CN109321932A - Graphene and the preparation method and application thereof - Google Patents
Graphene and the preparation method and application thereof Download PDFInfo
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- CN109321932A CN109321932A CN201811278583.9A CN201811278583A CN109321932A CN 109321932 A CN109321932 A CN 109321932A CN 201811278583 A CN201811278583 A CN 201811278583A CN 109321932 A CN109321932 A CN 109321932A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses graphenes and the preparation method and application thereof.The preparation method of above-mentioned graphene is to be inserted into graphite electrode as anode and metal electrode or non-metal electrode as cathode using ionic liquid as electrolyte;The voltage or density for applying 0.5V-10V between a cathode and an anode are 1mA/cm2‑100mA/cm2Electric current, electrochemical reaction preset time obtains reaction product;Reaction product is post-processed, obtains thin graphene using ionic liquid as electrolyte, is inserted into graphite electrode as anode and metal electrode or non-metal electrode as cathode;Apply voltage between a cathode and an anode or electric current, electrochemical reaction preset time obtain reaction product;The reaction product is post-processed, thin graphene is obtained;Graphene is adopted to be made with the aforedescribed process;Above-mentioned graphene is applied in battery.The preparation method of graphene of the present invention, graphene function dough degree obtained is high, and function is more.
Description
Technical field
The present invention relates to grapheme material technical fields, and in particular to graphene and the preparation method and application thereof.
Background technique
Graphene is the one of the discoveries such as the strong sea the .K. nurse of peace moral (Andre K.Geim) of Univ Manchester UK in 2004
Kind Two-dimensional Carbon atomic crystal, and the physics Nobel Prize in 2010 is obtained, cause carbon material research boom again.Since its is unique
Structure and photoelectric property become the research hotspot in the fields such as carbon material, nanotechnology, Condensed Matter Physics and functional material, inhale
Many scientific workers are drawn.
Graphene possesses excellent physics, chemical property, has high light transmittance and electric conductivity, high-specific surface area, high intensity
And the soft just excellent performance such as property, it is expected to be sent out in high-performance nanometer electronic device, photoelectric device, gas sensor, composite material, field
The fields such as material and energy stores are penetrated to be widely applied.
The preparation method of graphene is mainly graphite oxide reduction method at present, and this method will cause the broken of graphene-structured
It is bad, and using the toxic chemical reagent for having pollution, undesirable influence can be caused on environment, be unfavorable for environmental protection.In addition
There is using pyrolytic carbon source the method for preparing graphene, it is raw not to be suitable for high-volume for this method low output, higher cost
It produces.Also function dough, the functionalization degree for the graphene for having using electrochemical method the method for preparing graphene, but obtaining
It is not high.
Summary of the invention
Based on this, for the present invention it is necessary to provide a kind of function dough degree height, the more graphene quality of function is higher
Graphene preparation method.
The present invention also provides a kind of graphenes.
The present invention also provides a kind of applications of graphene.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of preparation method of graphene, includes the following steps:
Using ionic liquid as electrolyte, insertion graphite electrode is as anode and metal electrode or non-metal electrode as yin
Pole;
The voltage or density for applying 0.5V-10V between the cathode and the anode are 1mA/cm2-100mA/cm2's
Electric current, electrochemical reaction preset time, obtains reaction product;
The reaction product is post-processed, thin graphene is obtained.
The preparation method of above-mentioned graphene, using ionic liquid as electrolyte, in addition after anode, cathode and energization, hair
Raw electrochemical reaction, is made thin graphene, the quality of the graphene is higher, according to the different available a variety of officials of ionic liquid
The graphene of the graphene that can be rolled into a ball, different functional groups has different function, can be applied to a variety of occasions.
