CN101717083A - Graphene and preparation method thereof - Google Patents
Graphene and preparation method thereof Download PDFInfo
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- CN101717083A CN101717083A CN200910312486A CN200910312486A CN101717083A CN 101717083 A CN101717083 A CN 101717083A CN 200910312486 A CN200910312486 A CN 200910312486A CN 200910312486 A CN200910312486 A CN 200910312486A CN 101717083 A CN101717083 A CN 101717083A
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Abstract
The invention provides a graphene and a preparation method thereof, belonging to the technical field of grapheme synthesis. Nitrogen-doped grapheme can be prepared by using a direct current electric arc method and taking mixed gas of ammonia gas and helium gas as reaction atmosphere. The nitrogen-doped grapheme with high yield can be prepared by adopting the preparation method of the grapheme under low pressure and low current and has high production safety. The purity of the prepared grapheme is over 97 percent; by the characterization of a transmission electron microscope, the layer number of the prepared grapheme is between 2 and 6, the size of grapheme sheets is between 100 and 200 nanometers and the interlayer spacing is about 0.4 nanometer. The produced nitrogen-doped grapheme has favorable application prospect in catalyst carriers, lithium ion batteries, conductive thin films and other aspects.
Description
Technical field
The present invention relates to the synthetic technology of Graphene, specifically is a kind of nitrogen-doped graphene and preparation method thereof.
Background technology
Graphene is the new allotropic substance of the carbon of discovered in recent years, and it is to arrange the two-dirnentional structure that forms with the hexagonal mesh form by carbon atom.Only the single-layer graphene of being made up of one deck carbon atom has excellent electricity and mechanical property (Science, 2004,306,666-669; Science, 2008,321,385-388), have broad application prospects in fields such as nanometer electronic device, opto-electronic conversion and battery materials.Except that single-layer graphene, bilayer and multiwalled Graphene also have unique physics and chemical property (Journal of Materials Chemistry, 2009,19,2457-2469).Therefore, the synthetic and property research of Graphene becomes the focus in the nano science research in recent years.
The synthetic method of Graphene is broadly divided into two classes.First kind method is the material that will contain graphite linings carries out chemistry or thereby physical treatment obtains discrete graphite linings.For example, with adhesive tape with graphite repeatedly tear-off make its attenuate, can obtain double-deck and single-layer graphene (Science, 2004,306,666-669); With chemical process with graphite carry out intercalation peel off also can obtain single-layer graphene (Journal of Physical Chemistry B, 2006,110,8535-8539).In addition, by oxidation or plasma etching carbon nanotube is split vertically and also can form Graphene (Nature, 2009,458,872-875; Nature, 2009,458,877-880).Second class methods are to utilize the carbonaceous presoma formation Graphene of growing, and specifically comprise (Nature Nanotechnology, 2009,4,30-33 such as solvent-thermal method, chemical Vapor deposition process and arc process; Nature, 2009,457,706-710; Journal of Physical Chemistry C, 2009,113,4257-4259).In above the whole bag of tricks, arc process has big, the simple operation and other advantages of output, is a kind of method with scale operation potentiality.
Arc process the earliest by people such as Rao CNR be used for preparing Graphene (Journal of Physical Chemistry C, 2009,113,4257-4259), they use the mixed atmosphere of hydrogen and helium as reaction atmosphere.Use this method to prepare higher hydrogen pressure of Graphene needs and bigger discharging current, dangerous higher.
Summary of the invention
The object of the present invention is to provide a kind of nitrogen-doped graphene that adopts the arc process preparation.
Above-mentioned purpose of the present invention is achieved by the following technical solutions:
A kind of Graphene is characterized in that, is doped with nitrogen-atoms in Graphene.
Nitrogen percent content in the Graphene (number ratio) is 1-2%.
A kind of preparation method of nitrogen-doped graphene, adopting specpure graphite rod is the negative electrode and the anode of electric arc furnace, is that reaction atmosphere carries out the direct current arc discharge with the gas mixture of ammonia and helium, in discharge process, graphite anode rod constantly consumes, and obtains nitrogen-doped graphene on the inwall of electric arc furnace.
The volume ratio of described helium and ammonia can be 1: 1-1: 3.
The pressure of described reaction atmosphere can be 380-760Torr.
The electric current of described direct current arc discharge can be 80-120A.
Can remove small amount of amorphous carbon in the product with obtaining nitrogen-doped graphene calcination in air on the electric arc furnace inwall.
Described calcination temperature can be 400-500 ℃.
Described calcination time can be 30-60 minute.
Technological merit of the present invention and effect:
1) use direct current arc method, equipment is simple, production cost is low, and can reach mass-produced requirement.
2) degree of purity of production height, after simple calcination purifying, purity can reach more than 97%.
3) use of ammonia makes and is doped with nitrogen-atoms in the Graphene, and compare with the Graphene of pure carbon, the Graphene of nitrogen atom doping has new character.
4) gas mixture that uses ammonia and helium can prepare Graphene as reaction atmosphere under low pressure and little electric current, compares with the use hydrogen atmosphere and has improved security.
Use and can produce the tens of grams of Graphene every day of the present invention, product characterizes through transmission electron microscope, and between 2-6, the size of graphene film is between the 100-200 nanometer mostly for its number of plies, and graphite layers is apart from being about 0.4 nanometer.The Graphene that present method is produced has good application prospects at aspects such as support of the catalyst, lithium ion battery and conductive films.
