CN102408107A - Method for preparing high-quality graphene - Google Patents
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- CN102408107A CN102408107A CN2010102918912A CN201010291891A CN102408107A CN 102408107 A CN102408107 A CN 102408107A CN 2010102918912 A CN2010102918912 A CN 2010102918912A CN 201010291891 A CN201010291891 A CN 201010291891A CN 102408107 A CN102408107 A CN 102408107A
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Abstract
The invention discloses a method for preparing high-quality graphene, which is characterized by comprising the following steps of: reacting active metals with low-carbon halogenated hydrocarbons or absolute ethyl alcohols in a certain time at a certain temperature so as to generate new ecological carbon; then, restructuring the new ecological carbon so as to obtain graphene; and finally, carrying out purification on the obtained graphene so as to obtain high-quality graphene. Compared with the traditional chemical stripping method for preparing graphene, the method disclosed by the invention is simple in operation and low in cost, and can prepare less-defect, good-electroconductivity and high-quality graphene. The graphene prepared by using the method disclosed by the invention can have a broad application prospect in the fields of photoelectric devices such as CIGS (copper indium gallium selenide), CdTe(cadmium telluride) and dye sensitized solar cells and the like, flat-panel displays, super capacitors, field emission materials, lithium ion batteries, and the like.
Description
Technical field
The present invention relates to a kind of high quality graphene preparation method, belong to the materials chemistry preparing technical field.
Background technology
Graphene (graphene) is that what to be made up of carbon atom is the monoatomic layer material with bi-dimensional cellular shape structure of elementary cell with the phenyl ring, is the elementary cell that makes up other dimension blacking (like zero dimension soccerballene, one dimension carbon nanotube and three-dimensional graphite).Graphene has excellent electricity, calorifics and mechanical property, and for example, Graphene has 10 times of high carrier mobilities to commercial silicon chip and (reaches 15000cm
2V
-1s
-1), and current carrier shows the ballistic transport characteristic of tangible ambipolar field performance characteristic and room temperature submicron-scale, and high and continuously adjustable carrier concentration (can reach 10
13Cm
-2); The intensity of Graphene can reach 130GPa, is more than 100 times of steel; The thermal conductivity of Graphene can reach 5000W/mK, is 3 times of pure diamond under the room temperature; Graphene all has excellent perviousness or the like near infrared, visible light and UV-light.Therefore, Graphene is expected the acquisition widespread use in fields such as high-performance nanometer electronic device, matrix material, field emmision material, display device, gas sensor and energy storages.Because its unique two-dirnentional structure and excellent crystallography quality, Graphene have contained abundant and novel physical phenomenon, therefore, Graphene becomes chemistry, Materials science and Condensed Matter Physics field hot research in recent years rapidly.
At present, the application of Graphene relates generally to two fields of physics and chemistry, and physical study mainly concentrates on characteristic electron and mechanical characteristics, and chemical research mainly contains preparation, surface and chemically modified.And the large-scale application of Graphene is needed badly and is realized extensive, as can repeatedly to prepare smooth, even, thickness and controllable size high quality grapheme material.People's original adoptions such as Geim " micromechanical forces disintegrating method ", promptly through mechanical force from graphite crystal sur-face peeling Graphene lamella and transfer on the carrier surfaces such as silicon oxide.Though this method can prepare the Graphene of micron size, its poor controllability yields poorly.Through heating SiC (0001) single-crystal surface extending and growing graphene structure, this Graphene that supports can directly be made electron device through photoetching process.But because reconstruct takes place easily on SiC plane of crystal surface in high-temperature heating process, cause surface tissue comparatively complicated, be difficult to obtain the Graphene of big area, uniform in thickness.Chemical Vapor deposition process (CVD) is to be substrate with metal single crystal or polycrystalline mf, expose in its surface and the pyrolytic decomposition carbon compound can generate graphene-structured, but the metal substrate difficulty of the Graphene of growing is removed.What the application of preparation Graphene was maximum at present is the chemical stripping method, promptly passes through strong oxidizer graphite oxidation, forms graphene oxide, then with strong reductive agent graphene oxide is reduced into Graphene again.Employed strong oxidizer in the process of chemical stripping can destroy Graphene planar carbon skeleton, produces defective, causes the graphene conductive degradation of gained.Therefore, how the high-quality Graphene of preparation of simple controllable magnanimity is a big difficult point and a focus of research at present.
