CN104150473A - Chemical preparation method for nitrogen-doped graphene quantum dot - Google Patents
Chemical preparation method for nitrogen-doped graphene quantum dot Download PDFInfo
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- CN104150473A CN104150473A CN201410376809.4A CN201410376809A CN104150473A CN 104150473 A CN104150473 A CN 104150473A CN 201410376809 A CN201410376809 A CN 201410376809A CN 104150473 A CN104150473 A CN 104150473A
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Abstract
The invention relates to a chemical preparation method for a nitrogen-doped graphene quantum dot, belonging to the technical field of nano materials. The invention particularly relates to a preparation method for the nitrogen-doped graphene quantum dot. The method comprises the following steps: firstly, by taking graphite oxide as a carbon source and glycine as a nitrogen source, preparing a nitrogen-doped graphene sheet under a high-temperature annealing condition; then, cutting the deeply oxidized nitrogen-doped graphene sheet into an oxidized nitrogen-doped graphene nano sheet; preparing the nitrogen-doped-graphene quantum dot with super-strong blue fluorescence by way of a hydrothermal reaction. The synthetic method of the nitrogen-doped graphene quantum dot provided by the invention is simple in synthetic process, all raw materials are cheap and easy to get in the market, and the prepared nitrogen-doped graphene quantum dot is high in purity and yield, mono-dispersible and good in water solubility, has a very strong blue fluorescence performance and has a very good application prospect in the application fields of lithium batteries, micro supercapacitors, biological fluorescent labels, solar batteries and the like.
Description
Technical field
The preparation method who the present invention relates to a kind of nitrogen-doped graphene quantum dot (N-GQDS), belongs to technical field of nano material.
Background technology
Since the Geim of Univ Manchester UK in 2004 etc. find single-layer graphene, due to its unique good physicochemical property, Graphene all shows wide application prospect in research fields such as microelectronics, functional materials, chemical sensitisations.In recent years, graphene quantum dot is as a kind of novel quantum dot, because its unique performance has caused people's broad research interest.Compared with Graphene, graphene quantum dot shows stronger quantum confined effect and side effect, in addition, graphene quantum dot also shows low cytotoxicity, good is water-soluble, unreactiveness, the performances such as stable photoluminescence, make it have good application prospect at aspects such as photoelectric device, sensor, bio-imagings.
The preparation method of graphene quantum dot mainly contains from top to bottom and two large classes from bottom to top.Top-down method is mainly, by the method for physics or chemistry, the carbon materials such as large-sized Graphene, carbon nanotube, carbon nanofiber are cut into undersized graphene quantum dot, as hydrothermal method, acid oxidation, electrochemical method etc.; Method is from bottom to top mainly using small molecules as presoma, finally obtains graphene quantum dot by series of chemical.But, produce at present graphene quantum dot in batches and remain at cost costliness, a series of technical barriers such as technique is loaded down with trivial details, productive rate is lower.
Heteroatom doping can effectively regulate level structure, optical property, electricity and the surface chemistry of carbon material.Nitrogen-atoms has five valence electrons, and carbon atom has suitable atomic size size to be widely used in the chemical doping of carbon material, as nitrogen-doped carbon nanometer pipe (N-CNT) etc.According to the literature, nitrogen atom doping, to the effective band gap of grapheme material in grapheme material, is expanded its application in fields such as cell imaging, battery and analyses.Therefore, the present invention has developed a kind of new method and has prepared azepine graphene quantum dot (N-GQDS).
Summary of the invention
Deficiency and the shortcoming such as the object of the invention is to solve prior art cost costliness, technique is loaded down with trivial details, productive rate is lower, provides a kind of method of preparing azepine graphene quantum dot of novelty.It is raw material that this method adopts graphite oxide, by adding nitrogenous source to realize the successful preparation of azepine Graphene under the condition of high temperature annealing, be then oxidized to peel off with hydro-thermal reaction by strong acid respectively based on azepine Graphene and finally make the azepine graphene quantum dot (N-GQDS) with strong fluorescent effect and good aqueous solubility.
The preparation method of a kind of nitrogen-doped graphene quantum dot provided by the invention (N-GQDS), carries out according to following steps:
(1) preparation of azepine Graphene
In beaker, add graphite oxide and glycine, be dispersed in deionized water (consumption control is for dispersibling solvent, unsuitable too many), after the mixture of gained is ultrasonic, be transferred in aluminum oxide porcelain boat; Above-mentioned aluminum oxide porcelain boat is placed in to tube furnace and is warming up to preset temperature insulation afterwards, then cooling, obtain azepine graphene film.
