CN105948033A - Method of preparing graphene by means of wet microwave stripping - Google Patents
Method of preparing graphene by means of wet microwave stripping Download PDFInfo
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Abstract
The invention relates to a method of preparing graphene by means of wet microwave stripping, comprising the following steps: adding a certain amount of intercalating solvent into expandable graphite of different particle sizes for ultrasonic treatment for 1-10 hours, filtering treated solution, adding the obtained high-solid expandable graphite system into microwave stripping equipment provided with a solvent collector for microwave treatment to prepare and obtain the graphene. The intercalating solvent can infiltrate between expandable graphite sheet layers after the microwave treatment, and gasify quickly during the microwave stripping, so that the graphite is stripped into the graphene and fewer layers are realized. The method disclosed by the invention has the advantages of complete stripping effect, fewer layers of stripped grapheme, simple production process, environmental protection and capability of industrialized production.
Description
Technical field
The invention belongs to a kind of method that Graphene is prepared in wet method microwave stripping.
Background technology
Graphene is by the Two-dimensional Carbon material of monolayer carbon atomic building, and long-range conjugated structure makes it very rigid, and fracture is strong
Degree is up to 42N/m2, tensile strength and elastic modelling quantity are respectively 130GPa and 1.0TPa.Graphene the most also has fabulous leading
Heat, electric conductivity, at room temperature thermal conductivity is 5300W/ (m K), and under room temperature, electron mobility is more than 15000cm2/(V·s)。
Graphene light transmission is excellent, and absorptance is only 2.3%.Stone has the performance of many excellences due to ink alkene, thus the most right
The research and development of Graphene occurs in that quickly growth.
Though Graphene has many excellent properties, the production cost higher price costliness of Graphene hinders largely
The application of Graphene.Mechanical stripping method is the physical method prepared for Graphene the earliest, and the Graphene that the method obtains is relatively
Perfection, but productivity is low, high in cost of production feature, limits 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 stripping, Graphene quality prepared by this method is fine, but the method
The Graphene productivity prepared is the lowest, it is difficult to accomplish 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 have also been obtained relatively in some coating material fields
Good application, but this method has the residual of some impurity, will reduce character 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,
The production technology of current optimal preparation high-quality graphene film, but it have highly energy-consuming and expensive lack
Point, and large area and continuous prodution can not be carried out, it is only used for the such as most significant end field such as display and transistor manufacture.
SiC epitaxial growth method has the shortcoming of high cost and high-temperature, the technical characterstic of inadaptable modern silicon electronic device.And, its
High-temperature operation, high base material price and undersized manufacturing characteristics make it be only used for some much more expensive fields.Existing micro-
Ripple is peeled off and is mainly peeled off by direct for expansible graphite microwave.In the product of expansible graphite directly stripping, Graphene occupies
Ratio is peeled off not thorough less, and the Graphene number of plies more application after stripping is poor.
Summary of the invention
For the problems referred to above, basis is the brightest discloses a kind of method that Graphene is prepared in wet method microwave stripping, and the present invention utilizes super
Sound wave adds suitable intercalation solution and processes expansible graphite, and after filtration, system is the high solid with substantial amounts of intercalation solution
System, during microwave treatment, intercalation solution gasifies rapidly, and the existence of the most substantial amounts of intercalation solution allows for carrying out microwave stripping
Time, peel off more abundant, peel off the number of plies less, be also more uniformly distributed.And the method preparation technology ring simple, with low cost, green
Guarantor, production suitable for industrialized and practical application height.
