CN103935982A - Graphene nanoribbon preparation method - Google Patents
Graphene nanoribbon preparation method Download PDFInfo
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- CN103935982A CN103935982A CN201310019484.XA CN201310019484A CN103935982A CN 103935982 A CN103935982 A CN 103935982A CN 201310019484 A CN201310019484 A CN 201310019484A CN 103935982 A CN103935982 A CN 103935982A
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Abstract
The present invention relates to a graphene nanoribbon preparation method, which comprises steps as follows: etching a metal substrate in an acid solution, then heating the etched metal substrate to between 600 and 900 DEG C under anaerobic conditions, exposing the metal substrate to ultraviolet radiation under the flux of a carbon-containing gas and a protective gas, after the reaction, obtaining carbon nanowalls on the surface of the metal substrate; mixing the carbon nanowalls and chloride intercalation agent at a mass ratio of 1:(0.8 to 1.2), heating the mixture to between 460 and 550 DEG C, and maintaining the temperature and reacting for 2 hours to 6 hours to obtain the chloride intercalated carbon nanowalls; and mixing the chloride intercalated carbon nanowalls with an ionic liquid at a volume/mass ratio of 1 g:10 ml to 100 ml, placing the mixture in a constant parallel magnetic field with intensity of 0.01 T to 1 T and carrying out centrifuging to obtain a reaction solution, and filtering reaction solution to obtain the graphene nanoribbons. The graphene nanoribbons prepared by the method mentioned above have high electrical conductivity.
Description
Technical field
The present invention relates to the synthetic field of nano-carbon material, particularly a kind of preparation method of graphene nanobelt.
Background technology
The kind of carbon material has the soccerballene (C of zero dimension
60deng), the carbon nanotube of one dimension, carbon nanofiber etc., the Graphene of two dimension, three-dimensional graphite, diamond etc., carbon nanometer wall (carbon nanowall, CNW) is the carbon nano structure with two-dimensional diffusion, its most typical pattern is just perpendicular to substrate material surface growth, thickness is greater than the wall shape structure of Graphene, completely different from the feature of soccerballene, carbon nanotube, Graphene etc., can be used as the raw material of other carbon material of preparation.
Before finding early than Graphene, people have just begun one's study the preparation of carbon nanometer wall.The preparation and the related application thereof that in 2002, just have reported in literature carbon nanometer wall, but no matter be early stage preparation method or nearest preparation method, all can relate under plasma atmosphere and react, can cause certain destruction to the structure of CNW.
Graphene nanobelt not only has the performance of Graphene, also possess some special performances, for example its length-to-diameter ratio is larger, can be up to thousands of times, and the specific conductivity of graphene nanobelt is higher, at integrated circuit connection, can replace copper conductor, further improve integrated level, also can carry out modification to its structure and be prepared into switch device.But at present because graphene nanobelt still exists a lot of defects, cause its specific conductivity lower.
Summary of the invention
Given this, be necessary to provide a kind of preparation method with the graphene nanobelt of high conductance.
A preparation method for graphene nanobelt, comprises the steps:
Metal substrate is placed in to the acid solution etching 0.5 minute ~ 10 minutes that concentration is 0.01mol/L ~ 1mol/L; Under oxygen free condition, the described metal substrate after etching is heated to 600 ℃ ~ 900 ℃, use metal substrate surface described in UV-irradiation, and pass into carbonaceous gas and protect gas, keep 30 minutes ~ 300 minutes, after reaction, on the surface of described metal substrate, obtain carbon nanometer wall; Wherein, the flow that passes into described carbonaceous gas is 10sccm ~ 1000sccm, and the throughput ratio of described carbonaceous gas and described protection gas is 2 ~ 10:1;
According to mass ratio, be 1:0.8 ~ 1.2, described carbon nanometer wall is mixed with muriate intercalator, be heated to 460 ℃ ~ 550 ℃ insulation reaction 2 hours ~ 6 hours, obtain muriatic intercalation carbon nanometer wall; And
According to mass volume ratio, it is 1 gram: 10 milliliters ~ 100 milliliters, described muriatic intercalation carbon nanometer wall is mixed with ionic liquid, and be placed in the constant parallel magnetic field centrifugal treating that magneticstrength is 0.01 tesla ~ 1 tesla, and obtain reaction solution, filter described reaction solution and obtain graphene nanobelt.
In an embodiment, before the described metal substrate heating after etching, also comprise the step that adopts successively deionized water, ethanol and acetone to clean to the described metal substrate after etching therein.
In an embodiment, described acid solution is hydrochloric acid soln, sulphuric acid soln or salpeter solution therein; The concentration of described acid solution is 0.1mol/L ~ 0.5mol/L; The etching period of described metal substrate in described acid solution is 60 seconds ~ 180 seconds.
Therein in an embodiment, described metal substrate is a kind of in iron foil, nickel foil and cobalt paper tinsel.