(2) preparation of azepine graphene quantum dot (N-GQDS)
A. the azepine graphene film of gained in step (1) is dispersed in the mixed solvent of concentrated nitric acid and the vitriol oil,
Ultrasonic, then it is made to its cooling with deionized water dilution, then obtain with the acid that millipore filtration is removed wherein the azepine graphene film being oxidized.
The azepine graphene film of the oxidation B. steps A being obtained is dispersed in deionized water again, regulates its pH
Value; Finally, this dispersion liquid is transferred in the reactor of tetrafluoroethylene, and insulation reaction is to be cooled during to room temperature, again with collecting filtrate after filtering with microporous membrane.
C. above-mentioned reaction gained filtrate is put into dialysis tubing and dialyse, the azepine Graphene quantum that gets final product purely
Point (N-GQDS) solution.
Wherein, the mass ratio of the glycine described in step (1) and graphite oxide is 6-10:1; Described mixture ultrasonic time is 2 hours; Described be warming up to be incubated after preset temperature concrete operations under argon atmosphere with 5
othe speed of C/min is warming up to 500
oc, keeps temperature 2 hours.
Wherein, the amount ratio of azepine graphene film, concentrated nitric acid and the vitriol oil described in the A of step (2) is 50 mg:20-40 mL:5-20 mL; Described ultrasonic time is 16-24 hour; Described millipore filtration is Mierocrystalline cellulose filtering membrane; The working standard product that described concentrated nitric acid and the vitriol oil are laboratory, concentration is respectively 64-68 wt%, 95-98 wt%.
Wherein, described in step (2) B, regulate pH to regulate its pH value to 8 with the sodium hydroxide solution that concentration is 5 mol/L; Described insulation reaction is for keeping 200
oc reaction 10 hours.
Wherein, described in step (2) C, the interception of dialysis tubing is 8000-14000 Da, and dialysis time is 3-4 days.
beneficial effect of the present invention is:
(1) the synthetic method synthesis technique of azepine graphene quantum dot provided by the invention is simple, and desired raw material is the raw material being cheaply easy to get on market, and a kind of novel method of preparing azepine graphene quantum dot is provided;
(2) the azepine graphene quantum dot purity that prepared by the present invention and all higher, monodispersities of productive rate, good water solubility and have very strong blue-fluorescence performance, can look forward to it has extraordinary application prospect in Application Areass such as lithium cell, micro super capacitor, biological fluorescent labelling and solar cells.
Brief description of the drawings
Fig. 1 be azepine graphene quantum dot (N-GQDS) transmission electron microscope picture;
Fig. 2 is the fluorescence spectrum figure of azepine graphene quantum dot (N-GQDS) under different excitation wavelengths excite, and in figure, is followed successively by the spectrum under 340 nm, 360 nm, 380 nm, 400 nm, 420 nm, 440 nm, 460 nm, 480 nm wavelength from top to bottom; Illustration is the photo (right side) under (left side) and ultraviolet lamp (365 nm) under fluorescent lamp.
Embodiment
embodiment 1
1. the preparation of azepine Graphene
The graphite oxide and the 90 mg glycine that in beaker, add 15 mg, be dispersed in 5 mL deionized waters, and the mixture of gained was transferred in aluminum oxide porcelain boat after ultrasonic two hours.By above-mentioned aluminum oxide porcelain boat be placed in tube furnace under argon atmosphere with 5
othe speed of C/min is warming up to 500
oc, keeps temperature 2 hours, and naturally cooling afterwards, obtains azepine graphene film.
2. the preparation of azepine graphene quantum dot (N-GQDS)
A. azepine graphene film 50 mg described in step 1 are dispersed in the mixed solvent of concentrated nitric acid and the vitriol oil, ultrasonic 16 hours, then it is made to its cooling with suitable quantity of water dilution, then obtain with the acid that the millipore filtration that aperture is 0.22 μ m is removed wherein the azepine graphene film being oxidized; The azepine graphene film of every 50 mg, the concentrated nitric acid of 20 mL, the vitriol oil of 5 mL.
B. the azepine graphene film that step is after filtration attached to the solid oxidation on filtering membrane is dispersed in again
In ionized water, be diluted to 40 mL, regulate its pH value to 8 with 5 Mol/L sodium hydroxide solutions.Finally, this dispersion liquid is transferred in the reactor of tetrafluoroethylene of 25 mL, keeps 200
oc reaction 10 hours.To be cooled during to room temperature, again with collecting filtrate after filtering with microporous membrane.
C. above-mentioned reaction gained filtrate is put into interception and is the dialysis tubing of 8000-14000 Da and dialyse 3 ~ 4 days,
Azepine graphene quantum dot (N-GQDS) solution that gets final product purely.
embodiment 2
1. the preparation of azepine Graphene
The graphite oxide and the 120 mg glycine that in beaker, add 15 mg, be dispersed in 5 mL deionized waters, and the mixture of gained was transferred in aluminum oxide porcelain boat after ultrasonic two hours.By above-mentioned aluminum oxide porcelain boat be placed in tube furnace under argon atmosphere with 5
othe speed of C/min is warming up to 500
oc, keeps temperature 2 hours, and naturally cooling afterwards, obtains azepine graphene film.