Summary of the invention
The object of the present invention is to provide a kind of method that can magnanimity prepares the high quality Graphene.The basic ideas of invention are: utilize active metal and absolute ethyl alcohol or low-carbon (LC) halohydrocarbons reaction to generate the carbon of nascent state, the carbon of nascent state reconstitutes Graphene.Be equipped with the Graphene method with traditional chemical stripping legal system and compare, few, the good conductivity of Graphene defective that the present invention obtains, and simple to operate, step is few, preparation cost is very low, can magnanimity preparation.
The present invention is with one or more the combination in active metal lithium, potassium, sodium, magnesium, calcium, strontium, barium, the lanthanum etc.; The low-carbon (LC) halohydrocarbon is the one or more combination raw material in trichloromethane, tetracol phenixin, carbon tetrabromide, Perchlorobenzene, Sesquichloratum, heptachloropropane and the absolute ethyl alcohol; Under inert atmosphere protection, adopt the solvent thermal synthesizing graphite alkene.Describe the present invention below in detail.
A) Graphene is synthetic
One or more combination in the combination of one or more in active metal lithium, sodium, potassium, magnesium, calcium, strontium, barium, the lanthanum and low-carbon (LC) halohydrocarbon tetracol phenixin, carbon tetrabromide, trichloromethane, Perchlorobenzene, Sesquichloratum, heptachloropropane or the absolute ethyl alcohol is that raw material reacts in inert atmosphere such as argon gas, nitrogen etc.; Reaction times is 0.5-60 hour; Temperature is 60-500 ℃; Reaction times and temperature are all different according to the kind of metal and carbon source, and the mol ratio of active metal and carbon source is 0.5-6.
Reaction vessel is the high voltage bearing closed reactor of ability, will tighten reaction kettle before the reaction, in case the gas leakage that relates in the reaction process.
When metal and should be rapidly heated after halohydrocarbon contacts (within about 60min) to temperature required and insulation 5-50h.
B) purification of Graphene
After reaction finishes, contain the by products such as metal halide of unreacted halohydrocarbon and generation in the Graphene that obtains.Therefore, need purify to the Graphene that obtains.
1. add a large amount of acetone in the mixture that obtains toward reacting earlier, and fully stir 0.5-1h so that acetone fully dissolves halohydrocarbon.The amount of required acetone changes according to the amount of added halohydrocarbon in the reaction process.
2. obtain filter cake in the filtration step mixed solution 1., and filter cake is washed out with deionized water.
3. the past 2. middle x that adds 20-200mL is the hydrochloric acid of 10%-35%, is heated to 60-80 ℃, fully stirs.The purpose that adds hydrochloric acid here is in order better to remove the alkali metal halide of the generation in the reaction process.
4. 3. mixed solution is filtered, and with a large amount of deionized water wash.
5. vacuum-drying obtains the Graphene sample, and the vacuum-drying temperature is 60-100 ℃, vacuum-drying time 6-10h.
6. step promptly gets the Graphene product after 5. the sample ultrasonic 10-60min of gained disperses.
For the characteristic of the Graphene that characterizes method provided by the invention preparation, the spy has carried out performance characterization and has prepared the work that Graphene carries out the performance comparison with chemical peeling:
(1) pattern of Graphene and structural characterization
To gained Graphene sample of the present invention through ESEM (SEM, LEO-1530VP) and the pattern of transmission electron microscope (JEM 2010) observation sample; Observe the surface and the thickness of graphene platelet through AFM (AFM, Japanese Seiko II SPI3800V & spa300HV type).
Characterize the structure of Graphene with Raman spectrum (Renishaw invia Raman Microscope, excitation wavelength is 514.5nm).
Each element relative content ratio and chemical combination attitude thereof with x-ray photoelectron spectroscopy (XPS) analytic sample surface.Instrument is the PHI 5000C ESCA System of U.S. PHI company; The employing condition is the magnesium target, high pressure 14.0kV, and power 250W, vacuum is superior to 1 * 10
-8Torr.The RBD147 data collecting card of employing U.S. RBD company and AugerScan3.21 software is the full scan spectrum (lead to and can be 93.9eV) of 0～1200eV of collected specimens respectively; Then gather the narrow scan spectrum (lead to and to be 23.5eV) of each element related track, and adopt AugerScan3.21 software to carry out data analysis.With C1s=284.6eV is that benchmark carries out the bound energy correction.