Therein in an embodiment, described carbonaceous gas is a kind of in methane, ethane, propane, acetylene and alcohol vapour; Described protection gas is at least one in helium, nitrogen and argon gas.
Therein in an embodiment, before described muriatic intercalation carbon nanometer wall is mixed with described ionic liquid, also comprise described muriatic intercalation carbon nanometer wall cleaned and dry step: adopt muriatic intercalation carbon nanometer wall described in washed with de-ionized water, through 80 ℃ ~ 100 ℃ vacuum-dryings to constant weight.
In an embodiment, described muriate intercalator is at least one in iron(ic) chloride, nickelous chloride, cupric chloride, cobalt chloride, Repone K, magnesium chloride, lead chloride, zinc chloride, calcium chloride and bariumchloride therein, described ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3, 5-methylimidazole fluoroform sulfimide and 1, 3-diethyl-4-methylimidazole fluoroform sulfimide, 1, at least one in 3-diethyl-5-Methylimidazole fluoroform sulfimide 1-ethyl-3-methylimidazole two cyaniding nitrogen.
In an embodiment, the condition of described centrifugal treating is therein: 1000 revs/min～10000 revs/min of rotating speeds, 10 minutes～100 minutes treatment time.
Therein in an embodiment, also comprise described graphene nanobelt cleaned and dry step: by described graphene nanobelt through adding machine solvent to refilter 3 times ~ 6 times, add again deionized water to filter until filtrate is detected without chlorion with Silver Nitrate, then by filter residue in 60 ℃ ~ 100 ℃ vacuum-dryings to constant weight.
In an embodiment, described organic solvent is 1-Methyl-2-Pyrrolidone or DMF therein.
The preparation method of above-mentioned graphene nanobelt, by preparing first voluntarily carbon nanometer wall as starting material, by the carbon nanometer wall that adopts etching metal substrate and two steps of photochemical catalysis chemical gaseous phase deposition to prepare, can effectively avoid preparing carbon nanometer wall and causing it destructurized under traditional using plasma atmosphere, and the carbon nanometer wall of preparing has uniform thickness, and structure is more complete; Then be prepared into after muriatic intercalation carbon nanometer wall, adopt ionic liquid to make solvent, and pass through in conjunction with under constant parallel magnetic field and centrifugal treating acting in conjunction, not only can realize and peel off fast intercalation carbon nanometer wall, can also effectively prevent from again reuniting after graphene nanobelt from peeling off, also guaranteed that the graphene nanobelt preparing has good integrity, made to use the graphene nanobelt that the preparation method of above-mentioned graphene nanobelt prepares to there is higher specific conductivity.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of the graphene nanobelt of an embodiment;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the carbon nanometer wall of embodiment 1 preparation;
Fig. 3 is the scanning electron microscope (SEM) photograph (SEM) of the graphene nanobelt of embodiment 1 preparation.
Embodiment
Below mainly in conjunction with the drawings and the specific embodiments the preparation method of graphene nanobelt is described in further detail.
As shown in Figure 1, the preparation method of the graphene nanobelt of an embodiment, comprises the steps:
Step S110: metal substrate is placed in to the acid solution etching 0.5 minute ~ 10 minutes that concentration is 0.01mol/L ~ 1mol/L; Under oxygen free condition, the metal substrate after etching is heated to 600 ℃ ~ 900 ℃, use UV-irradiation metal substrate surface, and pass into carbonaceous gas and protection gas, keep 30 minutes ~ 300 minutes, after reaction, on the surface of metal substrate, obtain carbon nanometer wall; Wherein, the flow that passes into carbonaceous gas is 10sccm(standard state milliliter per minute) ~ 1000sccm, and the throughput ratio of carbonaceous gas and protection gas is 2 ~ 10:1.After having reacted, stop passing into carbonaceous gas, stop heating and UV-irradiation, to be cooled to room temperature, on the surface of metal substrate, obtain carbon nanometer wall.Finally, the carbon nanometer wall on metal substrate surface is scraped, just obtained carbon nanometer wall powder.
By to metal substrate etching, make the etched surfaces of metal substrate produce defect, can effectively improve the surface tissue of metal substrate, make carbon nanometer wall energy enough in this metal substrate surface growth.Wherein, acid solution is the conventional dilute acid soln in this area, is preferably hydrochloric acid soln, sulphuric acid soln or salpeter solution.The concentration of acid solution is preferably 0.1mol/L ~ 0.5mol/L; And the etching period of metal substrate in acid solution be preferably 60 seconds ~ and 180 seconds.Preferred etching condition, can reach good etching effect, can improve the growth efficiency of carbon nanometer wall.
Wherein, metal substrate can be the conventional metal substrate in this area, is preferably a kind of in iron foil, nickel foil and cobalt paper tinsel.