2. the preparation of azepine graphene quantum dot (N-GQDS)
A. the mixing that azepine graphene film 50 mg described in step 1 is dispersed in to concentrated nitric acid and the vitriol oil is molten
In agent, ultrasonic 20 hours, then it is made to its cooling with suitable quantity of water dilution, then obtain with the acid that the millipore filtration that aperture is 0.22 μ m is removed wherein the azepine graphene film being oxidized; The azepine graphene film of every 50 mg, the concentrated nitric acid of 30 mL, the vitriol oil of 10 mL.
B. the azepine graphene film that step is after filtration attached to the solid oxidation on filtering membrane is dispersed in again
In ionized water, be diluted to 40 mL, regulate its pH value to 8 with 5 Mol/L sodium hydroxide solutions.Finally, this dispersion liquid is transferred in the reactor of tetrafluoroethylene of 25 mL, keeps 200
oc reaction 10 hours.To be cooled during to room temperature, again with collecting filtrate after filtering with microporous membrane.
C. above-mentioned reaction gained filtrate is put into interception and be the dialysis tubing of 8000-14000 Da and dialyse 3 ~ 4
My god, azepine graphene quantum dot (N-GQDS) solution that gets final product purely.
Fig. 1 is the transmission electron microscope picture that the present embodiment obtains, and has as can be seen from the figure successfully prepared size
For the azepine graphene quantum dot (N-GQDS) of homogeneous; Fig. 2 is the fluorescence spectrum figure of azepine graphene quantum dot (N-GQDS) under different excitation wavelengths excite that the present embodiment obtains, illustration is the photo (right side) under (left side) and ultraviolet lamp (365 nm) under fluorescent lamp, in figure: the azepine graphene quantum dot (N-GQDS) of gained is the emission spectrum characteristics that wavelength is relevant, illustration shows that prepared is the quantum dot of blue-fluorescence.
embodiment 3
1. the preparation of azepine Graphene
The graphite oxide and the 150 mg glycine that in beaker, add 15 mg, be dispersed in 5 mL deionized waters, and the mixture of gained was transferred in aluminum oxide porcelain boat after ultrasonic two hours.By above-mentioned aluminum oxide porcelain boat be placed in tube furnace under argon atmosphere with 5
othe speed of C/min is warming up to 500
oc, keeps temperature 2 hours, and naturally cooling afterwards, obtains azepine graphene film.
2. the preparation of azepine graphene quantum dot (N-GQDS)
A. the mixing that azepine graphene film 50 mg described in step 1 is dispersed in to concentrated nitric acid and the vitriol oil is molten
In agent, ultrasonic 24 hours, then it is made to its cooling with suitable quantity of water dilution, then obtain with the acid that the millipore filtration that aperture is 0.22 μ m is removed wherein the azepine graphene film being oxidized; The azepine graphene film of every 50 mg, the concentrated nitric acid of 40 mL, the vitriol oil of 20 mL.
B. the azepine graphene film that step is after filtration attached to the solid oxidation on filtering membrane is dispersed in again
In ionized water, be diluted to 40 mL, regulate its pH value to 8 with 5 Mol/L sodium hydroxide solutions.Finally, this dispersion liquid is transferred in the reactor of tetrafluoroethylene of 25 mL, keeps 200
oc reaction 10 hours.To be cooled during to room temperature, again with collecting filtrate after filtering with microporous membrane.
C. above-mentioned reaction gained filtrate is put into interception and be the dialysis tubing of 8000-14000 Da and dialyse 3 ~ 4
My god, azepine graphene quantum dot (N-GQDS) solution that gets final product purely.
Claims (5)
1. a preparation method for nitrogen-doped graphene quantum dot, is characterized in that, carries out according to following steps:
(1) preparation of azepine Graphene:
In beaker, add graphite oxide and glycine, be dispersed in deionized water, after the mixture of gained is ultrasonic, be transferred in aluminum oxide porcelain boat; Above-mentioned aluminum oxide porcelain boat is placed in to tube furnace and is warming up to preset temperature insulation afterwards, then cooling, obtain azepine graphene film;
(2) preparation of azepine graphene quantum dot:
A. the azepine graphene film of gained in step (1) is dispersed in the mixed solvent of concentrated nitric acid and the vitriol oil,
Ultrasonic, then it is made to its cooling with deionized water dilution, then obtain with the acid that millipore filtration is removed wherein the azepine graphene film being oxidized;
The azepine graphene film of the oxidation B. steps A being obtained is dispersed in deionized water again, regulates its pH
Value; Finally, this dispersion liquid is transferred in the reactor of tetrafluoroethylene, and insulation reaction is to be cooled during to room temperature, again with collecting filtrate after filtering with microporous membrane;
C. above-mentioned reaction gained filtrate is put into after dialysis tubing dialysis to the azepine Graphene amount that gets final product purely
Son point solution.
