CN107098335A - A kind of three-dimensional nitridation graphene and preparation method thereof - Google Patents
A kind of three-dimensional nitridation graphene and preparation method thereof Download PDFInfo
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- CN107098335A CN107098335A CN201710515102.0A CN201710515102A CN107098335A CN 107098335 A CN107098335 A CN 107098335A CN 201710515102 A CN201710515102 A CN 201710515102A CN 107098335 A CN107098335 A CN 107098335A
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of three-dimensional nitridation grapheme material and preparation method thereof, the nitridation graphene is in be distributed a large amount of holes between three-dimensional sheet structure, nanoscale twins.Its preparation process includes：1）Take graphite 1g to be mixed with 0.4g LiNO3, add after being uniformly mixed in dense HNO3 solution, ice bath, move into 50 DEG C of tepidariums, add 4g NH4NO3 reactions；Then 40 mL deionized waters are added, and keep reaction temperature to be 90 DEG C, after stirring 10min, are filtered while hot, and are repeatedly washed with deionized water, is placed in NH3 atmosphere dry box and is dried at 90 DEG C after centrifugation.2）Dried product is dissolved in deionized water, ultrasonic disperse；Heating, is filtered after hydration hydrazine reaction is added dropwise, and is placed in NH3 atmosphere dry box at 70 DEG C second and is dried；It is placed in horizontal pipe furnace and anneals afterwards, three-dimensional nitridation grapheme material is made.Three-dimensional nitridation graphene prepared by the present invention, has the double grading of three-dimensional grapheme and nitridation graphene concurrently, has great application prospect.
Description
Technical field
The present invention relates to grapheme material field, grapheme material field is especially nitrogenized.
Background technology
Graphene be it is a kind of by carbon atom pass through sp2 hydridization after the two-dimensional nano material with alveolate texture that is formed
Material.From 2004, being isolated in an experiment from graphite first can be with the grapheme material of individualism, and at present, graphene can
To be known as the two-dimension nano materials being most widely used, it does not only exist very unique internal structure, and with very
Excellent electrical properties, mechanical property, thermal property and optical property.
Because grapheme material its own size of two dimension is smaller, increases to be processed it in some cases and use
Difficulty, this is very big to a certain extent to limit application of the grapheme material in real life.And three-dimensional grapheme material
Material is rich in pore structure, with higher specific surface area, relatively low density, and this also determines its good electric conductivity, thermally-stabilised
Property and other aspect properties, therefore, there is important potential using value in the field such as ultracapacitor and new catalytic.
Graphene can significantly improve the electric conductivity of its own by the method for N doping.N doping process is introduced to
Prepare during graphene, be expected to prepare chemical property more preferably nitrogen-doped graphene, and then so that performance is made more relatively
Good ultracapacitor.The research report of current graphene is a lot, and nitridation graphene is expected have some unique performances, but mesh
The report of preceding this respect is still limited.
The content of the invention
It is contemplated that a kind of nitridation graphene simple and easy to apply of invention and preparation method thereof.
The invention provides a kind of three-dimensional nitridation grapheme material and preparation method thereof, the nitridation graphene is in three-dimensional plate
Shape structure, nanometer sheet thickness is 1-3nm, and size uniformity is evenly distributed, and a large amount of holes are distributed between nanoscale twins.
Present invention also offers a kind of three-dimensional nitridation grapheme material and preparation method thereof, it is characterised in that including following step
Suddenly：
1）325 mesh graphite 1g are weighed, are mixed with 0.4g LiNO3, the dense HNO3 solution of 24 mL is added, is placed in ice bath and stirs 40
min；After well mixed, move into 50 DEG C of tepidariums, add 4g NH4NO3, react 50 min；40 mL are then slowly added into go
Ionized water, and keep reaction temperature to be 90 DEG C, after stirring 10min, filter while hot, and repeatedly washed with deionized water, from
It is placed in NH3 atmosphere dry box at 90 DEG C and fully dries after the heart；
2）Above-mentioned dried product 0.4g is dissolved in 100g deionized waters, ultrasonic disperse 60min obtains dispersion liquid；Plus
Heat partition liquid is filtered to 90 DEG C after hydrazine hydrate 8mL, reaction 3h is added dropwise, and is rinsed repeatedly with deionized water, is subsequently placed in NH3 gas
Dried for the second time at 70 DEG C in atmosphere drying box；
3）Above-mentioned second of dried product is placed in horizontal pipe furnace, and anneal 1-3h in NH3-H2-N2 mixed gas,
1200 DEG C of annealing temperature, gas pressure intensity is 10Pa, and NH3, H2, N2 intrinsic standoff ratio are 2:2:1.
The useful achievement of the present invention is：
1）Nitridation graphene prepared by the present invention, is three-dimensional sheet structure, and nanometer sheet size uniformity is evenly distributed.
