CN102431999A - Method for preparing high-quality graphene - Google Patents
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Abstract
The invention relates to the field of graphene, and specifically relates to a method for preparing high-quality graphene. According to the invention, a graphite intercalation compound with a halogen or a metal halide as an intercalating agent is adopted as a raw material; expansion is carried our by using an oxalic acid solution or a hydrogen peroxide solution; and the material is subject to ultrasonic exfoliation in a solvent, such that the high-quality graphene is prepared. The method comprises specific steps that: after the graphite intercalation process, graphite intercalation compound powder is added into an oxalic acid solution or a hydrogen peroxide solution; expansion is carried out, such that highly expanded worm-shaped graphene aggregates are obtained; the worm-shaped graphene aggregates are subject to an ultrasonic oscillation in organic solvents such as alcohol and ketone, or an aqueous solution of a surfactant, such that exfoliation is realized, and a graphene dispersion liquid is obtained; the graphene dispersion liquid is dried, the solvent is removed, such that high-quality graphene powder can be obtained. The method provided by the invention is simple and is easy to control. With the method, high-efficiency, high-yield and low-cost productions of high-quality graphene can be realized; problems in current graphene preparation technologies of high cost, low yield, and poor quality can be solved.
Description
Technical field
The present invention relates to the Graphene field, being specially a kind of is that the graphite intercalation compound of intercalator is a raw material with halogen or metal halide, expand in oxalic acid or the superoxol with solvent in ultrasonic peel off to combine prepare the method for high quality Graphene.
Background technology
Since 2004 came to light, Graphene received much concern as a kind of new carbon.It is the accurate two dimensional crystal material that a kind of complete thickness that is made up of the carbon atom of sp2 hydridization is merely monoatomic layer or several monoatomic layers; Have excellent performance such as high light transmittance and electroconductibility, high-specific surface area, HS and snappiness, be expected acquisition widespread use in fields such as high-performance nanometer electronic device, photoelectric device, gas sensor, matrix material, field emmision material and energy storages.But the low cost of high quality Graphene, a large amount of preparation are still faced adverse conditions, and have restricted this Development of Materials and application.
At present, the preparation of a large amount of Graphenes mainly is based on the Hummer method graphite is carried out oxide treatment, obtain graphite oxide after, it is peeled off obtain graphene oxide again, handle obtaining Graphene at last through reduction.Because oxidising process is understood the structure of havoc Graphene lamella usually, though handle through reduction, still there is bigger gap in each item performance index of gained grapheme material with high-quality Graphene.In addition, the oxidising process of graphite needs a large amount of strongly-acid oxygenants such as the vitriol oil, concentrated nitric acid, dichromic acid and potassium permanganate, SODIUMNITRATE etc. usually; And need pyroprocessing in the order reduction process or use toxic chemical substances such as hydrazine, dimethylhydrazine, not only energy consumption is big, efficient is low, cost is high but also contaminate environment.Therefore, press for exploitation a kind of can be in a large number, the novel method of low cost and eco-friendly preparation high quality Graphene.
Summary of the invention
The object of the present invention is to provide a kind of a large amount of, low-cost, high quality preparation method of graphene, solve problems such as the cost that exists in the prior art is high, productive rate is low, of poor quality.
Technical scheme of the present invention is:
A kind of method for preparing the high quality Graphene is that the graphite intercalation compound of intercalator is a raw material with halogen or metal halide, expand in oxalic acid or the superoxol with solvent in ultrasonic peel off to combine prepare the high quality Graphene.At first the graphite intercalation compound powder is joined in the oxalic acid or superoxol of concentration (massfraction) more than 15wt%; Under 0～100 ℃ condition, handle then and carried out expansion process in 0.5～24 hour, obtain the quasiflake graphite alkene aggregate of high level expansion.And then; With gained quasiflake graphite alkene aggregate after the expansion process in the aqueous solution or organic solvent solution of organic solvent or various tensio-active agents; Ultrasonic oscillation was handled 1 minute～5 hours, realized peeling off, and Graphene is dispersed in forms Graphene solution in the solvent.After utilizing spraying drying or cryodesiccated method to remove organic solvent or various tensio-active agent, can obtain high-quality Graphene powder.
