CN105948033B - The method that wet method microwave stripping prepares graphene - Google Patents
The method that wet method microwave stripping prepares graphene Download PDFInfo
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- CN105948033B CN105948033B CN201610541943.4A CN201610541943A CN105948033B CN 105948033 B CN105948033 B CN 105948033B CN 201610541943 A CN201610541943 A CN 201610541943A CN 105948033 B CN105948033 B CN 105948033B
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
Body of the present invention is related to a kind of method that wet method microwave stripping prepares graphene.This method is that a certain amount of intercalation solution and 1 10h of ultrasonication are added into the expansible graphite of different-grain diameter, solution after filtration treatment, obtained expansible graphite high solid system is added to carry in solvent collector microwave peel-off device and carries out microwave treatment, graphene is prepared.Intercalation solution can be penetrated between expanded graphite lamella after ultrasonication, and is gasified rapidly when microwave is peeled off, and graphite is peeled off into graphene, and the number of plies is less.This method peeling effect is thoroughly, the graphene number of plies that separates is few, simple production process, it is environmentally protective, can industrialized production.
Description
Technical field
The invention belongs to a kind of method that wet method microwave stripping prepares graphene.
Background technology
Graphene is the two-dimentional carbon material being made of single layer of carbon atom, and long-range conjugated structure makes its very rigid, and fracture is strong
Degree is up to 42N/m2, tensile strength and elasticity modulus are respectively 130GPa and 1.0TPa.Graphene also has fabulous lead at the same time
Heat, electric conductivity, thermal conductivity is 5300W/ (mK) at room temperature, and electron mobility is more than 15000cm under room temperature2/(V·s)。
Graphene light transmission is excellent, and absorptance is only 2.3%.Stone many excellent performances since black alkene has, thus it is right in recent years
There is rapid growth in the research and development of graphene.
Though graphene has many excellent properties, the production cost higher price costliness of graphene largely hinders
The application of graphene.Mechanical stripping method be earliest for graphene prepare physical method, the graphene that this method obtains compared with
Perfection, but low yield, it is of high cost the features such as, limit its industrialization and large-scale production.Liquid phase stripping method is a kind of molten
Agent stripping method, and be a kind of relatively effective method in peeling off, graphene quality prepared by this method is fine, but this method
Obtained graphene yield is very low, it is difficult to accomplishes scale production.Chemistry redox method technique is simple, obtains vast graphene
The favor of practitioner, and have been realized in the production of tonne scale, its product also obtained in some coating material fields compared with
Good application, but this method has the residual of some impurity, will reduce property to a certain extent, and after-treatment can
Bring the significantly rising of cost.Chemical vapour deposition technique (CVD) is mainly used to prepare high-purity, high performance solid film,
Be at present it is optimal prepare highest quality graphene film production technology, but it have highly energy-consuming and it is expensive lack
Point, and large area and continuous production cannot be carried out, it is only used for the most significant end field such as display and transistor manufacture.
SiC epitaxial growth methods have the shortcomings that high cost and high-temperature, are not suitable with the technical characterstic of modern times silicon electronic device.Moreover, its
The manufacturing characteristics of high-temperature operation, high base material price and small size make it be only used for some very expensive fields.It is existing micro-
Ripple, which is peeled off, mainly peels off the direct microwave of expansible graphite.Expansible graphite is directly peeled off graphene in the product of stripping and is occupied
Ratio is peeled off be not thorough less, and the graphene number of plies more application after stripping is poor.
The content of the invention
In view of the above-mentioned problems, this bright a kind of method for disclosing wet method microwave stripping and preparing graphene, the present invention utilize super
Sound wave adds appropriate intercalation solution processing expansible graphite, and system is the high solid with substantial amounts of intercalation solution after filtering
System, intercalation solution gasifies rapidly during microwave treatment, therefore the presence of substantial amounts of intercalation solution allows for carrying out microwave stripping
When, stripping is more abundant, and the stripping number of plies is less, is also more uniformly distributed.And simple, of low cost, the green ring of this method preparation process
Guarantor, suitable industrialized production and practical application are high.