Under the condition of anaerobic, preparing carbon nanometer wall, is to participate in reaction for fear of oxygen, and has influence on the growth of carbon nanometer wall, thereby a stable environment is provided to the growth of carbon nanometer wall.
By adopting UV-light to irradiate metal substrate surface, thereby play light-catalysed effect, can reduce the temperature of reaction, reduce energy consumption, reduced production cost.Wherein, providing the instrument of UV-irradiation can be ultraviolet source equipment.Wherein, ultraviolet light wavelength is 200 nanometer ~ 400 nanometers.
The more carbon source of growth needs of carbon nanometer wall; carbonaceous gas is 2 ~ 10:1 with the throughput ratio of protection gas, not only has more carbon source, and adopts the protection gas of this ratio as carrier gas; can dilute to a certain extent carbonaceous gas, be conducive to the growth of carbon nanometer wall.
By the carbon nanometer wall that adopts etching metal substrate and two steps of photochemical catalysis chemical gaseous phase deposition to prepare, can effectively avoid preparing carbon nanometer wall and causing it destructurized under traditional using plasma atmosphere, and the carbon nanometer wall of preparing has uniform thickness, and structure is more complete.And the carbon nanometer wall energy of preparation is enough vertically grown in etched metal substrate, and preparation technology is simple, and preparation condition is easy to control, and shortened etching period, thereby improved production efficiency.
Wherein, before the metal substrate heating after etching, also comprise the step that adopts successively deionized water, ethanol and acetone to clean to the metal substrate after etching.
Wherein, carbonaceous gas can be the conventional carbonaceous gas in this area, is preferably a kind of in methane, ethane, propane, acetylene and alcohol vapour.These several carbonaceous gass are simple in structure, are easy to cracking and deposition.
Wherein, protection gas can, for the conventional rare gas element in this area, be preferably at least one in helium, nitrogen and argon gas.
Step S120: be 1:0.8 ~ 1.2 according to mass ratio, carbon nanometer wall is mixed with muriate intercalator, be heated to 460 ℃ ~ 550 ℃ insulation reaction 2 hours ~ 6 hours, obtain muriatic intercalation carbon nanometer wall.
By first carbon nanometer wall and muriate intercalator being mixed with to muriatic intercalation carbon nanometer wall, can make carbon-coating spacing increase, thereby the reactive force of graphite layers is reduced, be conducive to follow-up peeling off.And by being first prepared into muriatic intercalation carbon nanometer wall, be the destruction for fear of carbon nano wall structure, be conducive to obtain after peeling off the integrity of the structure of graphene nanobelt.
Wherein, muriate intercalator is at least one in iron(ic) chloride, nickelous chloride, cupric chloride, cobalt chloride, Repone K, magnesium chloride, lead chloride, zinc chloride, calcium chloride and bariumchloride.Adopt these muriates to make preparation technology simple as intercalator, and to equipment require lowly, reduced preparation cost.
Step S130: be 1 gram according to mass volume ratio: 10 milliliters ~ 100 milliliters, muriatic intercalation carbon nanometer wall is mixed with ionic liquid, and be placed in the constant parallel magnetic field centrifugal treating that magneticstrength is tesla of 0.01 tesla (T) ~ 1 (T), obtain reaction solution, filtering reacting liquid obtains graphene nanobelt.
Wherein, constant parallel magnetic field refers to that the N utmost point in magnetic field is extremely parallel with S, and the magnetic field that magneticstrength is invariable, that is to say parallel magnetic field.By constant parallel magnetic field, charged particle is moved in magnetic field peel off muriatic intercalation carbon nanometer wall to obtain graphene nanobelt.Under constant parallel magnetic field and centrifugal treating acting in conjunction, can realize and peel off fast intercalation carbon nanometer wall, and under centrifugal treating, also can complete the collection of the graphene nanobelt preparing.
Wherein, the condition of centrifugal treating is: 1000 revs/min ~ 10000 revs/min of rotating speeds, 10 minutes～100 minutes treatment time.
By using ionic liquid to mix with muriatic intercalation carbon nanometer wall as solvent, can effectively prevent the reunion again of the graphene nanobelt for preparing.Wherein, ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid (EtMeImBF
4), 1-ethyl-3-methylimidazole fluoroform sulfimide (EtMeImN (CF
3sO
2)
2), 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF
3sO
3), 1-ethyl-3-methylimidazole trifluoroacetic acid (EtMeImN (CN)
2), 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon (EtMeImC (CF
3sO
2)
3), 1-ethyl-3-methylimidazole five acetyl fluoride imines (EtMeImN (C
2f
5sO
2)
2), 1-ethyl-3-methylimidazole two cyaniding nitrogen (EtMeImN (CN)
2), 1-ethyl-3,5-methylimidazole fluoroform sulfimide (1-Et-3,5-Me
2imN (CF
3sO
2)
2), 1,3-diethyl-4-methylimidazole fluoroform sulfimide (1,3-Et
2-4-MeImN (CF
3sO
2)
2) and 1,3-diethyl-5-Methylimidazole fluoroform sulfimide (1,3-Et
2-5-MeImN (CF
3sO
2)
2) at least one.