With halogen or metal halide is in the graphite intercalation compound of intercalator, and intercalator is bromine, iodine chloride, iodine bromide IBr, aluminum chloride, nickelous chloride, antimony chloride, iron(ic)chloride or antimonic fluoride etc.
In the gained Graphene powder, the number of plies of graphene film below 10 layers, lateral dimension is more than 1 micron, and crystallographic property is good, COR is more than 20.Preferable range is: 3～8 layers of the numbers of plies of graphene film, 5～50 microns of lateral dimensions, COR 30～120.
Among the present invention, in oxalic acid or the superoxol, the massfraction of oxalic acid or hydrogen peroxide is preferably 40～80wt%, and all the other are water.
When carrying out expansion process, the preferred time is 2～5 hours, and preferred temperature range is 10～40 ℃.
Among the present invention, per 1 liter of oxalic acid or superoxol can be handled 1～500 gram graphite intercalation compound, and preferred treatment capacity is 15～20 grams.
Among the present invention, to gained quasiflake graphite alkene aggregate ultrasonic oscillation treatment time in the aqueous solution of organic solvent or various tensio-active agents after the expansion process be preferably 30 minutes～1 hour.Wherein, Organic solvent can be alcohols, ketone, aldehydes, organic acid, N-Methyl pyrrolidone, N, N,N-DIMETHYLACETAMIDE, chlorobenzene or dichlorobenzene etc.; Tensio-active agent can be sodium lauryl sulphate, X 2073 or cetyl trimethylammonium bromide etc., and the strength of solution of tensio-active agent is 0.1-5wt%.
Among the present invention, be that the graphite intercalation compound of intercalator is a raw material with halogen or metal halide, this intercalation technique sees also document Intercalation compounds of graphite.Dresselhaus, M.S.; Dresselhaus, G., Advances in Physics 1981,30,1-186.
Advantage of the present invention:
1, the technology of graphite intercalation compound is comparatively ripe among the present invention, with halogen or metal halide be the graphite intercalation compound of intercalator can be in the normal atmospheric environment long-time stable existence, sufficient raw material can be provided.
2, the expansion process among the present invention is a liquid-phase chemical reaction, and the degrees of expansion of graphite and homogeneity are all very high, can guarantee high yield and homogeneity.
3, the present invention produces the needed time of 1 batch products and is less than 12 hours; Single batch of Graphene product is higher than 70% with respect to the productive rate of raw material graphite (not comprising the intercalator quality).
4, the present invention's stripping process that expands destroys the structure of Graphene hardly, can farthest keep structure and the electricity and the mechanical property of Graphene.
5, the present invention's intercalator of being present in graphite layers can spontaneously be removed in expansion process, therefore can guarantee to obtain highly purified Graphene product.
6, entire reaction course is very little to the influence of environment, and the processing cost of waste liquid is low.
Description of drawings
Fig. 1 is the intercalation of graphite intercalation compound and the image after the expansion.Among the figure; (a) the natural flake graphite original section before the intercalation not; (b) cross section of graphite intercalation compound; (c) with the quasiflake graphite alkene aggregate of graphite intercalation compound and 30wt% oxalic acid solution reaction generation, (d) the local enlarged photograph of quasiflake graphite alkene aggregate is it is thus clear that it is inflated the Graphene of peeling off slabbing.
Fig. 2 expands-peels off-the dry macro morphology (optical photograph, the about 0.1g of sample total mass) of Graphene afterwards.
Fig. 3 expands-peels off-the dry microscopic appearance of Graphene afterwards.
Fig. 4 is x-ray photoelectron spectroscopy (XPS) spectrogram (2 points) of (a)-(c) expand-peel off-dry back Graphene.Fig. 4 (a) composes for XPS entirely; Fig. 4 (b) is the meticulous spectrum of C 1s peak position; The meticulous spectrum of Fig. 4 (c) Cl 2p peak position; Fig. 4 (d) is the degree of each element in the Graphene sample that calculates according to XPS spectrum.
Embodiment
Shown in Fig. 1 a-b, the model ylid bloom action power of the graphite raw material interlayer of process intercalation processing is weakened, and interlamellar spacing is by expansion effectively.