The present invention is achieved by the following technical solutions：A kind of method that wet method microwave stripping prepares graphene, by work
The expansible graphite of industry metaplasia production adds intercalation solution, is put into progress ultrasonic wave intercalation in existing conventional Ultrasound wave device, ultrasound
The shear cavitation effect of ripple can destroy the Van der Waals force of graphite layers, the distance of piece interlayer is become larger, while make intercalation solution more
Penetrate between graphite flake layer well.Filtering removes part intercalator after supersound process.Contain a large amount of intercalation solutions by what is be obtained by filtration
Expansible graphite be added in the microwave equipment of solvent collector progress microwave stripping, microwave irradiation can instantaneously make high solid
Part system, which reaches very high temperature, makes intercalation solution transient evaporation strut graphite flake layer, graphite is changed into graphene, after gasification
Intercalation solution can be cooled down by solvent collector and recycled, you can obtain graphene finished product.
Further, a kind of method that wet method microwave stripping prepares graphene, the granularity of expansible graphite used is 50-
Best results during 5000 mesh.
Further, a kind of method that wet method microwave stripping prepares graphene, the dosage of intercalation solution is graphite quality
20 times to 100 times best results.
Further, a kind of method that wet method microwave stripping prepares graphene, intercalation solution used are N- methylpyrroles
Alkanone, N,N-dimethylformamide, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone, tetrahydrofuran, toluene, two
Any one in toluene, dichloromethane, chloroform.
Further, a kind of method that wet method microwave stripping prepares graphene, ultrasonication temperature are 30-80 DEG C, are surpassed
Acoustic power is 100-800W, sonication times 1-10h, best results after processing.
Further, a kind of method that wet method microwave stripping prepares graphene, needs inert atmosphere to protect when microwave is peeled off
Shield includes：Nitrogen, argon gas, helium.
Further, a kind of method that wet method microwave stripping prepares graphene, intercalation solution gasify when microwave is peeled off, institute
The gas of generation can be recycled by solvent collector and utilized.
Further, a kind of method that wet method microwave stripping prepares graphene, the microwave irradiation treatment conditions are：Microwave
Frequency 915MHz-2450MHz, microwave output power density are 50-150mW/cm3, microwave irradiation time 5-100s, after stripping
Best results.
The advantageous effects of the present invention：
(1) the method for the invention is utilized, it is swollen using the cavitation shear action of ultrasonic wave with supersound process expansible graphite
The increase of swollen graphite flake layer spacing, while make intercalation solution is deeper finer to penetrate into expansible graphite interlayer.Removed after filtering
Part intercalation solution, make expansible graphite be in high solid body part (make intercalator unexpectedly may more than be retained in expansible graphite piece
Between layer), gasification struts graphite flake layer to intercalator rapidly during microwave irradiation, graphite flake layer is separated into graphene.Due to
Intercalator is more in high solid, thus Microwave Burst stripping after with existing dry method microwave stripping compared with stripping more thoroughly simultaneously
And the graphene number of plies after peeling off is less, while this method is the process of a pure physical separation, so the graphene prepared
Structure is more excellent without organo-functional group using effect.
(2) can be by adjusting the dosage of intercalation solution, ultrasonic bar compared with the stripping of the method for the invention and conventional microwave
Part, microwave condition prepare different application demand graphene, controllability higher.
(3) and this method preparation process compared with existing graphene preparation method is simpler, of low cost, microwave
After stripping intercalator it is recyclable more environmentally protective compared with common stripping means and can industrialize large-scale production,
Product practical application higher.
Brief description of the drawings
Fig. 1 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 1；
Fig. 2 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 2；
Fig. 3 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 3；
Fig. 4 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 4；
Fig. 5 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 5；
Fig. 6 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 6；
Fig. 7 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 7；
Fig. 8 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 8；
Fig. 9 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 9；
Figure 10 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 10；
Figure 11 is the graphene scanning electron microscope (SEM) photograph prepared in embodiment 11；
Embodiment
The method that wet method microwave stripping prepares graphene, intercalation solution is added by expansible graphite, is put into existing routine and is surpassed
Ultrasonic wave intercalation is carried out in acoustic wave device, the shear cavitation effect of ultrasonic wave can destroy the Van der Waals force of graphite layers, make lamella
Between distance become larger, while intercalation solution is more preferably penetrated between graphite flake layer, after supersound process filtering remove part intercalator,
The expansible graphite containing a large amount of intercalation solutions being obtained by filtration is added in the microwave equipment of solvent collector carry out it is micro-
Ripple is peeled off, and microwave irradiation can instantaneously make high solid system reach very high temperature, make the intercalation solution of expansible graphite interlayer
Transient evaporation struts graphite flake layer, graphite is changed into graphene, and the intercalation solution after gasification can be cooled back by solvent collector
Receive, you can obtain graphene finished product.