Characterize the electric property of Graphene with electrochemical workstation (CHI 660B) test cross flow impedance.
Its electroconductibility that compares with Graphene of the present invention and chemical stripping method (being the Hummers method) preparation.
(2) the chemical stripping legal system is equipped with Graphene
Prepare the electroconductibility of Graphene for contrast the present invention; Prepare graphene oxide with the Hummers method; Promptly obtain graphite oxide with the vitriol oil, SODIUMNITRATE and potassium permanganate oxidation flake graphite; Obtain graphene oxide [W.S.Hummers, etc.J.Am.Chem.Soc. (1958) 1339] with ultrasonic peeling off again.Redox graphene is come with the method for high temperature pyrolysis in the back.Like accompanying drawing 7 [D.Li, etc.Nature Nanotech.3 (2008) 101-105.] (seeing embodiment 1 for details).
The present invention has simple to operate, and is with low cost, can obtain that defective is few, good conductivity, Graphene that quality is high.The Graphene that the present invention prepares can have broad application prospects in the fields such as FPD, ultracapacitor, field emmision material, lithium ion battery at solar cells such as photoelectric device such as copper-indium-galliun-selenium, cadmium telluride, dye sensitizations.
Description of drawings
The stereoscan photograph of Fig. 1 Graphene as can be seen from the figure is to spend the same sheet structure.
Fig. 2 AFM (AFM) figure, Fig. 2 (a) is the structure of large stretch of Graphene, its size can find out that from Fig. 2 (b) its thickness of Graphene that obtains is about 0.8nm between 15-20 μ m, be single-layer graphene.
Fig. 3 transmission electron microscope photo can know that the sample that obtains is a sheet structure from figure (a) (c), and Fig. 3 (b) is the high-resolution electron microscopy photo, therefrom can find out Graphene number of plies n＜3 that obtain.
Fig. 4 Raman spectrum, the Raman spectrogram of the Graphene that Fig. 4 (a) chemical stripping method obtains, the ratio I of G peak and D peak intensity
G/ I
D～1.1.Figure (b) is the Raman spectrogram of the Graphene that obtains for the present invention.
Fig. 5 is the narrow scan spectrum of carbon 1s track.
Graphene that Fig. 6 the present invention obtains and the correlated alternating-current impedance figure of Graphene that obtains with the chemical stripping method.The Graphene alternating-current impedance curve that curve 1 obtains for chemical stripping, the 2 Graphene alternating-current impedance curves that make for the present invention.
Fig. 7 diagram Hummer legal system is equipped with graphene oxide and further is reduced to Graphene.
Embodiment
Introduce embodiments of the invention below, to understanding of the present invention, but the present invention is limited to embodiment absolutely not with further increase.
Embodiment 1:
Synthesizing of Graphene
In kerosene, take out potassium metal, the glove box of putting into anhydrous and oxygen-free (contains H
2O＜0.1ppm, O
2＜0.1ppm) in, to use after convenient.In glove box, get the potassium of 2.0g, that puts into volume and be 30mL has a teflon-lined stainless steel cauldron, adds the tetracol phenixin of 10mL.Tighten sealing rapidly.Reaction kettle is put into baking oven, in 60min, be warming up to 120 ℃ rapidly, insulation 8h.
The purifying of Graphene
Reaction naturally cools to room temperature after finishing.Open reaction kettle, the acetone toward inside liner adding 100mL all washes out reaction product to the 200mL beaker, fully stirs 30min.Filter.Cakes with deionized water is washed out, add 10% the hydrochloric acid soln of 100mL, be heated to 60 ℃, fully stir 30min.Filter, and with the deionized water wash of about 1L, fully to remove the by product Repone K that produces in the reaction process.The product that obtains at 80 ℃ of following vacuum-drying 8h, and is promptly got Graphene product 1.2g through the 30min ultra-sonic dispersion.