In some of embodiments, the ionic liquid is 1- ethyl-3-methylimidazole bromide, 1- ethyl -3- methyl miaow
Azoles villaumite, 1- ethyl-3-methylimidazole salt compounded of iodine, 1- ethyl -2,3- methylimidazole fluoroform sulphonate, 1,2- diethyl -3-
Methylimidazole fluoroform sulphonate, 1,2- dimethyl -3- ethyl imidazol(e) bromide, 1,2- dimethyl -3- ethyl imidazol(e) villaumite and 1,
One or more of 2- dimethyl -3- ethyl imidazol(e) tetrafluoroborate.
In some of embodiments, the ionic liquid is 1- ethyl-3-methylimidazole bromide.
In some of embodiments, the time of the electrochemical reaction is 0.5h-5h.
In some of embodiments, the graphite electrode is formed by pressing expanded graphite.
In some of embodiments, the shape of the graphite electrode is rodlike, banding or sheet.
In some of embodiments, the metal electrode is copper electrode, silver electrode, platinum electrode, gold electrode, Ti electrode or lead
Electrode, the non-metal electrode are carbon electrode, calomel electrode or hydrogen electrode.
In some of embodiments, the post-processing approach of the reaction product are as follows: the reaction product is washed, mistake
One or more of filter, ultrasound and drying.
The present invention also provides a kind of graphenes, are made of the preparation method of the graphene.
The present invention also provides the application of the graphene described in one kind in the battery.
Detailed description of the invention
Fig. 1 is the structure chart of the SEM characterization of graphene described in one embodiment of the invention;
Fig. 2 is the structure chart of the SEM characterization of graphene described in comparative example of the invention.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted
Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes
It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The present invention provides a kind of preparation method of graphene, includes the following steps:
Using ionic liquid as electrolyte, insertion graphite electrode is as anode and metal electrode or non-metal electrode as yin
Pole;
The voltage or density for applying 1V-10V between a cathode and an anode are 1mA/cm2-100mA/cm2Electric current, electrochemistry
Preset time is reacted, reaction product is obtained;
Reaction product is post-processed, thin graphene is obtained.
Ionic liquid therein is 1- ethyl-3-methylimidazole bromide, 1- ethyl-3-methylimidazole villaumite, 1- ethyl -3-
Methylimidazole salt compounded of iodine, 1- ethyl -2,3- methylimidazole fluoroform sulphonate, 1,2- diethyl -3- methylimidazole trifluoro methylsulphur
Hydrochlorate, 1,2- dimethyl -3- ethyl imidazol(e) bromide, 1,2- dimethyl -3- ethyl imidazol(e) villaumite and 1,2- dimethyl -3- ethyl miaow
One or more of azoles tetrafluoroborate.Single ionic liquid can be chosen, the cooperation of different kinds of ions liquid can also be chosen
Together, different ionic liquids is chosen, the ion provided is different, and ionic liquid forms electrolytic ion under the action of electrolysis.It adopts
With above-mentioned ionic liquid, the peel force relative to common lye electrolyte, the ion pair graphite material of electrolysis is stronger, makes
The graphene as thin layer can more completely be removed by obtaining graphite material.Mainly there are carboxyl, hydroxyl, carbonyl in the functional group of graphene
Base, epoxy group and some peroxide can obtain the graphite of different function according to the difference of ionic liquid with controllable preparation
Alkene.Such as: oxygen-containing functional group such as carbonyl, epoxy and peroxide etc. make graphene have strong oxidizing property, may act as oxidant ginseng
With oxidation reaction;Diketone-glycol oxidation reduction in grapheme material is anti-to the oxidative dehydrogenation for being widely used in gas phase in recent years
Answer, wherein mostly important industrial application first is that dehydrogenation of ethylbenzene generate styrene;Carboxylic acid acidic functionality in graphene
So that graphene has acidity, it can be used as solid acid catalyst and upgrade applied to acid catalysis organic reaction and bio-fuel;Stone
The Defect Edge of black alkene can accommodate a series of unique functional groups such as acid, carbonyl, single electron free radical and halogen, have
Huge catalytic applications potential;The two-dimensional stage of graphene can also be modified through non-covalent, and it is multiple to obtain graphene
Condensation material can be used as synergistic catalyst and react applied to green catalysis.
