.
The invention has the following beneficial effects:
(1) according to the invention, the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material with nickel foam as a substrate is used as a precursor, and reacts in a double-electrode system with ammonia solution as electrolyte to obtain the graphene quantum dots with high nitrogen doping amount (18%) and high fluorescence quantum yield (19.3%), so that the surface polarity and the conductivity of the graphene quantum dots are greatly enhanced, and the graphene quantum dots can be applied to a micro super capacitor.
(5) According to the method, the ammonia water is electrochemically sheared by controlling the concentration of the ammonia water, so that the nitrogen-doped graphene quantum dots are prepared, and the precursor has a unique three-dimensional structure, so that the graphene sheet layers are not easy to stack, the electrochemical shearing process and the stripping process of the nitrogen-doped graphene quantum dots are facilitated, the formation of the carbon quantum dots is effectively prevented, and the obtained nitrogen-doped graphene quantum dots have high purity.
Drawings
Fig. 1 is a TEM image of a nitrogen atom-doped graphene quantum dot prepared in example 2 of the present invention;
fig. 2 is a raman spectrum of the nitrogen atom-doped graphene quantum dot prepared in example 2 of the present invention, wherein D, G and 2D feature peaks are respectively located at 1340cm-1、1580cm-1And 2700cm-1The D peak represents a defect of the carbon atom crystal, and the G peak represents an in-plane stretching vibration of the carbon atom sp2 hybridization.
Detailed Description
In order to further understand the present invention, the following describes a method for preparing a nitrogen atom doped graphene quantum dot according to the present invention with reference to an embodiment.
The methods described in the following examples are conventional methods unless otherwise specified; the materials are commercially available, unless otherwise specified.
Example 1:
(1) preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material: cleaning and drying 2g of nickel foam, mixing the nickel foam with 2g of melamine, putting the mixture into a quartz boat, and placing the quartz boat in a central heating zone of a constant-temperature tube furnace; introducing 70sccm hydrogen under normal pressure, heating the tube furnace to 600 ℃ at 30 ℃/min, and heating the tube furnace to 800 ℃ at 20 ℃/min; keeping the temperature of the tubular furnace at 800 ℃, simultaneously introducing 50sccm argon gas, adjusting the hydrogen flow to 10sccm, annealing for 30min under the mixed gas atmosphere of argon gas and hydrogen gas, stopping introducing the hydrogen gas, and finally cooling the tubular furnace to room temperature under the argon gas atmosphere of 30sccm to obtain the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate, wherein the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material is used as a precursor.
(2) Preparing nitrogen atom doped graphene quantum dots: the prepared precursor is placed in a double-electrode system taking 0.1mol/L ammonia solution as electrolyte, the precursor is taken as a working electrode, and the area is 15mm2The method comprises the following steps of taking a platinum sheet as a counter electrode, setting the distance between the two electrodes to be 2cm, setting the current to be 0.01A, keeping the voltage to be 5-10V, reacting for 8 hours, filtering a reaction solution after the reaction is finished, and performing rotary evaporation to obtain the nitrogen atom doped graphene quantum dot.
Example 2:
(1) preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material: cleaning and drying 1g of nickel foam, mixing with 5g of melamine, putting into a quartz boat, and placing into a central heating zone of a constant-temperature tube furnace; introducing 70sccm hydrogen under normal pressure, heating the tube furnace to 600 ℃ at 30 ℃/min, and heating the tube furnace to 800 ℃ at 20 ℃/min; keeping the temperature of the tubular furnace at 800 ℃, simultaneously introducing 50sccm argon gas, adjusting the hydrogen flow to 10sccm, annealing for 30min under the mixed gas atmosphere of argon gas and hydrogen gas, stopping introducing the hydrogen gas, and finally cooling the tubular furnace to room temperature under the argon gas atmosphere of 30sccm to obtain the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate, wherein the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material is used as a precursor.
(2) Preparing nitrogen atom doped graphene quantum dots: the prepared precursor was placed in a two-electrode system with 0.2mol/L ammonia solution as electrolyte, beforeThe object is used as a working electrode and has an area of 15mm2The method comprises the following steps of taking a platinum sheet as a counter electrode, setting the distance between the two electrodes to be 2cm, setting the current to be 0.01A, keeping the voltage to be 5-10V, reacting for 8 hours, filtering a reaction solution after the reaction is finished, and performing rotary evaporation to obtain the graphene quantum dots with 18% of nitrogen doping amount and 19.3% of fluorescence quantum yield.
A TEM image of the prepared nitrogen atom doped graphene quantum dot, as shown in fig. 1; the raman spectrum of the prepared nitrogen atom doped graphene quantum dot is shown in fig. 2.
Example 3:
(1) preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material: cleaning and drying 1g of nickel foam, mixing with 3g of melamine, putting into a quartz boat, and placing into a central heating zone of a constant-temperature tube furnace; introducing 70sccm hydrogen under normal pressure, heating the tube furnace to 600 ℃ at 30 ℃/min, and heating the tube furnace to 800 ℃ at 20 ℃/min; keeping the temperature of the tubular furnace at 800 ℃, simultaneously introducing 50sccm argon gas, adjusting the hydrogen flow to 10sccm, annealing for 30min under the mixed gas atmosphere of argon gas and hydrogen gas, stopping introducing the hydrogen gas, and finally cooling the tubular furnace to room temperature under the argon gas atmosphere of 30sccm to obtain the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate, wherein the nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material is used as a precursor.