2）The method of the present invention, it is simple and easy to apply, it is particularly suitable for mass industrialized production.
3）Three-dimensional nitridation graphene prepared by the present invention, has the double grading of three-dimensional grapheme and nitridation graphene, tool concurrently
There is very big application prospect.
Brief description of the drawings
Fig. 1 is embodiment 1）The Scanning Electron microscope of obtained three-dimensional nitridation graphene（SEM）Figure.
Embodiment
With reference to specific embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
1）325 mesh graphite 1g are weighed, are mixed with 0.4g LiNO3, the dense HNO3 solution of 24 mL is added, is placed in ice bath and stirs 40
min；After well mixed, move into 50 DEG C of tepidariums, add 4g NH4NO3, react 50 min；40 mL are then slowly added into go
Ionized water, and keep reaction temperature to be 90 DEG C, after stirring 10min, filter while hot, and repeatedly washed with deionized water, from
It is placed in NH3 atmosphere dry box at 90 DEG C and fully dries after the heart；
2）Above-mentioned dried product 0.4g is dissolved in 100g deionized waters, ultrasonic disperse 60min obtains dispersion liquid；Plus
Heat partition liquid is filtered to 90 DEG C after hydrazine hydrate 8mL, reaction 3h is added dropwise, and is rinsed repeatedly with deionized water, is subsequently placed in NH3 gas
Fully dried at 70 DEG C in atmosphere drying box；
3）It is above-mentioned it is high and dry again after product be placed in horizontal pipe furnace, anneal 1h in NH3-H2-N2 mixed gas, annealing
1200 DEG C of temperature, gas pressure intensity is 10Pa, and NH3, H2, N2 intrinsic standoff ratio are 2:2:1.
Embodiment 2
1）325 mesh graphite 1g are weighed, are mixed with 0.4g LiNO3, the dense HNO3 solution of 24 mL is added, is placed in ice bath and stirs 40
min；After well mixed, move into 50 DEG C of tepidariums, add 4g NH4NO3, react 50 min；40 mL are then slowly added into go
Ionized water, and keep reaction temperature to be 90 DEG C, after stirring 10min, filter while hot, and repeatedly washed with deionized water, from
It is placed in NH3 atmosphere dry box at 90 DEG C and fully dries after the heart；
2）Above-mentioned dried product 0.4g is dissolved in 100g deionized waters, ultrasonic disperse 60min obtains dispersion liquid；Plus
Heat partition liquid is filtered to 90 DEG C after hydrazine hydrate 8mL, reaction 3h is added dropwise, and is rinsed repeatedly with deionized water, is subsequently placed in NH3 gas
Fully dried at 70 DEG C in atmosphere drying box；
3）It is above-mentioned it is high and dry again after product be placed in horizontal pipe furnace, anneal 2h in NH3-H2-N2 mixed gas, annealing
1200 DEG C of temperature, gas pressure intensity is 10Pa, and NH3, H2, N2 intrinsic standoff ratio are 2:2:1.
Embodiment 3
1）325 mesh graphite 1g are weighed, are mixed with 0.4g LiNO3, the dense HNO3 solution of 24 mL is added, is placed in ice bath and stirs 40
min；After well mixed, move into 50 DEG C of tepidariums, add 4g NH4NO3, react 50 min；40 mL are then slowly added into go
Ionized water, and keep reaction temperature to be 90 DEG C, after stirring 10min, filter while hot, and repeatedly washed with deionized water, from
It is placed in NH3 atmosphere dry box at 90 DEG C and fully dries after the heart；
2）Above-mentioned dried product 0.4g is dissolved in 100g deionized waters, ultrasonic disperse 60min obtains dispersion liquid；Plus
Heat partition liquid is filtered to 90 DEG C after hydrazine hydrate 8mL, reaction 3h is added dropwise, and is rinsed repeatedly with deionized water, is subsequently placed in NH3 gas
Fully dried at 70 DEG C in atmosphere drying box；
3）It is above-mentioned it is high and dry again after product be placed in horizontal pipe furnace, anneal 3h in NH3-H2-N2 mixed gas, annealing
1200 DEG C of temperature, gas pressure intensity is 10Pa, and NH3, H2, N2 intrinsic standoff ratio are 2:2:1.
Pass through SEM（SEM）Microscopic appearance sight is carried out to three-dimensional nitridation graphene made from each embodiment
Examine, observation indicate that nitridation graphene is in three-dimensional sheet structure, nanometer sheet thickness is 1-3nm, and size uniformity is evenly distributed,
A large amount of holes are distributed between nanoscale twins.Such as the Scanning Electron microscope that Fig. 1 is the three-dimensional nitridation graphene that embodiment 1 is obtained
（SEM）Figure.Additionally by the nitrogen content in the EDX test graphenes being attached in SEM, test result is shown
Nitrogen content in three-dimensional nitridation graphene made from embodiment 1 is 1.5%；Nitrogen content in three-dimensional grapheme made from embodiment 2
For 1.7%；Nitrogen content in three-dimensional grapheme made from embodiment 3 is 2.5%.