The present invention is achieved by the following technical solutions: a kind of method that Graphene is prepared in wet method microwave stripping, by work
The expansible graphite that industry metaplasia is produced adds intercalation solution, puts in existing conventional Ultrasound wave device and carries out ultrasound wave intercalation, ultrasonic
The shear cavitation effect of ripple can destroy the Van der Waals force of graphite layers, makes the distance of sheet interlayer become big, makes intercalation solution more simultaneously
Penetrate between graphite flake layer well.Filter after supersound process and remove part intercalator.By be filtrated to get containing a large amount of intercalation solution
Expansible graphite join in the microwave equipment of solvent catcher and carry out microwave stripping, microwave exposure instantaneous can make high solid
Part system reaches the highest temperature makes intercalation solution transient evaporation strut graphite flake layer, makes graphite become Graphene, after gasification
Intercalation solution can be reclaimed by the cooling of solvent catcher, i.e. can get Graphene finished product.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, the granularity of expansible graphite used is 50-
Best results during 5000 mesh.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, the consumption of intercalation solution is graphite quality
20 times to 100 times best results.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, intercalation solution used is N-methylpyrrole
Alkanone, N,N-dimethylformamide, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone, oxolane, toluene, two
In toluene, dichloromethane, chloroform any one.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, ultrasonic Treatment temperature is 30-80 DEG C, super
Acoustic power is 100-800W, sonication times 1-10h, best results after process.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, need inert atmosphere to protect when microwave is peeled off
Protect and include: nitrogen, argon, helium.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, intercalation solution gasifies when microwave is peeled off, institute
The gas produced can be reclaimed by solvent catcher and utilize.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, described microwave exposure treatment conditions are: microwave
Frequency 915MHz-2450MHz, microwave output power density is 50-150mW/cm3, microwave irradiation time is 5-100s, after stripping
Best results.
The Advantageous Effects of the present invention:
(1) utilizing the method for the invention, use supersound process expansible graphite, the cavitation shear action utilizing ultrasound wave is swollen
Swollen graphite flake layer spacing increases, and makes that intercalation solution is deeper finer penetrates into expansible graphite interlayer simultaneously.Remove after filtration
Part intercalation solution, makes expansible graphite be in high solid body part and (makes what intercalator unexpectedly may be many to be retained in expansible graphite sheet
Between Ceng), during microwave exposure, intercalator gasifies rapidly and is strutted by graphite flake layer, makes graphite flake layer be separated into Graphene.Due to
In high solid, intercalator is more, thus peel off compared with peeling off with existing dry method microwave after Microwave Burst stripping more thoroughly also
And the Graphene number of plies after peeling off is less, the method is the process of a pure physical separation simultaneously, so the Graphene of preparation
Structure is more excellent without organo-functional group using effect.
(2) the method for the invention can be by regulating the consumption of intercalation solution, ultrasonic bar compared with conventional microwave stripping
Part, microwave condition prepares different application demand Graphene, and controllability is higher.
And the method preparation technology compared with existing graphene preparation method is simpler, with low cost, microwave (3)
Compared with the stripping means that after stripping, intercalator is recyclable with common more environmental protection and can industrialization large-scale production,
Product practical application is higher.
Accompanying drawing explanation
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;
Detailed description of the invention
The method that Graphene is prepared in wet method microwave stripping, adds intercalation solution by expansible graphite, puts into existing routine and surpasses
Carrying out ultrasound wave intercalation in acoustic wave device, the shear cavitation effect of ultrasound wave can destroy the Van der Waals force of graphite layers, makes lamella
Between distance become big, make intercalation solution more preferably penetrate between graphite flake layer simultaneously, filter after supersound process and remove part intercalator,
The expansible graphite containing a large amount of intercalation solution being filtrated to get is joined the microwave equipment of solvent catcher is carried out micro-
Ripple is peeled off, and microwave exposure instantaneous can make high solid system reach the highest temperature, makes the intercalation solution of expansible graphite interlayer
Transient evaporation struts graphite flake layer, makes graphite become Graphene, and the intercalation solution after gasification can be cooled back by solvent catcher
Receive, i.e. can get Graphene finished product.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, the granularity of expansible graphite used is 50-
Best results during 5000 mesh.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, the consumption of intercalation solution is graphite quality
20 times to 100 times best results.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, intercalation solution used is N-methylpyrrole
Alkanone, N,N-dimethylformamide, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone, oxolane, toluene, two
In toluene, dichloromethane, chloroform any one.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, ultrasonic Treatment temperature is 30-80 DEG C, super
Acoustic power is 100-800W, sonication times 1-10h, best results after process.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, need inert atmosphere to protect when microwave is peeled off
Protect and include: nitrogen, argon, helium.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, intercalation solution gasifies when microwave is peeled off, institute
The gas produced can be reclaimed by solvent catcher and utilize.