Further, a kind of method that wet method microwave stripping prepares graphene, the granularity of expansible graphite used is 50-
Best results during 5000 mesh.
Further, a kind of method that wet method microwave stripping prepares graphene, the dosage of intercalation solution is graphite quality
20 times to 100 times best results.
Further, a kind of method that wet method microwave stripping prepares graphene, intercalation solution used are N- methylpyrroles
Alkanone, N,N-dimethylformamide, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone, tetrahydrofuran, toluene, two
Any one in toluene, dichloromethane, chloroform.
Further, a kind of method that wet method microwave stripping prepares graphene, ultrasonication temperature are 30-80 DEG C, are surpassed
Acoustic power is 100-800W, sonication times 1-10h, best results after processing.
Further, a kind of method that wet method microwave stripping prepares graphene, needs inert atmosphere to protect when microwave is peeled off
Shield includes：Nitrogen, argon gas, helium.
Further, a kind of method that wet method microwave stripping prepares graphene, intercalation solution gasify when microwave is peeled off, institute
The gas of generation can be recycled by solvent collector and utilized.
Further, a kind of method that wet method microwave stripping prepares graphene, the microwave irradiation treatment conditions are：Microwave
Frequency 915MHz-2450MHz, microwave output power density are 50-150mW/cm3, microwave irradiation time 5-100s, after stripping
Best results.
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiies
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to the thin of the present invention
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also understand the present invention completely.
Embodiment 1
The expansible graphite 10g that granularity is 50 mesh is weighed, 1-methyl-2-pyrrolidinone 1000g is added, is put into ultrasonic equipment
In, 30 DEG C, ultrasonic power 800W, ultrasonication 10h of ultrasonic temperature.Filtered after ultrasonication, filter out 310g solids.
Filtered solid is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density 150mW/cm3, the microwave time is 100s.The scanning electron microscope (SEM) photograph of the graphene prepared is shown in
Fig. 1, Elemental analysis data, which are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics, is shown in Table 3.
The Elemental analysis data of final product in 1 embodiment 1-11 of table
| N [%] | C [%] | H [%] | S [%] | |
| Embodiment 1 | 0.016 | 0.911 | 0.012 | 0.011 |
| Embodiment 2 | 0.015 | 0.938 | 0.017 | 0.033 |
| Embodiment 3 | 0.024 | 0.966 | 0.010 | 0.009 |
| Embodiment 4 | 0.013 | 0.958 | 0.010 | 0.018 |
| Embodiment 5 | 0.012 | 0.967 | 0.008 | 0.013 |
| Embodiment 6 | 0.011 | 0.965 | 0.010 | 0.014 |
| Embodiment 7 | 0.009 | 0.970 | 0.012 | 0.009 |
| Embodiment 8 | 0.008 | 0.975 | 0.08 | 0.008 |
| Embodiment 9 | 0.009 | 0.971 | 0.010 | 0.009 |
| Embodiment 10 | 0.006 | 0.972 | 0.012 | 0.010 |
| Embodiment 11 | 0.002 | 0.967 | 0.010 | 0.021 |
The granularmetric analysis data of final product in 2 embodiment 1-11 of table
The AFM thickness statistics of final product in 3 embodiment 1-6 of table
Embodiment 2
The expansible graphite 10g that granularity is 50 mesh is weighed, n,N-Dimethylformamide 200g is added, is put into ultrasonic equipment
In, 80 DEG C, ultrasonic power 800W, ultrasonication 10h of ultrasonic temperature.Filtered after ultrasonication, filter out 15g solids.
Filtered solid is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density 150mW/cm3, the microwave time is 100s.The scanning electron microscope (SEM) photograph of the graphene prepared is shown in
Fig. 2, Elemental analysis data, which are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics, is shown in Table 3.
Embodiment 3
The expansible graphite 10g that granularity is 50 mesh is weighed, dioxane 1000g is added, is put into ultrasonic equipment, ultrasound
30 DEG C, ultrasonic power 100W, ultrasonication 10h of ripple temperature.Filtered after ultrasonication, filter out 100g solids.
Filtered solid is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density 150mW/cm3, the microwave time is 100s.The scanning electron microscope (SEM) photograph of the graphene prepared is shown in
Fig. 3, Elemental analysis data, which are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics, is shown in Table 3.
