CN106219533B - 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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- CN106219533B CN106219533B CN201610633798.2A CN201610633798A CN106219533B CN 106219533 B CN106219533 B CN 106219533B CN 201610633798 A CN201610633798 A CN 201610633798A CN 106219533 B CN106219533 B CN 106219533B
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of preparation method of cold plasma N doping porous graphene.(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：In the 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid, when stirring oxidation processes 2~5 are small at 30 DEG C~60 DEG C, graphite oxide is obtained；(2) by step（1）Obtained graphite oxide is placed in crucible, is placed in micro-wave oven handling the s of 3 s~8 with the power microwave of 800~1000 W, is obtained porous graphene；(3) by step（2）Obtained porous graphene is placed in N2、NH3Or in air atmosphere cold plasma generating means, gas flow is the L/min of 1 L/min~5, N doping is carried out with the W of 10 W~40 and is handled 10~60 minutes, obtains N doping porous graphene.It is low energy consumption of the present invention, easy to operate, environmental-friendly, process is cleaned and dried without follow-up, obtained product structure stability is good, and N doping amount is high.
Description
Technical field
The present invention relates to a kind of preparation method of cold plasma N doping porous graphene.
Background technology
Graphene is a kind of emerging two-dimentional carbon material, and it is excellent to have that electrical conductivity is high, specific surface area is big, chemical stability is good etc.
Point, N doping is carried out to graphene can adjust its electronic structure, change surface nature, introduce active group etc..N doping stone
Black alkene is widely used in ultracapacitor, lithium-air battery, lithium ion battery and hydrogen reduction catalysis etc..（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, this will greatly reduce the specific surface area of graphene, from
And reduce its battery capacity, catalytic activity etc..And the reunion of graphene can effectively be prevented by building three-dimensional structure.And its internal tool
Some loose structures are conducive to the preservation of graphene active surface.(Chinese invention patent, CN103601181A)
It is cold dazzle it is firelight or sunlight etc.（Chinese invention patent, CN104777207A）Using foamed material as matrix, using CVD method containing nitrogen source
Under the conditions of deposit nitrogen-doped graphene, obtained after acid etch three-dimensional without support nitrogen-doped graphene, but CVD method is of high cost,
Yield is few；Xu Chunxiang etc.（Chinese invention patent, CN103496695A）Six methines four are added in the graphene oxide hydrosol
Amine, carries out N doping during thermal reduction, freeze-dried to obtain three-dimensional porous structure nitrogen-doped graphene, but this structure
Solution caves in, and be easy to cause environmental pollution with chemical method reduction.Therefore, mixed using low energy consumption, easy to operate, environmental-friendly nitrogen
The preparation method of miscellaneous porous graphene still needs to be explored.
The content of the invention
The object of the present invention is to provide a kind of preparation method of cold plasma N doping porous graphene.
Concretely comprise the following steps：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 2~5 are small at 30 DEG C~60 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with 800~1000 W
Power microwave handle the s of 3 s~8, obtain porous graphene.
(3) by step（2）Obtained porous graphene is placed in N2、NH3Or in air atmosphere cold plasma generating means,
Gas flow is the L/min of 1 L/min~5, and carrying out N doping with the W of 10 W~40 is handled 10~60 minutes, and it is more to obtain N doping
Hole graphene.
It is low energy consumption of the present invention, easy to operate, environmental-friendly, process is cleaned and dried without follow-up, obtained product structure is stablized
Property it is good, N doping amount is high.
Brief description of the drawings
Fig. 1 is that the SEM of 1 porous graphene of the embodiment of the present invention schemes.
Fig. 2 is that the SEM of 1 N doping porous graphene of the embodiment of the present invention schemes.
Fig. 3 is that the XPS of 2 N doping porous graphene of the embodiment of the present invention schemes.
Embodiment
Embodiment 1：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 5 are small at 30 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the work(of 1000 W
5 s of rate microwave treatment, obtains porous graphene.
(3) by step（2）Obtained porous graphene is placed in N2In atmosphere cold plasma generating means, gas flow
For 5 L/min, carry out N doping with 30 W and handle 60 minutes, obtain N doping porous graphene.
Embodiment 2：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 2 are small at 60 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the power of 900 W
3 s of microwave treatment, obtains porous graphene.
(3) by step（2）Obtained porous graphene is placed in NH3In atmosphere cold plasma generating means, gas flow
For 2L/min, carry out N doping with 20 W and handle 50 minutes, obtain N doping porous graphene.
Embodiment 3：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 3 are small at 50 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the power of 900 W
5 s of microwave treatment, obtains porous graphene.
(3) by step（2）Obtained porous graphene is placed in air atmosphere cold plasma generating means, gas stream
Measure as 3L/min, carrying out N doping with 40 W is handled 15 minutes, obtains N doping porous graphene.
Embodiment 4：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 4 are small at 40 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the work(of 1000 W
5 s of rate microwave treatment, obtains porous graphene.
(3) by step（2）Obtained porous graphene is placed in N2In atmosphere cold plasma generating means, gas flow
For 5L/min, carry out N doping with 40 W and handle 35 minutes, obtain N doping porous graphene.
Embodiment 5：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：The 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid
In, when stirring oxidation processes 2 are small at 60 DEG C, obtain graphite oxide.
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the power of 800 W
5 s of microwave treatment, obtains porous graphene.
(3) by step（2）Obtained porous graphene is placed in NH3In atmosphere cold plasma generating means, gas flow
For 3L/min, carry out N doping with 50 W and handle 35 minutes, obtain N doping porous graphene.
Claims (1)
1. a kind of preparation method of cold plasma N doping porous graphene, it is characterised in that concretely comprise the following steps：
(1) the commercially available crystalline flake graphites of 1g are placed in crucible, are placed in volume ratio as 3：In the 1 commercially available concentrated sulfuric acid and commercially available concentrated nitric acid,
When stirring oxidation processes 2~5 are small at 30 DEG C~60 DEG C, graphite oxide is obtained；
(2) by step（1）Obtained graphite oxide is placed in crucible, and is placed in micro-wave oven with the work(of 800~1000 W
The s of 3 s of rate microwave treatment~8, obtains porous graphene；
(3) by step（2）Obtained porous graphene is placed in N2、NH3Or in air atmosphere cold plasma generating means, gas
Flow is the L/min of 1 L/min~5, and carrying out N doping with the W of 10 W~40 is handled 10~60 minutes, obtains N doping porous stone
Black alkene.
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| CN106219533B true CN106219533B (en) | 2018-04-13 |
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| 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 |
| CN109205598B (en) * | 2018-11-16 | 2020-10-02 | 重庆大学 | Application of graphene-based compound, graphene-based compound and preparation method of graphene-based compound |
| 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 |
| CN114195136B (en) * | 2022-01-05 | 2023-07-07 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
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| CN102167311B (en) * | 2011-03-09 | 2013-04-10 | 华侨大学 | Method for preparing graphene on large scale |
| CN105185605B (en) * | 2015-08-27 | 2017-11-10 | 长春工业大学 | Load the electrode preparation method of graphene/metallic compound |
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