CN109422259A - A kind of preparation method of nitrogen-doped graphene - Google Patents
A kind of preparation method of nitrogen-doped graphene Download PDFInfo
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- CN109422259A CN109422259A CN201710732334.1A CN201710732334A CN109422259A CN 109422259 A CN109422259 A CN 109422259A CN 201710732334 A CN201710732334 A CN 201710732334A CN 109422259 A CN109422259 A CN 109422259A
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- nitrogen
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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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Abstract
The invention discloses a kind of preparation methods of nitrogen-doped graphene compound, are all the advantage of nodular powder using graphite powder and rich nitrogen carbon-based material, remove graphite linings in situ using dry ball milling, prepare nitrogen-doped graphene compound.Specific steps are as follows: (1) premix of graphite powder and rich nitrogen carbon-based material abundant ball milling, removing in the ball mill, preparation richness nitrogen carbon-based material/graphene complex；(2) mixture after abundant drying is calcined in Muffle furnace, products therefrom is nitrogen-doped graphene composite material.Method operating procedure provided by the invention is simple, controllability is good, it is at low cost, without complicated chemical treatment, yet do not need expensive equipment, be easy to industrialization.
Description
Technical field
The invention belongs to inorganic nano composite material preparation fields, are related to a kind of preparation side of nitrogen-doped graphene compound
Method.
Background technique
Graphene is with unusual electric conductivity, resistivity about 10-6Ω m, high specific surface area, chemical stability
Good and wider electrochemical window, can be widely applied to the every field such as sensor, supercapacitor, lithium battery.To graphite
Alkene carry out chemical modification, such as generation derivative, surface functionalization, chemical modification, chemical doping, can effectively modulation its
Structure and performance, and then realize graphene and its more abundant function of associated materials and wide application
For chemical doping, nitrogen-atoms due to have with the approximate atomic radius of carbon atom, and its electronegativity than carbon original
It is sub big, it can be used as electron donor and graphene be doped in a manner of replacing, and the nitrogen-doped graphene generated is shown
The more excellent performance nitrogen atom dopings of purer graphene can effectively regulate and control the band structure of graphene, improve its electricity
The electro catalytic activity of graphene can be improved in chemical property.
Summary of the invention
Technical problem solved by the invention is that providing nitrogen-doped graphene that is a kind of simple and being easy to industrialization answers
The preparation method of condensation material, to solve the disadvantage in above-mentioned background technique.
Technical problem solved by the invention is realized using following technical scheme:
1. abrading-ball, graphite powder and rich nitrogen carbon-based material is admixed together according to the ratio of 80-60:4-2:4-2 and use ball mill
Grinding 30-120 minutes, then that mixture is sufficiently dry, drying time is 5-10 hours, and drying temperature is 100-150 DEG C；
2. the mixture after drying is fully calcined in Muffle furnace, calcination time is 5-20 hours, calcination temperature 300-500
DEG C, products therefrom is nitrogen-doped graphene composite material.
Preferably, the raw material of graphite powder is graphene microchip, crystalline flake graphite, expansible graphite, amorphous graphite, expansion stone
The combination of one or more of ink, thermal cracking graphite, highly oriented graphite；
Preferably, above-mentioned rich nitrogen carbon-based material is the combination of one or both of polyaniline, melamine；
Preferably, ball mill is the ball-grinding machines such as planetary ball mill, stirring ball mill or horizontal ball mill.
Preferably, abrading-ball is the combination of one or more of alloying pellet, zirconia ball, agate ball, steel ball, chromium ball.
The invention has the following beneficial effects:
1. the nitrogen-doped graphene compound nitrogen content with higher prepared through the invention, it is made to have high capacitance and excellent
Chemical property；
2. this method simple process, raw material sources are extensive, low in cost, it is easy to accomplish industrialization；
3. this method prepares nitrogen-doped graphene using thermal response method, solid nitrogen source and carbon source are uniformly mixed, raw material availability
It is high.
Specific embodiment:
In order to better understand the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention interior
Appearance is not limited solely to embodiment below.
Embodiment 1
It weighs 4 grams of crystalline flake graphites, 2g melamine, 60g zirconia ball respectively first, is put into row after these materials are sufficiently mixed
Grind 100 minutes in planetary ball mill, it is then that the mixture after grinding is 5 hours dry at 120 DEG C, then by the mixing after drying
Object is placed in Muffle furnace to be calcined 10 hours at 400 DEG C, just obtains nitrogen-doped graphene.
Embodiment 2
It weighs 3 grams of graphene microchips, 4g polyaniline, 80g agate ball respectively first, stirring is put into after these materials are sufficiently mixed
Grind 100 minutes in formula ball mill, it is then that the mixture after grinding is 6 hours dry at 100 DEG C, then by the mixture after drying
It is placed in Muffle furnace and is calcined 15 hours at 300 DEG C, just obtain nitrogen-doped graphene.