The time of above-mentioned electrochemical reaction is 0.5h-5h, such as reaction 0.5h, 1h, 1.5h, 3h, 4h and 5h, when reaction
Between with react complete until.
Graphite electrode therein is preferably formed by pressing expanded graphite, and the effect that it is removed under the effect of electrolysis is more
It is good, thin graphene more easily generated.
The shape of graphite electrode is rodlike, banding or sheet, and the shape of graphite influences the generation of graphene smaller.It is preferred that
For using the graphite of sheet, peeling effect is preferable.
Metal electrode is copper electrode, silver electrode, platinum electrode, gold electrode, Ti electrode or lead electrode, and non-metal electrode is carbon electricity
Pole, calomel electrode or hydrogen electrode.
The post-processing approach of reaction product are as follows: reaction product is washed, is filtered and one or more of ultrasound, is led to
Cross washing and can wash away the sundries of the attachment of graphene during the reaction, filtering can reduce sundries in graphene, using super
The method of sound can remove the sundries in graphene substantially, obtain pure grapheme material.
After the completion of reaction product post-processing, table can be carried out by structure of the scanning electron microscope (SEM) to graphene
Sign, observes the number of plies of graphene.
The present invention also provides a kind of graphenes, are made of the preparation method of above-mentioned graphene.
The present invention also provides a kind of application of above-mentioned graphene in the battery, i.e. the graphene uses and is mainly used in electricity
Pond field is fabricated to the electrode of lithium battery.
Certainly, above-mentioned graphene can also be applied to high-performance nanometer electronic device, photoelectric device, gas sensor, answer
Condensation material, field emmision material and energy stores lamp field are not limited to be applied to battery.
The preparation method of above-mentioned graphene, using ionic liquid as electrolyte, in addition after anode, cathode and energization, hair
Raw electrochemical reaction, is made thin graphene, the quality of the graphene is higher, according to the different available a variety of officials of ionic liquid
The graphene of the graphene that can be rolled into a ball, different functional groups has different function, can be applied to a variety of occasions.
Hereinafter embodiments of the present invention will be further illustrated using several embodiments.
Embodiment one
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1- ethyl-3-methylimidazole bromide
As ionic liquid, the electrode being fabricated to using the graphite paper (phosphorus content 99%) of 200mm*200mm is as anode, with 2mm*2mm's
Platinized platinum is inserted into above-mentioned ionic liquid as cathode, above-mentioned anode and cathode with the gap of 70mm, anode and cathode it
Between apply 5V voltage, graphite paper under the action of electrolytic ion and electric field, lamellar structure open, gradually cracking become thin layer stone
Black alkene reacts completion after reacting 1.5h, collects the reaction product in liquid, first washed, be ultrasonically treated after filtering, most
It is placed in 55 DEG C of environment and dries, obtain brominated thin graphene powder.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, graphene
Shape appearance figure referring to Fig.1, the pattern with typical graphene.