Wherein, before muriatic intercalation carbon nanometer wall is mixed with ionic liquid, also comprise muriatic intercalation carbon nanometer wall cleaned and dry step: adopt the muriatic intercalation carbon of washed with de-ionized water nanometer wall, through 80 ℃ ~ 100 ℃ vacuum-dryings to constant weight.
Wherein, after step S130, also comprise graphene nanobelt cleaned and dry step: by graphene nanobelt through adding machine solvent to refilter 3 times ~ 6 times, add again deionized water to filter until filtrate is detected without chlorion with Silver Nitrate, then by filter residue in 60 ℃ ~ 100 ℃ vacuum-dryings to constant weight.Wherein, organic solvent can be the conventional organic solvent in this area, is preferably 1-Methyl-2-Pyrrolidone (NMP) or DMF (DMF), 1-Methyl-2-Pyrrolidone (NMP) or DMF (DMF) can effectively be removed ionic liquid.
The preparation method of above-mentioned graphene nanobelt, by preparing first voluntarily carbon nanometer wall as starting material, by the carbon nanometer wall that adopts etching metal substrate and two steps of photochemical catalysis chemical gaseous phase deposition to prepare, can effectively avoid preparing carbon nanometer wall and causing it destructurized under traditional using plasma atmosphere, and the carbon nanometer wall of preparing has uniform thickness, and structure is more complete; Then be prepared into after muriatic intercalation carbon nanometer wall, adopt ionic liquid to make solvent, and pass through in conjunction with under constant parallel magnetic field and centrifugal treating acting in conjunction, not only can realize and peel off fast intercalation carbon nanometer wall, effectively prevent from again reuniting after graphene nanobelt from peeling off, also guaranteed that the graphene nanobelt preparing has good integrity, made to use the graphene nanobelt that the preparation method of above-mentioned graphene nanobelt prepares to there is higher specific conductivity.
The preparation method of above-mentioned graphene nanobelt is simple, and required equipment is all common chemical industry equipment, saves research and development equipment cost, is applicable to scale operation.
Be below specific embodiment part:
Embodiment 1
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) nickel foil is put into concentration and be the hydrochloric acid soln etching 0.5 minute of 1mol/L, after etching, with deionized water, ethanol, acetone, clean successively, (b) nickel foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, nickel foil is heated to 900 ℃, then open ultraviolet source equipment, make UV-irradiation on nickel foil surface, then pass into methane and nitrogen, keep 100 minutes, wherein, the flow that passes into steam methane is 200sccm, the throughput ratio of steam methane and nitrogen is 2:1, after having reacted, stop passing into steam methane, stop nickel foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into nitrogen, on nickel foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the carbon nanometer wall prepared of the present embodiment.As can be seen from the figure, carbon nanometer wall prepared by the present embodiment is perpendicular to the intensive growth of nickel foil, and even thickness, is about 30 nanometer ~ 60 nanometers.
(2) according to mass ratio, be 1:0.8, taking carbon nanometer wall prepared by step (1) mixes with iron(ic) chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 460 ℃, insulation reaction 2 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of iron(ic) chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water iron(ic) chloride, through vacuum drying oven, be dried to after constant weight in 80 ℃, obtain the intercalation carbon nanometer wall of pure iron(ic) chloride.
(3) according to mass volume ratio, be 1g:10ml, the intercalation carbon nanometer wall of dried iron(ic) chloride is joined 1-ethyl-3-methylimidazole Tetrafluoroboric acid (EtMeImBF is housed
4) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 1T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 1000 revs/min 100 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) to filter 6 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 60 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Fig. 3 is the scanning electron microscope (SEM) photograph (SEM) of the graphene nanobelt prepared of the present embodiment.As can be seen from the figure, the width distribution of graphene nanobelt prepared by the present embodiment is concentrated, and is about 20 nanometer ~ 40 nanometers, and length is about 2 microns ~ 20 microns, and length-to-diameter ratio is 50 ~ 1000.
Embodiment 2
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) iron foil is put into concentration and is the sulphuric acid soln etching 4 minutes of 0.5mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) iron foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, iron foil is heated to 600 ℃, then open ultraviolet source equipment, make UV-irradiation on iron foil surface, then pass into ethane steam and argon gas, keep 200 minutes, wherein, the flow that passes into ethane steam is 100sccm, ethane steam is 5:1 with the throughput ratio ratio of argon gas, after having reacted, stop passing into ethane steam, stop iron foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into argon gas, on iron foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from iron foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:0.9, taking carbon nanometer wall prepared by step (1) mixes with cupric chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 500 ℃, insulation reaction 3 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of cupric chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water cupric chloride, through vacuum drying oven, be dried to after constant weight in 90 ℃, obtain the intercalation carbon nanometer wall of pure cupric chloride.