Because structural integrity, the gained Graphene still keeps very strong hydrophobicity, therefore in the oxalic acid or superoxol that with water are primary solvent, demonstrates the vermiform state of aggregation shown in Fig. 1 c and d, and we are referred to as quasiflake graphite alkene aggregate.This quasiflake graphite alkene aggregate can be in the organic solvent of low surface tension or added in the aqueous solution of tensio-active agent be aided with the short period of time, Graphene is peeled off in lower powered ultrasonic concussion fully, obtains the Graphene dispersion liquid.Can obtain the fluffy Graphene powder shown in Fig. 2 and 3 after utilizing conventional lyophilize or spraying drying to remove solvent.X-ray photoelectron spectroscopy (XPS; Characterization result Fig. 4) shows that chlorine atomic percent remaining in the powder is about 0.1%; COR is greater than 90, detects less than there being the residual metal ion to exist, and shows that it has good crystallinity, extremely low oxygen level and higher purity.
Among Fig. 4 (d), the atomic percent of Cl, C and O is (table 1) as follows:
Table 1: the atomic percent of Cl, C and O in the gained Graphene sample
| Cl2p | C1s | O1s |
| Atomic percent (%) | Atomic percent (%) | Atomic percent (%) |
| 0.0993329 | 98.7434 | 1.1573 |
| 0.0980622 | 98.6365 | 1.26543 |
Embodiment 1:
With 1g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the bromine; The consumption of bromine is 0.6g) join in the oxalic acid solution that 100mL concentration is 60wt%; The control solution temperature is 30 ℃; Slowly stirred 4 hours, obtain swimming in the adequately expanded quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 1L N-Methyl pyrrolidone solution, utilize power density to obtain the Graphene dispersion liquid in 30 minutes for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene after utilizing spray-drying process to remove the N-crassitude, the mass yield of not calculating bromine intercalator in the raw material is about 72%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 2:
With 10g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the iodine chloride; The consumption of iodine chloride is 6.5g) join in the superoxol that 500mL concentration is 50wt%; The control solution temperature is 30 ℃; Slowly stirred 2.5 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 2L N (DMF), utilize power density to obtain the Graphene dispersion liquid in 2 hours for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing spray-drying process to remove N (DMF), quality is about 3g, and the mass yield of not calculating iodine chloride intercalator in the raw material is about 75%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 3:
With 15g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the iodine bromide IBr; The consumption of iodine bromide IBr is 10g) join in the oxalic acid solution that 500mL concentration is 60wt%; The control solution temperature is 30 ℃; Slowly stirred 2 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 2L dichlorobenzene (DCB), utilize power density to obtain the Graphene dispersion liquid in 30 minutes for the 1W/mL ultrasonic oscillation to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing spray-drying process to remove DCB, quality is about 5g, and the mass yield of not calculating iodine bromide IBr intercalator in the raw material is about 78%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 4:
With 50g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with aluminum chloride; The consumption of aluminum chloride is 30g) join in the superoxol that 1L concentration is 70wt%; The control solution temperature is 50 ℃; Slowly stirred 1.5 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 5L ethanol, utilize power density to obtain the Graphene dispersion liquid in 30 minutes for the ultrasonic oscillation of 1W/mL to scavenging solution with washed with de-ionized water.