Embodiment two
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1- ethyl-3-methylimidazole villaumite
As ionic liquid, using the electrode that high purity graphite item (phosphorus content 99%) is fabricated to as anode, using the platinized platinum of 2mm*2mm as yin
Pole, above-mentioned anode and cathode are inserted into above-mentioned ionic liquid with the gap of 70mm, apply 5V's between the anode and cathode
Voltage, graphite paper under the action of electrolytic ion and electric field, open by lamellar structure, and gradually cracking becomes thin graphene, reaction
It reacts and completes after 2h, collect the reaction product in liquid, first washed, be ultrasonically treated after filtering, be finally placed in 55 DEG C
It is dried in environment, obtains the thin graphene powder containing chlorine.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Embodiment three
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1- ethyl-3-methylimidazole bromide
Ionic liquid is made into the volume ratio of 1:1 with 1- ethyl -2,3- methylimidazole fluoroform sulphonate, it is (carbon containing with high purity graphite piece
The electrode 99%) being fabricated to is measured as anode, using the copper sheet of 2mm*2mm as cathode, above-mentioned anode and cathode is with 50mm's
Gap is inserted into above-mentioned ionic liquid, applies the voltage of 10V between the anode and cathode, graphite paper is in electrolytic ion and electric field
Under the action of, lamellar structure is opened, and gradually cracking becomes thin graphene, and reaction is completed after reacting 1h, is collected anti-in liquid
Product is answered, is first washed, is ultrasonically treated after filtering, is finally placed in 55 DEG C of environment and dries, is obtained brominated and sulfonated
Thin graphene powder.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Example IV
The present invention provides a kind of preparation method of graphene, includes the following steps: 1,2- dimethyl -3- ethyl imidazol(e) bromide
Ionic liquid is made into the volume ratio of 1:2 with 1,2- dimethyl -3- ethyl imidazol(e) villaumite, with high purity graphite piece (phosphorus content 99%) system
The electrode being made is as anode, and using the copper sheet of 2mm*2mm as cathode, above-mentioned anode and cathode is inserted into the gap of 50mm
In above-mentioned ionic liquid, between the anode and cathode apply 10V voltage, graphite paper under the action of electrolytic ion and electric field,
Lamellar structure is opened, and gradually cracking becomes thin graphene, and reaction is completed after reacting 1h, collects the reaction product in liquid, first
It is washed, is ultrasonically treated after filtering, be finally placed in 55 DEG C of environment and dry, obtain the thin graphene powder containing chlorine and bromine
End.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Embodiment five
The present invention provides a kind of preparation method of graphene, includes the following steps: 1- ethyl -2,3- methylimidazole trifluoro
Mesylate is as ionic liquid, using the electrode that high purity graphite piece (phosphorus content 99%) is fabricated to as anode, with the copper of 2mm*2mm
Piece is inserted into above-mentioned ionic liquid as cathode, above-mentioned anode and cathode with the gap of 50mm, between the anode and cathode
Apply the voltage of 3V, graphite paper under the action of electrolytic ion and electric field, open by lamellar structure, and gradually cracking becomes thin layer graphite
Alkene reacts completion after reacting 3h, collects the reaction product in liquid, first washed, be ultrasonically treated after filtering, most postposition
It is dried in 55 DEG C of environment, obtains sulfonated thin graphene powder.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Embodiment six
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1- ethyl-3-methylimidazole villaumite
As ionic liquid, the electrode being fabricated to using the graphite paper (phosphorus content 99%) of 200mm*200mm is as anode, with 2mm*2mm's
Platinized platinum is inserted into above-mentioned ionic liquid as cathode, above-mentioned anode and cathode with the gap of 70mm, anode and cathode it
Between apply 50mA/cm2Electric current, graphite paper under the action of electrolytic ion and electric field, lamellar structure open, gradually cracking become
Thin graphene reacts completion after reacting 1.5h, collects the reaction product in liquid, first washed, ultrasound is carried out after filtering
Processing, is finally placed in 55 DEG C of environment and dries, obtain the thin graphene powder containing chlorine.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Embodiment seven
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1,2- diethyl -3- methylimidazole
Fluoroform sulphonate is as ionic liquid, and the electrode being fabricated to using high purity graphite piece (phosphorus content 99%) is as anode, with 2mm*2mm
Platinized platinum as cathode, above-mentioned anode and cathode is inserted into above-mentioned ionic liquid with the gap of 40mm, in anode and cathode
Between apply 100mA/cm2Electric current, graphite paper under the action of electrolytic ion and electric field, lamellar structure open, gradually crack
As thin graphene, completion is reacted after reacting 1.5h, the reaction product in liquid is collected, is first washed, carried out after filtering
Ultrasonic treatment, is finally placed in 55 DEG C of environment and dries, obtain the thin graphene powder of sulfonic fluoropolymer.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Embodiment eight
The present invention provides a kind of preparation method of graphene, includes the following steps: using 1,2- dimethyl -3- ethyl imidazol(e)
Tetrafluoroborate is as ionic liquid, and the electrode being fabricated to using high purity graphite piece (phosphorus content 99%) is as anode, with 2mm*2mm's
Titanium sheet is inserted into above-mentioned ionic liquid as cathode, above-mentioned anode and cathode with the gap of 40mm, anode and cathode it
Between apply 1mA/cm2Electric current, graphite paper under the action of electrolytic ion and electric field, lamellar structure open, gradually cracking become
Thin graphene reacts completion after reacting 2h, collects the reaction product in liquid, first washed, carries out at ultrasound after filtering
Reason, is finally placed in 55 DEG C of environment and dries, obtain the thin graphene powder of fluorine-containing boration.