(3) according to mass volume ratio, be 1g:100ml, the intercalation carbon nanometer wall of dried cupric chloride is joined 1-ethyl-3-methylimidazole fluoroform sulfimide (EtMeImN (CF is housed
3sO
2)
2) container in,, get 1L mixed solution and join in the supercentrifuge that capacity is 2L and build, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.5T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 2000 revs/min 50 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding DMF (DMF) filter 23 time, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven to dry constant weight at 80 ℃, obtains pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 3
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) cobalt paper tinsel is put into concentration and is the salpeter solution etching 10 minutes of 0.01mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) the cobalt paper tinsel after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, cobalt paper tinsel is heated to 700 ℃, then open ultraviolet source equipment, make UV-irradiation on cobalt paper tinsel surface, then pass into acetylene steam and argon gas, keep 300 minutes, wherein, the flow that passes into acetylene steam is 10sccm, the throughput ratio of acetylene steam and helium is 8:1, after having reacted, stop passing into acetylene steam, stop cobalt paper tinsel to heat, and close light source, question response chamber is cooled to after room temperature, stop passing into helium, on cobalt paper tinsel surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, it is 1: 1.2, taking carbon nanometer wall prepared by step (1) mixes with nickelous chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 480 ℃, insulation reaction 6 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of nickelous chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water nickelous chloride, through vacuum drying oven, be dried to after constant weight in 100 ℃, obtain the intercalation carbon nanometer wall of pure nickelous chloride.
(3) according to mass volume ratio, be 1g:50ml, the intercalation carbon nanometer wall of dried nickelous chloride is joined 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF is housed
3sO
3) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.1T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 5000 revs/min 30 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) to filter 5 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 100 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 4
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) nickel foil is put into concentration and is the hydrochloric acid soln etching 2 minutes of 0.2mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) nickel foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, nickel foil is heated to 750 ℃, then open ultraviolet source equipment, make UV-irradiation on nickel foil surface, then pass into propane vapor and nitrogen and argon gas mixed gas, keep 30 minutes, wherein, the flow that passes into propane vapor is 1000sccm, the throughput ratio of propane vapor and nitrogen and argon gas mixed gas is 10:1, after having reacted, stop passing into propane vapor, stop nickel foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into nitrogen and argon gas mixed gas, on nickel foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:1.0, taking carbon nanometer wall prepared by step (1) mixes with cobalt chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 550 ℃, insulation reaction 4 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of cobalt chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water cobalt chloride, through vacuum drying oven, be dried to after constant weight in 90 ℃, obtain the intercalation carbon nanometer wall of pure cobalt chloride.
(3) according to mass volume ratio, be 1g:20ml, the intercalation carbon nanometer wall of dried cobalt chloride is joined 1-ethyl-3-methylimidazole trifluoroacetic acid (EtMeImN (CN) is housed
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.05T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 8000 revs/min 10 minutes, obtain reaction solution, filtering reacting liquid, obtains the graphene nanobelt of the present embodiment, by graphene nanobelt through adding N, dinethylformamide (DMF) filter 23, then be filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 90 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 5
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) iron foil is put into concentration and is the sulphuric acid soln etching 5 minutes of 0.1mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) iron foil after cleaned is put into reaction chamber, and get rid of after the air in reaction chamber, iron foil is heated to 800 ℃, then open ultraviolet source equipment, make UV-irradiation on iron foil surface, then pass into alcohol vapour and argon gas, keep 50 minutes, wherein, the flow that passes into alcohol vapour is 500sccm, the throughput ratio of alcohol vapour and argon gas is 6:1, after having reacted, stop passing into argon gas, stop iron foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into argon gas, on iron foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from iron foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, it is 1: 1.1, taking carbon nanometer wall prepared by step (1) mixes with Repone K intercalator, insert in silica tube, sealed silica envelope, heats up after 520 ℃, insulation reaction 5 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of Repone K, adopt the intercalation carbon nanometer wall of washed with de-ionized water Repone K, through vacuum drying oven, be dried to after constant weight in 85 ℃, obtain the intercalation carbon nanometer wall of pure Repone K.