Embodiment 4
The expansible graphite 10g that granularity is 500 mesh is weighed, water 500g is added, is put into ultrasonic equipment, ultrasonic temperature
30 DEG C, ultrasonic power 800W, ultrasonication 1h.Filtered after ultrasonication, filter out 310g solids.
Filtered solid is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density 150mW/cm3, the microwave time is 100s.The scanning electron microscope (SEM) photograph of the graphene prepared is shown in
Fig. 4, Elemental analysis data, which are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics, is shown in Table 3.
Embodiment 5
The expansible graphite 10g that granularity is 400 mesh is weighed, methanol 1000g is added, is put into ultrasonic equipment, ultrasonic wave
30 DEG C, ultrasonic power 100W, ultrasonication 10h of temperature.Filtered after ultrasonication, filter out 100g solids.
Filtered solid is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density 150mW/cm3, the microwave time is 100s.The scanning electron microscope (SEM) photograph of the graphene prepared is shown in
Fig. 5, Elemental analysis data, which are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics, is shown in Table 3.
Embodiment 6
The expansible graphite 10g that granularity is 800 mesh is weighed, ethanol 1000g is added, is put into ultrasonic equipment, ultrasonic wave
30 DEG C, ultrasonic power 100W, ultrasonication 10h of temperature.Filtered after ultrasonication, filter out 200 high solid solution.
Filtered high solid solution is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density 50mW/cm3, the microwave time is 100s.The scanning of the graphene prepared
Electron microscope is shown in that Fig. 6, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 3.
Embodiment 7
The expansible graphite 10g that granularity is 800 mesh is weighed, ethylene glycol 1000g is added, is put into ultrasonic equipment, ultrasound
30 DEG C, ultrasonic power 100W, ultrasonication 10h of ripple temperature.Filtered after ultrasonication, it is molten to filter out 200g high solids
Liquid.
Filtered high solid solution is sent into microwave equipment, nitrogen atmosphere is kept in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density 150mW/cm3, the microwave time is 5s.The scanning electricity of the graphene prepared
Mirror figure is shown in that Fig. 7, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 4.
The AFM thickness statistics of final product in 4 embodiment 6-12 of table
Embodiment 8
The expansible graphite 10g that granularity is 800 mesh is weighed, acetone 1000g is added, is put into ultrasonic equipment, ultrasonic wave
30 DEG C, ultrasonic power 400W, ultrasonication 8h of temperature.Filtered after ultrasonication, filter out 100g high solid solution.
Filtered high solid solution is sent into microwave equipment, argon gas atmosphere is kept in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density 150mW/cm3, the microwave time is 45s.The scanning of the graphene prepared
Electron microscope is shown in that Fig. 8, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 4.
Embodiment 9
The expansible graphite 10g that granularity is 800 mesh is weighed, tetrahydrofuran 1000g is added, is put into ultrasonic equipment, is surpassed
30 DEG C, ultrasonic power 400W, ultrasonication 8h of acoustic wave temperature.Filtered after ultrasonication, it is molten to filter out 150g high solids
Liquid.
Filtered high solid solution is sent into microwave equipment, vacuum state is kept in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density 150mW/cm3, the microwave time is 45s.The scanning of the graphene prepared
Electron microscope is shown in that Fig. 9, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 4.
Embodiment 10
The expansible graphite 10g that granularity is 1500 mesh is weighed, toluene 1000g is added, is put into ultrasonic equipment, ultrasonic wave
30 DEG C, ultrasonic power 400W, ultrasonication 8h of temperature.Filtered after ultrasonication, filter out 200g high solid solution.
Filtered high solid solution is sent into microwave equipment, vacuum state is kept in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density 150mW/cm3, the microwave time is 45s.The scanning of the graphene prepared
Electron microscope is shown in that Figure 10, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 4.
Embodiment 11
The expansible graphite 10g that granularity is 5000 mesh is weighed, dichloromethane 1000g is added, is put into ultrasonic equipment, is surpassed
30 DEG C, ultrasonic power 400W, ultrasonication 8h of acoustic wave temperature.Filtered after ultrasonication, it is molten to filter out 200g high solids
Liquid.