The graphene powder that above-described embodiment is obtained is placed in progress SEM characterization in scanning electron microscope, with allusion quotation
The pattern of the graphene of type.
Comparative example
The comparative example is what is different from the first embodiment is that electrolyte uses the sodium hydroxide solution of 6mol/L, the body of electrolyte
Product is identical.
The graphene that the comparative example obtains, using SEM phenogram referring to Fig. 2, two layers of the number of plies, obtaining graphene has
Hydroxy functional group has hydrophilic nmature, may be uniformly dispersed in aqueous solution.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of graphene, which comprises the steps of:
Using ionic liquid as electrolyte, graphite electrode is inserted into as anode and metal electrode or non-metal electrode as cathode;
The voltage or density for applying 0.5V-10V between the cathode and the anode are 1mA/cm2-100mA/cm2Electric current,
Electrochemical reaction preset time, obtains reaction product;
The reaction product is post-processed, thin graphene is obtained.
2. the preparation method of graphene according to claim 1, which is characterized in that the ionic liquid is 1- ethyl -3-
Methylimidazole bromide, 1- ethyl-3-methylimidazole villaumite, 1- ethyl-3-methylimidazole salt compounded of iodine, 1- ethyl -2,3- dimethyl miaow
Azoles fluoroform sulphonate, 1,2- diethyl -3- methylimidazole fluoroform sulphonate, 1,2- dimethyl -3- ethyl imidazol(e) bromide, 1,
2- dimethyl -3- ethyl imidazol(e) villaumite and 1, one or more of 2- dimethyl -3- ethyl imidazol(e) tetrafluoroborate.
3. the preparation method of graphene according to claim 2, which is characterized in that the ionic liquid is 1- ethyl -3-
Methylimidazole bromide.
4. the preparation method of graphene according to claim 1, which is characterized in that the time of the electrochemical reaction is
0.5h-5h。
5. the preparation method of graphene according to claim 1, which is characterized in that the graphite electrode is by expanded graphite pressure
System is formed.
6. the preparation method of graphene according to claim 1 or 5, which is characterized in that the shape of the graphite electrode is
Rodlike, banding or sheet.
7. the preparation method of graphene according to claim 1, which is characterized in that the metal electrode is copper electrode, silver
Electrode, platinum electrode, gold electrode, Ti electrode or lead electrode, the non-metal electrode are carbon electrode, calomel electrode or hydrogen electrode.
8. the preparation method of graphene according to claim 1, which is characterized in that the post-processing approach of the reaction product
Are as follows: the reaction product is washed, is filtered, ultrasound and drying one or more of.
9. a kind of graphene, which is characterized in that be made of the preparation method of the described in any item graphenes of claim 1-8.
10. a kind of application of graphene as claimed in claim 9 in the battery.
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CN114032560A (en) * | 2021-11-05 | 2022-02-11 | 安庆师范大学 | Graphene and preparation method thereof |
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