Further, a kind of method that Graphene is prepared in wet method microwave stripping, described microwave exposure treatment conditions are: microwave
Frequency 915MHz-2450MHz, microwave output power density is 50-150mW/cm3, microwave irradiation time is 5-100s, after stripping
Best results.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is explained in further detail.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 contain any be defined by the claims the replacement done in the spirit and scope of the present invention, repair
Change, equivalent method and scheme.Further, in order to make the public that the present invention to be had a better understanding, thin to the present invention below
During joint describes, detailed describe some specific detail sections.There is no these detail sections for a person skilled in the art
Description can also understand the present invention completely.
Embodiment 1
Weigh the expansible graphite 10g that granularity is 50 mesh, add N-Methyl pyrrolidone 1000g, put into ultrasonic equipment
In, ultrasonic temperature 30 DEG C, ultrasonic power 800W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 310g solid.
Being sent into by solid after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density is 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 are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
The Elemental analysis data of end product in table 1 embodiment 1-11
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 end product in table 2 embodiment 1-11
The AFM thickness statistical data of end product in table 3 embodiment 1-6
Embodiment 2
Weigh the expansible graphite 10g that granularity is 50 mesh, add DMF 200g, put into ultrasonic equipment
In, ultrasonic temperature 80 DEG C, ultrasonic power 800W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 15g solid.
Being sent into by solid after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density is 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 are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
Embodiment 3
Weigh the expansible graphite 10g that granularity is 50 mesh, add dioxane 1000g, put in ultrasonic equipment, ultrasonic
Ripple temperature 30 DEG C, ultrasonic power 100W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 100g solid.
Being sent into by solid after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density is 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 are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
Embodiment 4
Weigh the expansible graphite 10g that granularity is 500 mesh, add water 500g, put in ultrasonic equipment, ultrasonic temperature
30 DEG C, ultrasonic power 800W, ultrasonic Treatment 1h.Sucking filtration after ultrasonic Treatment, leaches 310g solid.
Being sent into by solid after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density is 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 are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
Embodiment 5
Weigh the expansible graphite 10g that granularity is 400 mesh, add methanol 1000g, put in ultrasonic equipment, ultrasound wave
Temperature 30 DEG C, ultrasonic power 100W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 100g solid.
Being sent into by solid after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is microwave frequency
915MHz, Microwave Power Density is 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 are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
Embodiment 6
Weigh the expansible graphite 10g that granularity is 800 mesh, add ethanol 1000g, put in ultrasonic equipment, ultrasound wave
Temperature 30 DEG C, ultrasonic power 100W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 200 high solid solution.
Being sent into by high solid solution after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density is 50mW/cm3, the microwave time is 100s.The scanning of the Graphene prepared
Electronic Speculum figure is shown in that Fig. 6, Elemental analysis data are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 3.
Embodiment 7
Weigh the expansible graphite 10g that granularity is 800 mesh, add ethylene glycol 1000g, put in ultrasonic equipment, ultrasonic
Ripple temperature 30 DEG C, ultrasonic power 100W, ultrasonic Treatment 10h.Sucking filtration after ultrasonic Treatment, leaches 200g high solid molten
Liquid.
Being sent into by high solid solution after sucking filtration in microwave equipment, keep nitrogen atmosphere in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density is 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 are shown in Table 2, AFM thickness statistical data is shown in Table 4.
The AFM thickness statistical data of end product in table 4 embodiment 6-12
Embodiment 8
Weigh the expansible graphite 10g that granularity is 800 mesh, add acetone 1000g, put in ultrasonic equipment, ultrasound wave
Temperature 30 DEG C, ultrasonic power 400W, ultrasonic Treatment 8h.Sucking filtration after ultrasonic Treatment, leaches 100g high solid solution.
Being sent into by high solid solution after sucking filtration in microwave equipment, keep argon gas atmosphere in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density is 150mW/cm3, the microwave time is 45s.The scanning of the Graphene prepared
Electronic Speculum figure is shown in that Fig. 8, Elemental analysis data are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 4.
Embodiment 9
Weigh the expansible graphite 10g that granularity is 800 mesh, add oxolane 1000g, put in ultrasonic equipment, super
Acoustic wave temperature 30 DEG C, ultrasonic power 400W, ultrasonic Treatment 8h.Sucking filtration after ultrasonic Treatment, leaches 150g high solid molten
Liquid.