The pattern of Graphene and structural characterization
Can obtain the sheet structure that is of Graphene sample from SEM and TEM characterization result (respectively shown in accompanying drawing 1 and 3).After ultrasonic 40min, characterize its thickness with AFM (as shown in Figure 2), be about 0.8nm, be single-layer graphene.Raman spectrum is one of effective means that characterizes the Graphene quality, and high-quality Graphene has the D peak a little less than very strong G peak has with the 2D peak.Can know that from Fig. 4 the Graphene that the present invention obtains has the characteristic of high quality Graphene, and has very strong D peak with the Graphene that chemical stripping obtains, explain that Graphene quality that the present invention obtains obtains far above traditional chemical stripping method.From the narrow spectrum scanning of the C (1s) of XPS (accompanying drawing 5) but the Graphene that obtains of knowledge capital invention be that carbon by nascent state reconstitutes and forms.
The sign of chemical property
We characterize the conductivity of product through the test alternating-current impedance.Be to make the alternating-current impedance working electrode, we mix graphene powder and N-Methyl pyrrolidone (NMP) becomes the homogeneous of 50mg/ml slurry, is coated on adhesive tape with glass stick and produces isolation region (1cm
2) conductive glass FTO (on 15 Ω/square), it is the film of 4 μ m that oven dry forms thickness, starches with silver and draws lead.During test EIS, be counter electrode with the Pt electrode, SCE (SCE) is a reference electrode, with the K of the 10mmol/L in the KCl solution of 0.1mol/L
3[Fe (CN)
6]/K
4[Fe (CN)
6] (1: 1) be the redox probe, the perturbation condition is 5mV, 100mHz～100KHz.
The chemical stripping legal system is equipped with the preparation of Graphene
The electroconductibility of the excellence of the Graphene for preparing for outstanding the present invention, the application also is equipped with Graphene with the chemical stripping legal system, i.e. Hummers method, its preparating mechanism is as shown in Figure 7.The preparation process comprises following four steps:
The first step is got the flake graphite of 1.0g, the SODIUMNITRATE (NaNO of 1g
3) and the vitriol oil of 46ml in ice bath, stir 15min, add the potassium permanganate (KMnO of 6g slowly
4).After the mixing, system transferred in 35 ± 5 ℃ the water-bath, stirred 6 hours, form the mixture of the mud appearance of black.
Second step, under agitation condition, the deionized water of adding 20ml in the mixture, system temperature is raised to 90 ± 5 ℃.The water dilution that adds 200ml behind the 30min.The H that adds 6ml
2O
2(30%) the excessive KMnO of reduction
4, the system color is a glassy yellow by brown stain.
In the 3rd step, the above-mentioned solution that obtains is filtered, and wash with a large amount of water (being about 2L).The filter cake that obtains is dispersed in the deionized water again, ultra-sonic dispersion 20min.With the centrifugal 5min under low speed 1000rpm of whizzer elder generation, to remove the graphite that does not react completely, the water in the graphene oxide is removed at high speed 12000rpm in the back.Promptly get graphene oxide behind 100 ℃ of dry 8h of vacuum again.
The 4th the step, with the graphene oxide that obtains at H
2/ Ar (contains 5% H
2) be heated to 1000 ℃ in the gas mixture, insulation 6h, reduction obtains Graphene.
Can find out ratio I from Fig. 4 (a) with G peak intensity the Graphene of chemical stripping method preparation
G/ I
D～1.1; And, can find out G peak position～1580cm from the Raman spectrogram of the Graphene of Fig. 4 (b) the present invention preparation
-1, the position～2700cm at 2D peak
-1, the G peak obviously is better than D peak (～1350cm
-1), the ratio I of intensity
G/ I
D～2.5, explain that the Graphene defective that is obtained by the present invention is few.
Can know that from Fig. 5 its bound energy is 284.5eV, this is consistent with the bound energy of carbon atom in the Graphene.What can prove further thus that the present invention obtains is Graphene.
Figure can know from Fig. 6 alternating-current impedance, 1 Graphene that obtains for the chemical stripping method wherein, the alternating-current impedance figure of 2 Graphenes that obtain for the present invention.The corresponding zone of semicircle among the figure is corresponding to the alternating-current impedance of Graphene sample, and this resistance that shows the Graphene that the present invention obtains is less than the Graphene that the chemical stripping method obtains, and explains that the Graphene defective that the present invention obtains is few, quality is high.