Filtered high solid solution is sent into microwave equipment, hydrogen atmosphere, micro-strip are kept in microwave office
Part is microwave frequency 2450MHz, Microwave Power Density 150mW/cm3, the microwave time is 25s.The graphene prepared
Scanning electron microscope (SEM) photograph is shown in that Figure 11, Elemental analysis data are shown in Table 1, granularmetric analysis data and are shown in Table 2, AFM thickness statistics and is shown in Table 4.
Analysis of experimental results：, can using the surface topography of the graphene of scanning electron microscopic observation the method for the invention production
To find out that graphene surface there are a large amount of folds, illustrate that the number of plies of graphene is less；This method can be seen that by elemental analysis at the same time
The graphene carbon content of production is very high, illustrates that the graphene is practically free of some organo-functional groups, graphene purity is higher；Grain
Footpath analysis and characterization peel off after particle size；Atomic force microscope thickness statistical result shows, the piece of the graphene produced
Layer is relatively thin and relatively more uniform.
Claims (2)
1. a kind of method that wet method microwave stripping prepares graphene, it is characterized in that：Expansible graphite is added into intercalation solution, is put into
Ultrasonic wave intercalation is carried out in existing conventional Ultrasound wave device, the shear cavitation effect of ultrasonic wave can destroy the Van der Waals of graphite layers
Power, makes the distance of piece interlayer become larger, while intercalation solution is more preferably penetrated between graphite flake layer, and removal portion is filtered after supersound process
Divide intercalator, the expansible graphite containing a large amount of intercalation solutions being obtained by filtration is added to the microwave equipment of solvent collector
Middle progress microwave stripping, microwave irradiation can instantaneously make high solid system reach very high temperature, make expansible graphite interlayer
Intercalation solution transient evaporation struts graphite flake layer, graphite is changed into graphene, and the intercalation solution after gasification passes through solvent collector
Cooling recycling, you can obtain graphene finished product, the granularity of expansible graphite used is 50-5000 mesh, the dosage of intercalation solution
It is 20 times to 100 times of expansible graphite quality, intercalation solution used is 1-methyl-2-pyrrolidinone, N, N- dimethyl formyls
Amine, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone, tetrahydrofuran, toluene, dimethylbenzene, dichloromethane, chloroform
In any one, ultrasonication temperature be 30-80 DEG C, ultrasonic power 100-800W, sonication times 1-10h,
Microwave needs inert atmosphere protection when peeling off, and intercalation solution gasifies when microwave is peeled off, and caused gas is collected by solvent
Device recycling, the microwave irradiation treatment conditions are：Microwave frequency 915MHz-2450MHz, microwave output power density are
50-150mW/cm3, microwave irradiation time 5-100s.
2. the method that a kind of wet method microwave stripping according to claim 1 prepares graphene, it is characterized in that：The indifferent gas
Atmosphere is：Nitrogen, argon gas, helium.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464312A (en) * | 2010-11-05 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN103224230A (en) * | 2013-04-16 | 2013-07-31 | 谭彬 | Preparation method of graphene |
| CN103253659A (en) * | 2013-05-23 | 2013-08-21 | 渤海大学 | Method for preparing graphene through carrying out ultrasonic stripping on graphite |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
| CN103935997A (en) * | 2014-05-10 | 2014-07-23 | 由伟 | Method for producing graphene based on sodium dodecylbenzene sulfonate |
| CN105502371A (en) * | 2016-01-05 | 2016-04-20 | 上海和伍复合材料有限公司 | Liquid-phase stripping preparation method of graphene |
-
2016
- 2016-07-11 CN CN201610541943.4A patent/CN105948033B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464312A (en) * | 2010-11-05 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN103224230A (en) * | 2013-04-16 | 2013-07-31 | 谭彬 | Preparation method of graphene |
| CN103253659A (en) * | 2013-05-23 | 2013-08-21 | 渤海大学 | Method for preparing graphene through carrying out ultrasonic stripping on graphite |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
| CN103935997A (en) * | 2014-05-10 | 2014-07-23 | 由伟 | Method for producing graphene based on sodium dodecylbenzene sulfonate |
| CN105502371A (en) * | 2016-01-05 | 2016-04-20 | 上海和伍复合材料有限公司 | Liquid-phase stripping preparation method of graphene |
Non-Patent Citations (1)
| Title |
|---|
| 微波加热剥离法制备石墨烯;闫浩然等;《化学推进剂与高分子材料》;20121231;第10卷(第3期);第47页 * |
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