Being sent into by high solid solution after sucking filtration in microwave equipment, keep vacuum state in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density is 150mW/cm3, the microwave time is 45s.The scanning of the Graphene prepared
Electronic Speculum figure is shown in that Fig. 9, Elemental analysis data are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 4.
Embodiment 10
Weigh the expansible graphite 10g that granularity is 1500 mesh, add toluene 1000g, put in ultrasonic equipment, ultrasound wave
Temperature 30 DEG C, ultrasonic power 400W, ultrasonic Treatment 8h.Sucking filtration after ultrasonic Treatment, leaches 200g high solid solution.
Being sent into by high solid solution after sucking filtration in microwave equipment, keep vacuum state in microwave office, microwave condition is
Microwave frequency 2450MHz, Microwave Power Density is 150mW/cm3, the microwave time is 45s.The scanning of the Graphene prepared
Electronic Speculum figure is shown in that Figure 10, Elemental analysis data are shown in Table 1, granularmetric analysis data are shown in Table 2, AFM thickness statistical data is shown in Table 4.
Embodiment 11
Weigh the expansible graphite 10g that granularity is 5000 mesh, add dichloromethane 1000g, put in ultrasonic equipment, super
Acoustic wave temperature 30 DEG C, ultrasonic power 400W, ultrasonic Treatment 8h.Sucking filtration after ultrasonic Treatment, leaches 200g high solid molten
Liquid.
High solid solution after sucking filtration is sent in microwave equipment, microwave office keeps hydrogen atmosphere, micro-strip
Part is microwave frequency 2450MHz, and Microwave Power Density is 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 are shown in Table 2, AFM thickness statistical data is shown in Table 4.
Interpretation: utilize the surface topography of the Graphene that scanning electron microscopic observation the method for the invention produces, can
To find out that graphenic surface has a large amount of fold, illustrate that the number of plies of Graphene is less;Can be seen that the method by elementary analysis simultaneously
The graphene carbon content produced is the highest, illustrates that this Graphene is practically free of some organo-functional groups, and Graphene purity is higher;Grain
Footpath analysis and characterization peel off after size;Atomic force microscope thickness statistical result shows, the sheet of the Graphene produced
Layer is relatively thin and the most uniform.
Claims (8)
1. the method that Graphene is prepared in the stripping of wet method microwave, is characterized in that, expansible graphite is added intercalation solution, puts into
Carrying out ultrasound wave intercalation in existing conventional Ultrasound wave device, the shear cavitation effect of ultrasound wave can destroy the Van der Waals of graphite layers
Power, makes the distance of sheet interlayer become big, makes intercalation solution more preferably penetrate between graphite flake layer simultaneously, filter removal portion after supersound process
Divide intercalator, the expansible graphite containing a large amount of intercalation solution being filtrated to get is joined the microwave equipment of solvent catcher
In carry out microwave stripping, microwave exposure instantaneous can make high solid system reach the highest temperature, makes expansible graphite interlayer
Intercalation solution transient evaporation struts graphite flake layer, makes graphite become Graphene, and the intercalation solution after gasification can be collected by solvent
Device cooling is reclaimed, and i.e. can get Graphene finished product.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that, used can be swollen
The granularity of swollen graphite is 50-5000 mesh.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that: intercalation solution
Consumption is 20 times to 100 times of expansible graphite quality.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that, intercalation used
Solvent be N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, methanol, ethanol, ethylene glycol, acetone, butanone,
Any one in oxolane, toluene, dimethylbenzene, dichloromethane, chloroform.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that: ultrasonic Treatment
Temperature is 30-80 DEG C, and ultrasonic power is 100-800W, sonication times 1-10h.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that: peel off at microwave
Time need inert atmosphere protection (such as nitrogen, argon, helium).
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that: intercalation solution exists
Gasification when microwave is peeled off, produced gas can be reclaimed by solvent catcher and utilize.
The most according to claim 1, a kind of method that Graphene is prepared in wet method microwave stripping, it is characterized in that: described microwave spoke
It is: microwave frequency 915MHz-2450MHz that microwave output power density is 50-150mW/cm according to treatment conditions3, during microwave exposure
Between be 5-100s.
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