(2) Preparing nitrogen atom doped graphene quantum dots: the prepared precursor is placed in a double-electrode system taking 0.3mol/L ammonia solution as electrolyte, the precursor is taken as a working electrode, and the area is 15mm2The method comprises the following steps of taking a platinum sheet as a counter electrode, setting the distance between the two electrodes to be 4cm, setting the current to be 0.01A, keeping the voltage to be 5-10V, reacting for 4 hours, filtering a reaction solution after the reaction is finished, and performing rotary evaporation to obtain the nitrogen atom doped graphene quantum dot.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A preparation method of nitrogen atom doped graphene quantum dots is characterized by comprising the following steps:
(1) preparing a nitrogen-doped carbon nanotube/nitrogen-doped graphene three-dimensional hybrid material taking nickel foam as a substrate as a precursor;
(2) placing the precursor prepared in the step (1) in a double-electrode system with 0.1-0.3 mol/L ammonia solution as electrolyte, wherein the current is 0.01A, the reaction time is 4-8 h, the precursor is used as a working electrode, and a platinum sheet is used as a counter electrode;
(3) and after the reaction is finished, filtering the reaction solution, and performing rotary evaporation to obtain the nitrogen atom doped graphene quantum dots.
2. The preparation method according to claim 1, wherein the step (1) comprises the following specific steps: nickel foam was mixed with melamine in a ratio of 1: 5, placing the quartz boat on the quartz boat after mixing, placing the quartz boat in a tube furnace, heating to 800 ℃ in a hydrogen atmosphere, maintaining the temperature at 800 ℃, annealing for 0.5h in a mixed gas atmosphere, and finally cooling to room temperature in an argon atmosphere, wherein the mixed gas comprises argon and hydrogen in a volume ratio of 5: 1.
3. The method according to claim 1, wherein the voltage of the two-electrode system in step (2) is 5 to 10V, and the distance between the working electrode and the counter electrode is 2 to 4 cm.
4. The production method according to claim 1, wherein the ammonia solution in the step (2) has a concentration of 0.2mol/L, the reaction time is 8 hours, and the area of the platinum sheet is 15mm2。
5. The method of claim 2, wherein the nickel foam is further washed and dried prior to mixing.
6. The method of claim 2, wherein the tube furnace is heated to 600 ℃ at a first heating rate and then to 800 ℃ at a second heating rate, the first heating rate being greater than the second heating rate, the first heating rate being 30 ℃/min and the second heating rate being 20 ℃/min.
7. The production method according to claim 2, wherein the hydrogen gas is supplied at a flow rate of 70sccm when the temperature in the hydrogen atmosphere is raised to 800 ℃; when annealing is carried out for 0.5h in the mixed gas atmosphere, the flow rate of the mixed gas is 60 sccm; when the temperature in the argon atmosphere is reduced to room temperature, the argon flow is 30 sccm.
8. The nitrogen-atom-doped graphene quantum dot is obtained by the preparation method of the nitrogen-atom-doped graphene quantum dot according to any one of claims 1 to 4, wherein the nitrogen doping amount of the obtained graphene quantum dot is 18%, and the fluorescence quantum yield is 19.3%.
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| CN114751400A (en) * | 2022-05-23 | 2022-07-15 | 湖北工业大学 | Nitrogen and zinc co-doped graphene quantum dot, ratio type immunosensor, and preparation method and application thereof |
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| CN108037171A (en) * | 2017-12-26 | 2018-05-15 | 南京师范大学 | The preparation method and application of the nitrogen-doped graphene quantum dot of high dispersive in a kind of water phase |
| CN110015653A (en) * | 2019-04-23 | 2019-07-16 | 重庆文理学院 | A kind of preparation method of carbon nanotube foam |
| US20200381717A1 (en) * | 2017-12-18 | 2020-12-03 | Daegu Gyeongbuk Institute Of Science And Technology | Lto negative electrode material, having graphene quantum dot doped with nitrogen attached thereto, with excellent rate characteristics and no gas generation during long term charge and discharge |
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| US20200381717A1 (en) * | 2017-12-18 | 2020-12-03 | Daegu Gyeongbuk Institute Of Science And Technology | Lto negative electrode material, having graphene quantum dot doped with nitrogen attached thereto, with excellent rate characteristics and no gas generation during long term charge and discharge |
| CN108037171A (en) * | 2017-12-26 | 2018-05-15 | 南京师范大学 | The preparation method and application of the nitrogen-doped graphene quantum dot of high dispersive in a kind of water phase |
| CN110015653A (en) * | 2019-04-23 | 2019-07-16 | 重庆文理学院 | A kind of preparation method of carbon nanotube foam |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114751400A (en) * | 2022-05-23 | 2022-07-15 | 湖北工业大学 | Nitrogen and zinc co-doped graphene quantum dot, ratio type immunosensor, and preparation method and application thereof |
| CN114751400B (en) * | 2022-05-23 | 2023-08-25 | 湖北工业大学 | Nitrogen-zinc co-doped graphene quantum dot, ratio immunosensor and preparation method and application thereof |
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