Obviously, completely and clearly described although present disclosure has been made with regard to its disclosed embodiment,
It is not limited only to this, and embodiments described above is only a part of embodiment of the invention, rather than whole embodiments.It is right
For the personnel of art, obtained institute is made improvements and substitutes to the present invention by the guidance that these are stated
There is other embodiment, among the present invention.
Claims (5)
1. a kind of three-dimensional nitridation graphene and preparation method thereof, it is characterised in that：The nitridation graphene is in three-dimensional sheet structure,
Size uniformity, is evenly distributed, and a large amount of holes are distributed between nanoscale twins.
2. a kind of three-dimensional nitridation graphene according to claim 1 and preparation method thereof, it is characterised in that：The nitridation stone
Black alkene nanometer sheet thickness is 1-3nm.
3. a kind of three-dimensional nitridation graphene according to claim 1 or 2 and preparation method thereof, it is characterised in that including as follows
Step：
1）Graphite 1g is weighed, is mixed with 0.4g LiNO3, the dense HNO3 solution of 24mL is added, is placed in ice bath and stirs 40min；It is mixed
After closing uniformly, move into 50 DEG C of tepidariums, add 4g NH4NO3, react 50 min；40 mL deionized waters are then slowly added into,
And keep reaction temperature to be 90 DEG C, after stirring 10min, filter while hot, and repeatedly washed with deionized water, it is placed in after centrifugation
Fully dried at 90 DEG C in NH3 atmosphere dry box；
2）Above-mentioned dried product 0.4g is dissolved in 100g deionized waters, ultrasonic disperse 60min obtains dispersion liquid；Plus
Heat partition liquid is filtered to 90 DEG C after hydrazine hydrate 8mL, reaction 3h is added dropwise, and is rinsed repeatedly with deionized water, is subsequently placed in NH3 gas
Dried for the second time at 70 DEG C in atmosphere drying box；
3）Above-mentioned second of dried product is placed in horizontal pipe furnace, and anneal 1-3h in NH3-H2-N2 mixed gas,
1200 DEG C of annealing temperature, gas pressure intensity is 10Pa.
4. a kind of three-dimensional nitridation graphene according to claim 3 and preparation method thereof, it is characterised in that：Step 1）Weigh
Graphite be 325 mesh.
5. a kind of three-dimensional nitridation graphene according to claim 3 and preparation method thereof, it is characterised in that：Step 3）NH3-
In H2-N2 mixed gas, NH3, H2, N2 intrinsic standoff ratio are 2:2:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010059505A4 (en) * | 2008-11-12 | 2010-07-22 | Zornes David A | Perpendicular suspension of one planer two dimensional (2d) graphene sheet stack by aligning its six-member carbon atoms within the hexagonal centerpoint holes of a second graphene sheet stack that occupy the same three dimensional (3d) space |
| CN103601181A (en) * | 2013-12-04 | 2014-02-26 | 南京大学扬州化学化工研究院 | Method for preparing nitrogen-doped graphene with polydopamine as raw material |
| US20140313636A1 (en) * | 2011-11-18 | 2014-10-23 | William Marsh Rice University | Graphene-carbon nanotube hybrid materials and use as electrodes |
| CN104495833A (en) * | 2015-01-14 | 2015-04-08 | 北京化工大学 | Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof |
-
2017
- 2017-06-29 CN CN201710515102.0A patent/CN107098335A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010059505A4 (en) * | 2008-11-12 | 2010-07-22 | Zornes David A | Perpendicular suspension of one planer two dimensional (2d) graphene sheet stack by aligning its six-member carbon atoms within the hexagonal centerpoint holes of a second graphene sheet stack that occupy the same three dimensional (3d) space |
| US20140313636A1 (en) * | 2011-11-18 | 2014-10-23 | William Marsh Rice University | Graphene-carbon nanotube hybrid materials and use as electrodes |
| CN103601181A (en) * | 2013-12-04 | 2014-02-26 | 南京大学扬州化学化工研究院 | Method for preparing nitrogen-doped graphene with polydopamine as raw material |
| CN104495833A (en) * | 2015-01-14 | 2015-04-08 | 北京化工大学 | Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof |
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Application publication date: 20170829 |