Can obtain pulverous Graphene after utilizing spray-drying process to remove ethanol, the mass yield of not calculating raw material aluminum chloride intercalator is about 75%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 5:
With 50g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the nickelous chloride; The consumption of nickelous chloride is 30g) join in the oxalic acid solution that 2L concentration is 80wt%; The control solution temperature is 0 ℃, slowly stirs 1 hour, obtains swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 5L propyl alcohol, utilize power density to obtain the Graphene dispersion liquid in 60 minutes for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene after utilizing spray-drying process to remove propyl alcohol, the mass yield of not calculating nickelous chloride intercalator in the raw material is about 70%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 6:
With 1kg is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with iron(ic)chloride; The consumption of iron(ic)chloride is 0.66kg) join in the superoxol that 10L concentration is 90wt%; The control solution temperature is 0 ℃; Slowly stirred 0.5 hour, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 30L butanols, utilize power density to obtain the Graphene dispersion liquid in 60 minutes for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing spray-drying process to remove butanols, quality is about 360g, and the mass yield of not calculating iron(ic)chloride intercalator in the raw material is about 76%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 7:
With 5g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the antimonic fluoride; The consumption of antimonic fluoride is 3g) join in the superoxol that 200mL concentration is 70wt%; The control solution temperature is 60 ℃; Slowly stirred 1.5 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 1L propyl alcohol, utilize power density to obtain the Graphene dispersion liquid in 2 hours for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing spray-drying process to remove propyl alcohol, the mass yield of not calculating antimonic fluoride intercalator in the raw material is about 72%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 8:
With 10g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the antimony chloride; The consumption of antimony chloride is 4.8g) join in the superoxol that 500mL concentration is 60wt%; The control solution temperature is 60 ℃; Slowly stirred 2 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 1L formaldehyde, utilize power density to obtain the Graphene dispersion liquid for the ultrasonic oscillation 1h of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing spray-drying process to remove formaldehyde, the mass yield of not calculating antimony chloride intercalator in the raw material is about 72%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 9:
With 20g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the bromine; The consumption of bromine is 12g) join in the oxalic acid solution that 500mL concentration is 50wt%; The control solution temperature is 80 ℃, slowly stirs 2.5 hours, obtains swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 1L N-Methyl pyrrolidone (NMP), utilize power density to obtain the Graphene dispersion liquid in 1 hour for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing freeze-drying to remove N-Methyl pyrrolidone (NMP), quality is about 6g, and the mass yield of not calculating bromine intercalator in the raw material is about 75%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 10:
With 100g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with aluminum chloride; The consumption of aluminum chloride is 65g) join in the superoxol that 1L concentration is 40wt%; The control solution temperature is 80 ℃; Slowly stirred 3 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 2L N (DMF), utilize power density to obtain the Graphene dispersion liquid in 1 hour for the ultrasonic oscillation of 1W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing freeze-drying to remove N (DMF), quality is about 35g, and the mass yield of not calculating aluminum chloride intercalator in the raw material is about 78%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 11:
With 50g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with iron(ic)chloride; The consumption of iron(ic)chloride is 35g) join in the oxalic acid solution that 1L concentration is 50wt%; The control solution temperature is 80 ℃, slowly stirs 2.5 hours, obtains swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 2L dichlorobenzene (DCB), utilize power density to obtain the Graphene dispersion liquid in 3 hours for the ultrasonic oscillation of 1W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing freeze-drying to remove DCB, quality is about 16g, and the mass yield of not calculating iron(ic)chloride intercalator in the raw material is about 78%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 12:
With 100g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the nickelous chloride; The consumption of nickelous chloride is 51g) to join in the superoxol that 2L concentration is 60wt% the control solution temperature be 0 ℃; Slowly stirred 2 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 4L ethanol, utilize power density to obtain the Graphene dispersion liquid in 2 hours for the ultrasonic oscillation of 0.5W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing freeze-drying to remove ethanol, quality is about 30g, and the productive rate when not calculating the quality of nickelous chloride intercalator in the raw material is about 78%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 13:
With 100g is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the antimony chloride; The consumption of antimony chloride is 70g) join in the oxalic acid solution that 2L concentration is 70wt%; The control solution temperature is 30 ℃; Slowly stirred 1.5 hours, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out, repeatedly drain after colourless, join in the 1.5L acetone, utilize power density to obtain the Graphene dispersion liquid in 60 minutes for the ultrasonic oscillation of 1W/mL to scavenging solution with washed with de-ionized water.
Obtain pulverous Graphene product after utilizing freeze-drying to remove acetone, quality is about 36g, and the mass yield of not calculating antimony chloride intercalator in the raw material is about 75%.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Embodiment 14:
With 1kg is that the graphite intercalation compound of intercalator is (in the graphite intercalation compound with the antimonic fluoride; The consumption of antimonic fluoride is 0.55kg) join in the superoxol that 20L concentration is 80wt%; The control solution temperature is 40 ℃; Slowly stirred 1 hour, obtain swimming in the quasiflake graphite alkene aggregate on the liquid level.