Embodiment 3
It weighs 4 grams of expanded graphites, 1g melamine, 2g polyaniline, 80g alloying pellet respectively first, these materials is sufficiently mixed
After be put into horizontal ball mill and grind 120 minutes, it is then that the mixture after grinding is 6 hours dry at 100 DEG C, then will it is dry after
Mixture be placed in Muffle furnace and calcined 8 hours at 350 DEG C, just obtain nitrogen-doped graphene.
Claims (3)
1. a kind of preparation method of nitrogen-doped graphene compound, which is characterized in that at least include the following steps:
(1) abrading-ball, graphite powder and rich nitrogen carbon-based material is admixed together according to the ratio of 80-60:4-2:4-2 and use ball milling
Machine is ground 30-120 minutes, then that mixture is sufficiently dry, and drying time is 5-10 hours, and drying temperature is 100-150 DEG C；
(2) mixture after drying is fully calcined in Muffle furnace, calcination time is 5-20 hours, calcination temperature 300-
500 DEG C, products therefrom is nitrogen-doped graphene composite material.
2. a kind of preparation method of nitrogen-doped graphene compound according to claim 1, it is characterised in that: above-mentioned graphite
The raw material of powder is crystalline flake graphite, amorphous graphite, expansible graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphene
The combination of one or more of microplate；
A kind of preparation method of nitrogen-doped graphene compound according to claim 1, it is characterised in that: above-mentioned richness nitrogen carbon
Sill is the combination of one or both of polyaniline, melamine；
A kind of preparation method of nitrogen-doped graphene compound according to claim 1, it is characterised in that: above-mentioned ball mill
For ball-grinding machines such as planetary ball mill, stirring ball mill or horizontal ball mills.
3. a kind of preparation method of nitrogen-doped graphene compound according to claim 1, it is characterised in that: above-mentioned abrading-ball
For the combination of one or more of zirconia ball, steel ball, agate ball, chromium ball, alloying pellet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710732334.1A CN109422259A (en) | 2017-08-24 | 2017-08-24 | A kind of preparation method of nitrogen-doped graphene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710732334.1A CN109422259A (en) | 2017-08-24 | 2017-08-24 | A kind of preparation method of nitrogen-doped graphene |
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| Publication Number | Publication Date |
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| CN109422259A true CN109422259A (en) | 2019-03-05 |
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| CN201710732334.1A Pending CN109422259A (en) | 2017-08-24 | 2017-08-24 | A kind of preparation method of nitrogen-doped graphene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498408A (en) * | 2019-09-02 | 2019-11-26 | 燕山大学 | Graphene self assembly powder and preparation method thereof |
| CN111992237A (en) * | 2020-09-05 | 2020-11-27 | 福州大学 | Nitrogen-rich carbon material catalyst, preparation method and application thereof in selective oxidation of hydrogen sulfide |
| CN113371701A (en) * | 2021-06-08 | 2021-09-10 | 清华大学 | Graphene and green preparation method thereof |
Citations (4)
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| KR20130139461A (en) * | 2012-06-12 | 2013-12-23 | 이혜경 | Pure Graphene Mass Production Method II |
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| CN105417532A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | One-step preparation method for high nitrogen doped graphene |
| US20170174522A1 (en) * | 2015-12-16 | 2017-06-22 | Agency For Defense Development | Nitrogen-doped graphene assembly and method of preparing the same |
-
2017
- 2017-08-24 CN CN201710732334.1A patent/CN109422259A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130139461A (en) * | 2012-06-12 | 2013-12-23 | 이혜경 | Pure Graphene Mass Production Method II |
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| US20170174522A1 (en) * | 2015-12-16 | 2017-06-22 | Agency For Defense Development | Nitrogen-doped graphene assembly and method of preparing the same |
| CN105417532A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | One-step preparation method for high nitrogen doped graphene |
Non-Patent Citations (2)
| Title |
|---|
| SOARES, O.S.G.P.等: "Easy method to prepare N-doped carbon nanotubes", 《CARBON》 * |
| XUE, YH等: "Nitrogen-doped graphene by ball-milling graphite with melamine for energy conversion and storage", 《2D MATERIALS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498408A (en) * | 2019-09-02 | 2019-11-26 | 燕山大学 | Graphene self assembly powder and preparation method thereof |
| CN111992237A (en) * | 2020-09-05 | 2020-11-27 | 福州大学 | Nitrogen-rich carbon material catalyst, preparation method and application thereof in selective oxidation of hydrogen sulfide |
| CN113371701A (en) * | 2021-06-08 | 2021-09-10 | 清华大学 | Graphene and green preparation method thereof |
| CN113371701B (en) * | 2021-06-08 | 2022-11-18 | 清华大学 | Graphene and green preparation method thereof |
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Application publication date: 20190305 |