Embodiment 2:
In glove box, get the carbon tetrabromide (CBr of 4.5g
4) be dissolved in the benzene of 20mL, put into the polytetrafluoroethyllining lining that volume is 30mL, get the potassium of 2.0g.Put into stainless steel cauldron rapidly, tighten sealing.Reaction kettle is put into baking oven, in 60min, be warming up to 160 ℃ rapidly, insulation 12h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 3:
In glove box, get the trichloromethane of 8mL, put into the polytetrafluoroethyllining lining that volume is 30mL, get the potassium of 2.0g.Put into stainless steel cauldron rapidly, tighten sealing.Reaction kettle is put into baking oven, be warming up to 60 ℃ rapidly, insulation 10h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 4:
In glove box, get the sodium of 2.0g and the carbon tetrabromide of 4.5g, put into the polytetrafluoroethyllining lining that volume is 30mL.Put into stainless steel cauldron rapidly, tighten sealing.Reaction kettle is put into baking oven, in 60min, be warming up to 250 ℃ rapidly, insulation 60h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Potassium among the embodiment 1 changes calcium into, and difference is that temperature of reaction is 160 ℃, and the reaction times is 12h.Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 6
Potassium among the embodiment 2 changes calcium into, and difference is that temperature of reaction is 200 ℃, and the time is 12h.Purifying and electrochemical property test process such as embodiment 1 to product.
Embodiment 7
In glove box, get potassium and the 1.5g sodium of 1.0g, that puts into volume and be 30mL has a teflon-lined stainless steel cauldron, adds the tetracol phenixin of 10mL.Tighten sealing rapidly.Reaction kettle is put into baking oven, in 60min, be warming up to 140 ℃ rapidly, insulation 10h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 8
In glove box, get the potassium of 2.0g, that puts into volume and be 30mL has a teflon-lined stainless steel cauldron, adds the carbon tetrachloride solution that 5.0mL is dissolved with the carbon tetrabromide of 3.0g.Tighten sealing rapidly.Reaction kettle is put into baking oven, in 60min, be warming up to 180 ℃ rapidly, insulation 18h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 9
In glove box, get potassium and the 1.0g sodium of 1.5g, that puts into volume and be 30mL has a teflon-lined stainless steel cauldron, adds the carbon tetrachloride solution that 5.0mL is dissolved with the carbon tetrabromide of 2.0g.Tighten sealing rapidly.Reaction kettle is put into baking oven, in 60min, be warming up to 200 ℃ rapidly, insulation 24h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
In glove box, get the lithium of 1.5g, put into the stainless steel cauldron that volume is 30mL, add the carbon tetrachloride solution of 5.0mL.Tighten sealing rapidly.Reaction kettle is put into retort furnace, in 100min, be warming up to 400 ℃, insulation 8h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 11
In glove box, get the potassium of 2.0g, put into the stainless steel cauldron that volume is 30mL, add the Perchlorobenzene of 4.0g.Tighten sealing rapidly.Reaction kettle is put into retort furnace, in 100min, be warming up to 400 ℃ rapidly, insulation 14h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 12
Get the Perchlorobenzene (C of 2.5g
6Cl
6) be dissolved in the benzene of 20mL, transfer in the 30mL stainless steel cauldron the past potassium metal that wherein adds 2.5g in glove box.Reaction kettle is put into retort furnace, in 100min, be warming up to 350 ℃ rapidly, insulation 8h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 13
In glove box, get the sodium of 2.0g, put into the stainless steel cauldron that volume is 30mL, add the absolute ethyl alcohol of 5mL.Tighten sealing rapidly.Reaction kettle is put into retort furnace, in 60min, be warming up to 300 ℃ rapidly, insulation 60h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 14
In glove box, get 1.0g magnesium powder, put into the stainless steel cauldron that volume is 30mL, add the absolute ethyl alcohol of 10mL.Tighten sealing rapidly.Reaction kettle is put into retort furnace, in 100min, be warming up to 500 ℃ rapidly, insulation 12h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
In glove box, get 2.0g magnesium powder, put into the stainless steel cauldron that volume is 30mL, add the tetracol phenixin of 4.5mL.Tighten sealing rapidly.Reaction kettle is put into retort furnace, in 60min, be warming up to 500 ℃ rapidly, insulation 16h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 16
Get the Sesquichloratum (C of 0.6g
2Cl
6) be dissolved in the benzene of 20mL, transfer in the 30mL stainless steel cauldron the past barium metal that wherein adds 2.0g in glove box.Reaction kettle is put into retort furnace, in 60min, be warming up to 100 ℃ rapidly, insulation 3h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 17
Get the heptachloropropane (C of 1.0g
3HCl
7) be dissolved in the CCl of 15mL
4In, transfer in the stainless steel cauldron of 30mL the past lanthanum that wherein adds 2.8g in glove box.Reaction kettle is put into the retort furnace that has been warming up to 500 ℃ rapidly, insulation 0.5h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Embodiment 18:
In kerosene, take out sodium Metal 99.5, put into glove box after with filter paper kerosene being blotted, for future use.In glove box, get the sodium of 2.0g, put into the polytetrafluoroethyllining lining that volume is 30mL, add the tetracol phenixin of 5mL.Put into stainless steel cauldron rapidly, tighten sealing.Reaction kettle is put into baking oven, in 60min, be warming up to 300 ℃ rapidly, insulation 48h.