Gained quasiflake graphite alkene aggregate is taken out; Repeatedly drain after colourless with washed with de-ionized water to scavenging solution; Join in the lauryl sodium sulfate aqueous solution that 20L concentration is 1wt%, utilize power density to obtain the Graphene dispersion liquid in 5 hours for the ultrasonic oscillation of 0.1W/mL.
Can arrive pulverous Graphene product after utilizing freeze-drying to remove water, quality is about 380g, does not calculate that antimonic fluoride intercalator mass yield is about 72% in the raw material.
In the present embodiment gained Graphene powder, the number of plies of graphene film is that 5-8 layer, lateral dimension are the 10-20 micron, and good crystallinity, and COR is 80-100.
Claims (10)
1. a method for preparing the high quality Graphene is characterized in that, is that the graphite intercalation compound of intercalator is a raw material with halogen or metal halide, oxalic acid or superoxol expand with solvent in ultrasonic peel off to combine prepare the high quality Graphene; At first the graphite intercalation compound powder is joined in the oxalic acid or superoxol of concentration more than 15wt%, under 0～100 ℃ condition, carry out 0.5～24 hour expansion process then, obtain the quasiflake graphite alkene aggregate of high level expansion; And then; With gained quasiflake graphite alkene aggregate after the expansion process in the aqueous solution or organic solvent solution of organic solvent or various tensio-active agents; Ultrasonic oscillation was handled 1 minute～5 hours, realized peeling off, and Graphene is dispersed in forms Graphene solution in the solvent; After utilizing spraying drying or cryodesiccated method to remove organic solvent or various tensio-active agent, obtain high-quality Graphene powder.
2. according to the described method for preparing the high quality Graphene of claim 1; It is characterized in that; With halogen or metal halide is in the graphite intercalation compound of intercalator intercalation, and intercalator is bromine, iodine chloride, iodine bromide IBr, aluminum chloride, nickelous chloride, antimony chloride, iron(ic)chloride or antimonic fluoride.
3. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that, in the gained Graphene powder, the number of plies of graphene film below 10 layers, the lamella size is more than 1 micron, and crystallographic property is good, COR is more than 20.
4. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that in the gained Graphene powder, preferable range is: 3～8 layers of the numbers of plies of graphene film, 5～50 microns of lamella sizes, COR 30～120.
5. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that in oxalic acid or the superoxol, the massfraction of oxalic acid or hydrogen peroxide is preferably 40～80wt%, all the other are water.
6. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that when carrying out expansion process, the preferred time is 2～5 hours, preferred temperature range is 10～40 ℃.
7. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that per 1 liter of oxalic acid or superoxol are handled 1～500 gram graphite intercalation compound.
8. according to the described method for preparing the high quality Graphene of claim 1, it is characterized in that per 1 liter of oxalic acid or superoxol preferably treatment 15～20 gram graphite intercalation compounds.
9. according to the described method for preparing the high quality Graphene of claim 1; It is characterized in that, to gained quasiflake graphite alkene aggregate ultrasonic oscillation treatment time in the aqueous solution of organic solvent or various tensio-active agents after the expansion process be preferably 30 minutes～1 hour.
10. according to the described method for preparing the high quality Graphene of claim 1; It is characterized in that; Organic solvent is alcohols, ketone, aldehydes, organic acid, N-Methyl pyrrolidone, N, N,N-DIMETHYLACETAMIDE, chlorobenzene or dichlorobenzene; Tensio-active agent is sodium lauryl sulphate, X 2073 or cetyl trimethylammonium bromide, and the strength of solution of tensio-active agent is 0.1-5wt%.
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Free format text: CORRECT: ADDRESS; FROM: 110016 SHENYANG, LIAONING PROVINCE TO: 618000 DEYANG, SICHUAN PROVINCE |
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Effective date of registration: 20140717 Address after: 618000, No. two, No. 57 Minjiang West Road, Deyang, Sichuan Province, 1 Patentee after: Deyang Gaphene Technology Co., Ltd. Address before: 110016 Shenyang, Liaoning Province Cultural Road, No. 72, Shenhe Patentee before: Institute of metal research, Chinese Academy of Sciences |