Description of drawings
Below in conjunction with accompanying drawing the present invention is illustrated in further detail:
The electron scanning micrograph of Fig. 1 Graphene;
The transmission electron microscope photo of Fig. 2 Graphene;
The high resolution transmission electron microscopy photo of Fig. 3 Graphene;
The thermogravimetric of Fig. 4 Graphene and differential curve thereof;
The XPS spectrum of Fig. 5 Graphene.
Embodiment
Below with reference to accompanying drawing of the present invention, more detailed description goes out most preferred embodiment of the present invention.
Embodiment one
Adopt electric arc furnace to prepare Graphene, cool off with recirculated water the furnace wall of electric arc furnace.Adopting specpure graphite rod respectively is the negative electrode and the anode of electric arc furnace, and the diameter of the two poles of the earth graphite rod is 8mm.At helium and ammonia gas mixture (volume ratio is 1: 1) pressure is that 760Torr, electric current are under the condition of 120A, carries out the direct current arc discharge.Collect product after anode consumption is intact, in air,, obtain the nitrogen atom doping Graphene in 450 ℃ of calcinations 1 hour.The electron scanning micrograph of this Graphene, as shown in Figure 1.The outstanding edge of Graphene illustrates and makes flaky Graphene as can be seen from Figure 1; Fig. 2 is the transmission electron microscope photo of this Graphene, and the size of graphene film is between the 100-200 nanometer; Fig. 3 is the high resolution transmission electron microscopy photo of this Graphene, and that a-c is respectively is double-deck, the edge of three layers and four layer graphenes; Fig. 4 is the thermogravimetric and the differential curve thereof of this Graphene, there not being obviously weightlessness below 500 ℃, does not contain decolorizing carbon in the interpret sample; Fig. 5 is the XPS spectrum of this Graphene, contains nitrogen-atoms in the Graphene as can be seen from Figure 5.
Embodiment two
Adopt electric arc furnace to prepare Graphene, cool off with recirculated water the furnace wall of electric arc furnace.Adopting specpure graphite rod respectively is the negative electrode and the anode of electric arc furnace, and the diameter of the two poles of the earth graphite rod is 8mm.At helium and ammonia gas mixture (volume ratio is 1: 2) pressure is that 760Torr, electric current are under the condition of 120A, carries out the direct current arc discharge.Collect product after anode consumption is intact, in air,, obtain the nitrogen atom doping Graphene in 450 ℃ of calcinations 1 hour.
Embodiment three
Adopt electric arc furnace to prepare Graphene, cool off with recirculated water the furnace wall of electric arc furnace.Adopting specpure graphite rod respectively is the negative electrode and the anode of electric arc furnace, and the diameter of the two poles of the earth graphite rod is 8mm.At helium and ammonia gas mixture (volume ratio is 1: 3) pressure is that 380Torr, electric current are under the condition of 80A, carries out the direct current arc discharge.Collect product after anode consumption is intact, in air,, obtain the nitrogen atom doping Graphene in 500 ℃ of calcinations 1 hour.
The foregoing description is of the present invention giving an example, although disclose most preferred embodiment of the present invention and accompanying drawing for the purpose of illustration, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various replacements, variation and modification all are possible.Therefore, the present invention should not be limited to most preferred embodiment and the disclosed content of accompanying drawing.
Claims (9)
1. a Graphene is characterized in that, is doped with nitrogen-atoms in Graphene.
2. Graphene as claimed in claim 1 is characterized in that, nitrogen percent content is 1-2% in the Graphene.
3. the preparation method of a nitrogen-doped graphene is characterized in that, uses direct current arc method, and the gas mixture of using ammonia and helium makes nitrogen-doped graphene as reaction atmosphere.
4. method as claimed in claim 3 is characterized in that, the volume ratio of described helium and ammonia is 1: 1-1: 3.
5. method as claimed in claim 3 is characterized in that, the pressure of described reaction atmosphere is 380-760Torr.
6. as claim 3 or 5 described methods, it is characterized in that the electric current of described direct current arc discharge is 80-120A.
7. method as claimed in claim 3 is characterized in that, decolorizing carbon is removed in nitrogen-doped graphene calcination in air.
8. method as claimed in claim 7 is characterized in that, described calcination temperature is 400-500 ℃.
9. as claim 7 or 8 described methods, it is characterized in that described calcination time is 30-60 minute.
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| CN101913599A (en) * | 2010-08-13 | 2010-12-15 | 东华大学 | Method for preparing graphene nanobelt |
| CN102034975A (en) * | 2010-11-15 | 2011-04-27 | 中国科学院青岛生物能源与过程研究所 | Nitrogen-doped graphite carbon serving as anode material of lithium ion battery, and preparation method and application thereof |
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| CN102120572A (en) * | 2011-01-24 | 2011-07-13 | 南京大学 | Method for preparing nitrogen-doped graphene |
| CN102191476A (en) * | 2011-04-11 | 2011-09-21 | 兰州大学 | Method for preparing sulfur-doped graphene films |
| CN102306781A (en) * | 2011-09-05 | 2012-01-04 | 中国科学院金属研究所 | Doped graphene electrode material, macro preparation method and application of doped graphene electrode material |
| CN102671686A (en) * | 2012-05-31 | 2012-09-19 | 新疆大学 | Preparation of nitrogen-doping graphene and oxygen reduction performance thereof |
| CN102760866A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Preparation method of nitrogen-doped graphene |
| CN102936746A (en) * | 2012-10-29 | 2013-02-20 | 武汉理工大学 | Method for directly converting amorphous carbide into graphene under low-temperature and normal-pressure halogenation conditions |
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2009
- 2009-12-29 CN CN200910312486A patent/CN101717083A/en active Pending
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| CN101913599B (en) * | 2010-08-13 | 2012-11-07 | 东华大学 | Method for preparing graphene nanobelt |
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