Edulcoration purification and electrochemical property test process such as embodiment 1.
Claims (6)
1. high quality preparation method of graphene; It is characterized in that utilizing active metal and low-carbon (LC) halohydrocarbon or absolute ethyl alcohol reaction to generate the carbon of nascent state; The carbon of nascent state reconstitutes Graphene; At last the purified technology of Graphene that constitutes is processed, the mol ratio of described active metal and carbon source is 0.5-6.
2. by the described method of claim 1, it is characterized in that the synthetic purification with the synthetic Graphene that comprises Graphene divides two big steps:
A) Graphene is synthetic
1. one or more combination or the absolute ethyl alcohol in the combination of one or more in active metal lithium, sodium, potassium, magnesium, calcium, strontium, barium, the lanthanum and low-carbon (LC) halohydrocarbon tetracol phenixin, carbon tetrabromide, trichloromethane, Perchlorobenzene, Sesquichloratum, the heptachloropropane is raw material; In argon gas or nitrogen inert atmosphere, react; Temperature is 60-500 ℃, and reaction times and temperature are all different according to the kind of metal and carbon source;
2. reaction vessel is high voltage bearing closed reactor, before the reaction tightens reaction kettle, in case the gas leakage that relates in the reaction process; When metal be rapidly heated after halohydrocarbon contacts to temperature required and insulation;
B) purification of synthetic Graphene
1. a large amount of acetone of adding in the mixture that obtains toward reactions step a earlier, and fully stir 0.5-1h so that acetone fully dissolves unreacted low-carbon (LC) halohydrocarbon; The amount of required acetone changes according to the amount of added halohydrocarbon in the reaction process;
2. filtration step mixed solution 1. obtains filter cake, and with deionized water filter cake is washed out;
3. be the hydrochloric acid of 10%-35% toward the 2. middle x that adds 20-200mL of step, be heated to 60-80 ℃, stir, to remove the alkali metal halide of the generation in the reaction process;
4. step mixed solution is 3. filtered, and use deionized water wash;
5. vacuum-drying obtains Graphene, and the vacuum-drying temperature is 60-100 ℃;
6. with step 5. the Graphene of gained process high-quality Graphene through ultra-sonic dispersion.
3. by the described method of claim 2, it is characterized in that in the Graphene synthesis step:
A) the step reaction times 1. is 0.5-60 hour;
B) step 2. in the time of being rapidly heated be in the 60min;
C) to be warming up to temperature required soaking time in 2. be 5-50 hour to step.
4. by the described method of claim 2, it is characterized in that in the purification step of Graphene:
A) the 3. middle time 0.5-1h that stirs of step;
B) the 5. middle vacuum-drying time of step is 6-10 hour;
C) the 6. middle ultra-sonic dispersion time of step is 10-60min.
5. by claim 1 or 2 described methods, it is characterized in that prepared Graphene is a single-layer graphene, thickness is 0.8nm, is of a size of 10-20 μ m.
6. by claim 1 or 2 described methods, it is characterized in that the G peak intensity obviously is better than D peak, I in the Raman spectrum of prepared Graphene
G/ I
D=2.5, the Graphene defective that characterizes preparation is few.
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