(3) according to mass volume ratio, be 1g:80ml, the intercalation carbon nanometer wall of dried Repone K is joined 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon (EtMeImC (CF is housed
3sO
2)
3) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.01T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 10000 revs/min 20 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) to filter 4 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 70 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 6
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) cobalt paper tinsel is put into concentration and is the salpeter solution etching 8 minutes of 0.4mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) the cobalt paper tinsel after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, cobalt paper tinsel is heated to 850 ℃, then open ultraviolet source equipment, make UV-irradiation on cobalt paper tinsel surface, then pass into steam methane and helium, keep 90 minutes, wherein, the flow that passes into steam methane is 800sccm, the throughput ratio of steam methane and helium is 4:1, after having reacted, stop passing into steam methane, stop cobalt paper tinsel to heat, and close light source, question response chamber is cooled to after room temperature, stop passing into helium, on cobalt paper tinsel surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:0.8, taking carbon nanometer wall prepared by step (1) mixes with sodium-chlor intercalator, insert in silica tube, sealed silica envelope, heats up after 530 ℃, insulation reaction 2 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of sodium-chlor, adopt the intercalation carbon nanometer wall of washed with de-ionized water sodium-chlor, through vacuum drying oven, be dried to after constant weight in 95 ℃, obtain the intercalation carbon nanometer wall of pure sodium-chlor.
(3) according to mass volume ratio, be 1g:60ml, the intercalation carbon nanometer wall of dried sodium-chlor is joined 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF is housed
3sO
3) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.2T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 2000 revs/min 40 minutes, obtain reaction solution, filtering reacting liquid, obtains the graphene nanobelt of the present embodiment, by graphene nanobelt through adding N, dinethylformamide (DMF) filters 5 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 60 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 7
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) nickel foil is put into concentration and be the hydrochloric acid soln etching 3 minutes of 0.25mol/L, after etching, with deionized water, ethanol, acetone, clean successively, (b) nickel foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, nickel foil is heated to 900 ℃, then open ultraviolet source equipment, make UV-irradiation on nickel foil surface, then pass into ethane steam and nitrogen, keep 120 minutes, wherein, the flow that passes into ethane steam is 300sccm, the throughput ratio of ethane steam and nitrogen is 3:1, after having reacted, stop passing into ethane steam, stop nickel foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into nitrogen, on nickel foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:1, taking carbon nanometer wall prepared by step (1) mixes with magnesium chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 490 ℃, insulation reaction 3 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of magnesium chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water magnesium chloride, through vacuum drying oven, be dried to after constant weight in 90 ℃, obtain the intercalation carbon nanometer wall of pure magnesium chloride.
(3) according to mass volume ratio, be 1g:40ml, the intercalation carbon nanometer wall of dried magnesium chloride is joined 1-ethyl-3-methylimidazole two cyaniding nitrogen (EtMeImN (CN) is housed
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.4T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 2500 revs/min 60 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) filter 23 time, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 100 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 8
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) iron foil is put into concentration and is the hydrochloric acid soln etching 4 minutes of 1mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) iron foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, iron foil is heated to 650 ℃, then open ultraviolet source equipment, make UV-irradiation on iron foil surface, then pass into acetylene steam and argon gas, keep 180 minutes, wherein, the flow that passes into acetylene steam is 200sccm, the throughput ratio of acetylene steam and argon gas is 2:1, after having reacted, stop passing into acetylene steam, stop iron foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into argon gas, on iron foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from iron foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, it is 1: 1.0, taking carbon nanometer wall prepared by step (1) mixes with lead chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 540 ℃, insulation reaction 6 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of lead chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water lead chloride, through vacuum drying oven, be dried to after constant weight in 100 ℃, obtain the intercalation carbon nanometer wall of pure lead chloride.
(3) according to mass volume ratio, be 1g:30ml, the intercalation carbon nanometer wall of dried lead chloride is joined 1-ethyl-3 are housed, 5-methylimidazole fluoroform sulfimide (1-Et-3,5-Me
2imN (CF
3sO
2)
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.8T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 1000 revs/min 80 minutes, obtain reaction solution, filtering reacting liquid, obtains the graphene nanobelt of the present embodiment, by graphene nanobelt through adding N, dinethylformamide (DMF) filters 6 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 80 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 9
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) cobalt paper tinsel is put into concentration and is the sulphuric acid soln etching 2 minutes of 0.3mol/L, after etching with cleaning with deionized water, ethanol, acetone successively, (b) the cobalt paper tinsel after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, cobalt paper tinsel is heated to 700 ℃, then open ultraviolet source equipment, make UV-irradiation on cobalt paper tinsel surface, then pass into propane vapor and helium, keep 240 minutes, wherein, the flow that passes into propane vapor is 50sccm, the throughput ratio of propane vapor and helium is 5:1, after having reacted, stop passing into propane vapor, stop cobalt paper tinsel to heat, and close light source, question response chamber is cooled to after room temperature, stop passing into helium, on cobalt paper tinsel surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:0.9, taking carbon nanometer wall prepared by step (1) mixes with zinc chloride intercalator, insert in silica tube, sealed silica envelope, heats up after 520 ℃, insulation reaction 5 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of zinc chloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water zinc chloride, through vacuum drying oven, be dried to after constant weight in 80 ℃, obtain the intercalation carbon nanometer wall of pure zinc chloride.
