CN106219533A - A kind of preparation method of cold plasma N doping porous graphene - Google Patents
A kind of preparation method of cold plasma N doping porous graphene Download PDFInfo
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- CN106219533A CN106219533A CN201610633798.2A CN201610633798A CN106219533A CN 106219533 A CN106219533 A CN 106219533A CN 201610633798 A CN201610633798 A CN 201610633798A CN 106219533 A CN106219533 A CN 106219533A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses the preparation method of a kind of cold plasma N doping porous graphene.(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1, stir oxidation processes 2～5 hours at 30 DEG C～60 DEG C, obtain graphite oxide；(2) graphite oxide that step (1) obtains is placed in crucible, is placed in microwave oven processing with the power microwave of 800～1000 W 3 s～8 s, obtains porous graphene；(3) porous graphene that step (2) obtains is placed in N2、NH3Or in air atmosphere cold plasma generating means, gas flow is 1 L/min～5 L/min, carries out N doping with 10 W～40 W and process 10～60 minutes, obtain N doping porous graphene.Low energy consumption of the present invention, easily operation, environmental friendliness, it is not necessary to follow-up cleaning-drying process, the product structure good stability obtained, N doping amount is high.
Description
Technical field
The present invention relates to the preparation method of a kind of cold plasma N doping porous graphene.
Background technology
Graphene is a kind of emerging Two-dimensional Carbon material, and it is excellent to have that electrical conductivity is high, specific surface area is big, chemical stability is good etc.
Point, carries out N doping and can regulate its electronic structure, change surface nature, introduce active group etc. Graphene.N doping stone
Ink alkene is widely used at aspects such as ultracapacitor, lithium-air battery, lithium ion battery and hydrogen reduction catalysis.(ACS
Appl. Mater.Interfaces,2014,6,6361-6368.Energy Environ. Sci., 2012, 5,6928-
6932;Nano Lett., 2014,14,1164,1171.)
Graphene has planar structure, and single-layer graphene is easily reunited, and this will greatly reduce the specific surface area of Graphene, thus drops
Its battery capacity low, catalysis activity etc..And build three dimensional structure and can effectively prevent the reunion of Graphene.And have inside it
Loose structure is conducive to the preservation of Graphene active surface.(Chinese invention patent, CN103601181A)
Cold firelight or sunlight grade (Chinese invention patent, CN104777207A) of dazzling, with foamed materials as matrix, uses CVD containing nitrogen conditions
Lower deposition nitrogen-doped graphene, obtains three-dimensional without supporting nitrogen-doped graphene after acid etch, but CVD cost is high, yield
Few；Xu Chunxiang etc. (Chinese invention patent, CN103496695A) add hexamethylenetetramine in the graphene oxide hydrosol,
N doping, the freeze-dried three-dimensional porous structure nitrogen-doped graphene that obtains, but this structure-solution is carried out during thermal reduction
Cave in, and easily cause environmental pollution with chemical method reduction.Therefore, use low energy consumption, easily operation, eco-friendly N doping many
The preparation method of hole Graphene still needs to be explored.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of cold plasma N doping porous graphene.
Concretely comprise the following steps:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 30 DEG C～60 DEG C, stir oxidation processes 2～5 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with 800～1000 W
Power microwave process 3 s～8 s, obtain porous graphene.
(3) porous graphene that step (2) obtains is placed in N2、NH3Or in air atmosphere cold plasma generating means,
Gas flow is 1 L/min～5 L/min, carries out N doping with 10 W～40 W and processes 10～60 minutes, obtains N doping many
Hole Graphene.
Low energy consumption of the present invention, easily operation, environmental friendliness, it is not necessary to follow-up cleaning-drying process, the product structure obtained is stable
Property good, N doping amount is high.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the embodiment of the present invention 1 porous graphene.
Fig. 2 is the SEM figure of the embodiment of the present invention 1 N doping porous graphene.
Fig. 3 is the XPS figure of the embodiment of the present invention 2 N doping porous graphene.
Detailed description of the invention
Embodiment 1:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 30 DEG C, stir oxidation processes 5 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the merit of 1000 W
Rate microwave treatment 5 s, obtains porous graphene.
(3) porous graphene that step (2) obtains is placed in N2In atmosphere cold plasma generating means, gas flow
It is 5 L/min, carries out N doping with 30 W and process 60 minutes, obtain N doping porous graphene.
Embodiment 2:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 60 DEG C, stir oxidation processes 2 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the power of 900 W
Microwave treatment 3 s, obtains porous graphene.
(3) porous graphene that step (2) obtains is placed in NH3In atmosphere cold plasma generating means, gas flow
For 2L/min, carry out N doping with 20 W and process 50 minutes, obtain N doping porous graphene.