2. the preparation method of a kind of nitrogen-doped graphene quantum dot according to claim 1, is characterized in that, the mass ratio of the glycine described in step (1) and graphite oxide is 6-10:1; Described mixture ultrasonic time is 2 hours; Described be warming up to be incubated after preset temperature concrete operations under argon atmosphere with 5
othe speed of C/min is warming up to 500
oc, keeps temperature 2 hours.
3. the preparation method of a kind of nitrogen-doped graphene quantum dot according to claim 1, is characterized in that, the amount ratio of azepine graphene film, concentrated nitric acid and the vitriol oil described in the A of step (2) is 50 mg:20-40 mL:5-20 mL; Described ultrasonic time is 16-24 hour; Described millipore filtration is Mierocrystalline cellulose filtering membrane; The working standard product that described concentrated nitric acid and the vitriol oil are laboratory, concentration is respectively 64-68 wt%, 95-98 wt%.
4. the preparation method of a kind of nitrogen-doped graphene quantum dot according to claim 1, is characterized in that, regulates pH to regulate its pH value to 8 with the sodium hydroxide solution that concentration is 5 mol/L described in step (2) B; Described insulation reaction is for keeping 200
oc reaction 10 hours.
5. the preparation method of a kind of nitrogen-doped graphene quantum dot according to claim 1, is characterized in that, described in step (2) C, the interception of dialysis tubing is 8000-14000 Da, and dialysis time is 3-4 days.
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| CN104528833A (en) * | 2014-12-12 | 2015-04-22 | 江苏大学 | Preparation method of metal oxide/nitrogen doped graphene composite material |
| CN104555983A (en) * | 2014-12-26 | 2015-04-29 | 暨南大学 | Subliming precipitated carbon with metallic lustre and preparation method and application of subliming precipitated carbon |
| CN104710983A (en) * | 2015-03-02 | 2015-06-17 | 四川大学 | Method for preparing nitrogen-doped graphene quantum dots through metal ion coordination catalysis |
| CN104861967A (en) * | 2015-04-14 | 2015-08-26 | 中国工程物理研究院化工材料研究所 | Preparation method and application of nitrogen-doped graphene quantum dots |
| CN105329876A (en) * | 2015-10-29 | 2016-02-17 | 东华大学 | Preparation method of boron-nitrogen-co-doped carbon dots |
| CN105396606A (en) * | 2015-11-28 | 2016-03-16 | 吴滨 | Cerium oxide, graphene quantum dots and graphene-like phase carbon nitride composite photoactivate material and preparation method thereof |
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| CN107879335A (en) * | 2017-12-31 | 2018-04-06 | 西北师范大学 | A kind of preparation method of nitrogen-doped graphene quanta point material |
| CN107910525A (en) * | 2017-11-16 | 2018-04-13 | 中山大学 | A kind of preparation method of N doping manganese carbonate and its compound |
| CN108455578A (en) * | 2018-03-17 | 2018-08-28 | 宁夏大学 | Graphene quantum dot and preparation method and application |
| CN108529601A (en) * | 2017-03-01 | 2018-09-14 | 中国科学院福建物质结构研究所 | A kind of preparation method of high-quality nitrogen-doped graphene quantum dot |
| CN108538648A (en) * | 2018-07-18 | 2018-09-14 | 铜仁学院 | A kind of method that anode stripping graphite prepares nitridation graphene |
| CN110389167A (en) * | 2018-04-16 | 2019-10-29 | 南京大学 | It is a kind of using nitrogen-doped graphene quantum dot as the laser desorption ionization mass spectra analysis method of matrix |
| CN110577757A (en) * | 2018-06-07 | 2019-12-17 | 山东欧铂新材料有限公司 | Preparation method of high-dispersion graphene |
| CN110931265A (en) * | 2019-11-11 | 2020-03-27 | 江苏大学 | (Co)0.55Mn0.45)2P2O7Synthetic method and application of/NG composite electrode material |
| CN112607727A (en) * | 2020-12-30 | 2021-04-06 | 常州恒利宝纳米新材料科技有限公司 | Preparation method of high-nitrogen-content doped graphene quantum dots |
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| CN113213456A (en) * | 2020-01-21 | 2021-08-06 | 常州第六元素材料科技股份有限公司 | Amino acid modified graphene oxide film and preparation method thereof |
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Application publication date: 20141119 |