(3) according to mass volume ratio, be 1g:100ml, the intercalation carbon nanometer wall of dried zinc chloride is joined 1,3-diethyl-4-methylimidazole fluoroform sulfimide (1,3-Et is housed
2-4-MeImN (CF
3sO
2)
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 1T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 3000 revs/min 50 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) filter 23 time, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 90 ℃, is dried constant weight, obtain pure graphene nanobelt.And obtain the specific conductivity of the graphene nanobelt of the present embodiment, in Table 1.
Embodiment 10
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) nickel foil is put into concentration and be the salpeter solution etching 5 minutes of 0.5mol/L, after etching, with deionized water, ethanol, acetone, clean successively, (b) nickel foil after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, nickel foil is heated to 800 ℃, then open ultraviolet source equipment, make UV-irradiation on nickel foil surface, then pass into alcohol vapour and nitrogen, keep 300 minutes, wherein, the flow that passes into alcohol vapour is 20sccm, the throughput ratio of alcohol vapour and nitrogen is 8:1, after having reacted, stop passing into alcohol vapour, stop nickel foil heating, and close light source, question response chamber is cooled to after room temperature, stop passing into nitrogen, on nickel foil surface, obtain the carbon nanometer wall of the present embodiment, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:1.1, taking carbon nanometer wall prepared by step (1) mixes with bariumchloride intercalator, insert in silica tube, sealed silica envelope, heats up after 550 ℃, insulation reaction 4 hours, after reaction finishes, be cooled to room temperature, obtain the intercalation carbon nanometer wall of bariumchloride, adopt the intercalation carbon nanometer wall of washed with de-ionized water bariumchloride, through vacuum drying oven, be dried to after constant weight in 90 ℃, obtain the intercalation carbon nanometer wall of pure bariumchloride.
(3) according to mass volume ratio, be 1g:10ml, the intercalation carbon nanometer wall of dried bariumchloride is joined 1,3-diethyl-5-Methylimidazole fluoroform sulfimide (1,3-Et is housed
2-5-MeImN (CF
3sO
2)
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.1T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 5000 revs/min 10 minutes, obtain reaction solution, filtering reacting liquid, obtains the graphene nanobelt of the present embodiment, by graphene nanobelt through adding N, dinethylformamide (DMF) filters 4 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 70 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
Embodiment 11
Being prepared as follows of the graphene nanobelt of the present embodiment:
(1) prepare carbon nanometer wall: (a) cobalt paper tinsel is put into concentration and is the hydrochloric acid soln etching 1 minute of 0.05mol/L, after etching with cleaning with deionized water, ethanol, acetone successively; (b) the cobalt paper tinsel after cleaning is put into reaction chamber, and get rid of after the air in reaction chamber, cobalt paper tinsel is heated to 900 ℃, then open ultraviolet source equipment, make UV-irradiation on cobalt paper tinsel surface, then pass into steam methane and argon gas, wherein, the flow that passes into steam methane is 100sccm, and the throughput ratio of steam methane and argon gas is 10:1, keeps 30 minutes; After having reacted, stop passing into steam methane, stop cobalt paper tinsel to heat, and close light source, question response chamber is cooled to after room temperature, stops passing into argon gas, the carbon nanometer wall that obtains the present embodiment on cobalt paper tinsel surface, scrapes it from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
(2) according to mass ratio, be 1:0.2, take carbon nanometer wall and 50% ferric oxide prepared by step (1): 50% cupric oxide intercalator mixes, insert in silica tube, sealed silica envelope, heat up after 460 ℃, insulation reaction 2 hours, after finishing, reaction is cooled to room temperature, obtain 50% ferric oxide: the intercalation carbon nanometer wall of 50% cupric oxide, adopt washed with de-ionized water 50% ferric oxide: the intercalation carbon nanometer wall of 50% cupric oxide, through vacuum drying oven, be dried to after constant weight in 100 ℃, obtain 50% pure ferric oxide: the intercalation carbon nanometer wall of 50% cupric oxide.
(3) according to mass volume ratio, be 1g:50ml, by dried 50% ferric oxide: the intercalation carbon nanometer wall of 50% cupric oxide joins 1-ethyl-3-methylimidazole two cyaniding nitrogen (EtMeImN (CN) is housed
2) container in, getting 1L mixed solution joins in the supercentrifuge that capacity is 2L and builds, at whizzer top base two ends, add that magneticstrength is the constant parallel magnetic field of 0.01T, start magnetic field, whizzer, allow whizzer with the speed centrifugal treating of 8000 revs/min 100 minutes, obtain reaction solution, filtering reacting liquid, obtain the graphene nanobelt of the present embodiment, graphene nanobelt, through adding 1-Methyl-2-Pyrrolidone (NMP) to filter 5 times, then is filtered to filtrate AgNO with deionized water
3detection is without chlorion; Then the filter residue cleaning up is put in vacuum drying oven and at 100 ℃, is dried constant weight, obtain pure graphene nanobelt.And the specific conductivity of the graphene nanobelt of the present embodiment obtaining, in Table 1.