Embodiment 3:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 50 DEG C, stir oxidation processes 3 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the power of 900 W
Microwave treatment 5 s, obtains porous graphene.
(3) porous graphene that step (2) obtains is placed in air atmosphere cold plasma generating means, gas stream
Amount is 3L/min, carries out N doping with 40 W and processes 15 minutes, obtains N doping porous graphene.
Embodiment 4:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 40 DEG C, stir oxidation processes 4 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the merit of 1000 W
Rate microwave treatment 5 s, obtains porous graphene.
(3) porous graphene that step (2) obtains is placed in N2In atmosphere cold plasma generating means, gas flow
For 5L/min, carry out N doping with 40 W and process 35 minutes, obtain N doping porous graphene.
Embodiment 5:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 60 DEG C, stir oxidation processes 2 hours, obtain graphite oxide.
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the power of 800 W
Microwave treatment 5 s, obtains porous graphene.
(3) porous graphene that step (2) obtains is placed in NH3In atmosphere cold plasma generating means, gas flow
For 3L/min, carry out N doping with 50 W and process 35 minutes, obtain N doping porous graphene.
Claims (1)
1. the preparation method of a cold plasma N doping porous graphene, it is characterised in that concretely comprise the following steps:
(1) commercially available for 1g crystalline flake graphite is placed in crucible, is placed in the commercially available concentrated sulphuric acid and commercially available concentrated nitric acid that volume ratio is 3:1,
At 30 DEG C～60 DEG C, stir oxidation processes 2～5 hours, obtain graphite oxide；
(2) graphite oxide that step (1) obtains is placed in crucible, and is placed in microwave oven with the merit of 800～1000 W
Rate microwave treatment 3 s～8 s, obtains porous graphene；
(3) porous graphene that step (2) obtains is placed in N2、NH3Or in air atmosphere cold plasma generating means, gas
Flow is 1 L/min～5 L/min, carries out N doping with 10 W～40 W and processes 10～60 minutes, obtains N doping porous stone
Ink alkene.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107268023A (en) * | 2017-07-04 | 2017-10-20 | 中国船舶重工集团公司第七二五研究所 | A kind of grapheme modified preparation method for supporting noble metallic oxide anode |
| CN109205598A (en) * | 2018-11-16 | 2019-01-15 | 重庆大学 | The purposes of graphene-based compound, graphene-based compound and preparation method thereof |
| CN109368618A (en) * | 2018-11-07 | 2019-02-22 | 中科院合肥技术创新工程院 | The method of low temperature plasma preparation different type nitrogen-doped graphene |
| CN111342060A (en) * | 2020-03-03 | 2020-06-26 | 中科院合肥技术创新工程院 | Preparation method of platinum-nickel/nitrogen-doped reduced graphene oxide |
| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
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| CN102167311A (en) * | 2011-03-09 | 2011-08-31 | 华侨大学 | Method for preparing graphene on large scale |
| CN105185605A (en) * | 2015-08-27 | 2015-12-23 | 长春工业大学 | Loaded graphene/metallic compound-contained electrode preparation method based on hollow cathode plasma reduction and nitridation |
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| CN102167311A (en) * | 2011-03-09 | 2011-08-31 | 华侨大学 | Method for preparing graphene on large scale |
| CN105185605A (en) * | 2015-08-27 | 2015-12-23 | 长春工业大学 | Loaded graphene/metallic compound-contained electrode preparation method based on hollow cathode plasma reduction and nitridation |
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| 罗志虹等: "冷等离子掺氮处理对多壁碳纳米管超级电容器性能影响的研究", 《2015年第十四届全国应用化学年会论文集（上）》 * |
| 郭珺等: "冷等离子掺氮处理对多壁碳纳米管氧还原催化活性影响的研究", 《2015年第十四届全国应用化学年会论文集（上）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107268023A (en) * | 2017-07-04 | 2017-10-20 | 中国船舶重工集团公司第七二五研究所 | A kind of grapheme modified preparation method for supporting noble metallic oxide anode |
| CN109368618A (en) * | 2018-11-07 | 2019-02-22 | 中科院合肥技术创新工程院 | The method of low temperature plasma preparation different type nitrogen-doped graphene |
| CN109205598A (en) * | 2018-11-16 | 2019-01-15 | 重庆大学 | The purposes of graphene-based compound, graphene-based compound and preparation method thereof |
| CN111342060A (en) * | 2020-03-03 | 2020-06-26 | 中科院合肥技术创新工程院 | Preparation method of platinum-nickel/nitrogen-doped reduced graphene oxide |
| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
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| CN106219533B (en) | 2018-04-13 |
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