What table 1 represented is the specific conductivity of the graphene nanobelt of embodiment 1 ~ embodiment 11 preparations.
Table 1
From table 1, can learn, graphene nanobelt specific conductivity prepared by the preparation method of the graphene nanobelt of embodiment 1 ~ embodiment 11 is at least 0.7 * 10
5s/m, and apparently higher than tradition, prepare the specific conductivity 10 of graphene nanobelt prepared by the method for graphene nanobelt
4s/m, the graphene nanobelt that this explanation adopts the preparation method of graphene nanobelt of the present invention to prepare has good integrity.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for graphene nanobelt, is characterized in that, comprises the steps:
Metal substrate is placed in to the acid solution etching 0.5 minute ~ 10 minutes that concentration is 0.01mol/L ~ 1mol/L; Under oxygen free condition, the described metal substrate after etching is heated to 600 ℃ ~ 900 ℃, use metal substrate surface described in UV-irradiation, and pass into carbonaceous gas and protect gas, keep 30 minutes ~ 300 minutes, after reaction, on the surface of described metal substrate, obtain carbon nanometer wall; Wherein, the flow that passes into described carbonaceous gas is 10sccm ~ 1000sccm, and the throughput ratio of described carbonaceous gas and described protection gas is 2 ~ 10:1;
According to mass ratio, be 1:0.8 ~ 1.2, described carbon nanometer wall is mixed with muriate intercalator, be heated to 460 ℃ ~ 550 ℃ insulation reaction 2 hours ~ 6 hours, obtain muriatic intercalation carbon nanometer wall; And
According to mass volume ratio, it is 1 gram: 10 milliliters ~ 100 milliliters, described muriatic intercalation carbon nanometer wall is mixed with ionic liquid, and be placed in the constant parallel magnetic field centrifugal treating that magneticstrength is 0.01 tesla ~ 1 tesla, and obtain reaction solution, filter described reaction solution and obtain graphene nanobelt.
2. the preparation method of graphene nanobelt according to claim 1, is characterized in that, before the described metal substrate heating after etching, also comprises the step that adopts successively deionized water, ethanol and acetone to clean to the described metal substrate after etching.
3. the preparation method of graphene nanobelt according to claim 1, is characterized in that, described acid solution is hydrochloric acid soln, sulphuric acid soln or salpeter solution; The concentration of described acid solution is 0.1mol/L ~ 0.5mol/L; The etching period of described metal substrate in described acid solution is 60 seconds ~ 180 seconds.
4. the preparation method of graphene nanobelt according to claim 1, is characterized in that, described metal substrate is a kind of in iron foil, nickel foil and cobalt paper tinsel.
5. the preparation method of graphene nanobelt according to claim 1, is characterized in that, described carbonaceous gas is a kind of in methane, ethane, propane, acetylene and alcohol vapour; Described protection gas is at least one in helium, nitrogen and argon gas.
6. the preparation method of graphene nanobelt according to claim 1, it is characterized in that, before described muriatic intercalation carbon nanometer wall is mixed with described ionic liquid, also comprise described muriatic intercalation carbon nanometer wall cleaned and dry step: adopt muriatic intercalation carbon nanometer wall described in washed with de-ionized water, through 80 ℃ ~ 100 ℃ vacuum-dryings to constant weight.
7. the preparation method of graphene nanobelt according to claim 1, it is characterized in that, described muriate intercalator is at least one in iron(ic) chloride, nickelous chloride, cupric chloride, cobalt chloride, Repone K, magnesium chloride, lead chloride, zinc chloride, calcium chloride and bariumchloride; Described ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3,5-methylimidazole fluoroform sulfimide, 1, at least one in 3-diethyl-4-methylimidazole fluoroform sulfimide and 1,3-diethyl-5-Methylimidazole fluoroform sulfimide.
8. the preparation method of graphene nanobelt according to claim 1, is characterized in that, the condition of described centrifugal treating is: 1000 revs/min～10000 revs/min of rotating speeds, 10 minutes～100 minutes treatment time.
9. the preparation method of graphene nanobelt according to claim 1, it is characterized in that, also comprise described graphene nanobelt cleaned and dry step: by described graphene nanobelt through adding machine solvent to refilter 3 times ~ 6 times, add again deionized water to filter until filtrate is detected without chlorion with Silver Nitrate, then by filter residue in 60 ℃ ~ 100 ℃ vacuum-dryings to constant weight.
10. the preparation method of graphene nanobelt according to claim 9, is characterized in that, described organic solvent is 1-Methyl-2-Pyrrolidone or DMF.
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