CN110364731A - A kind of graphene conductive slurry - Google Patents
A kind of graphene conductive slurry Download PDFInfo
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- CN110364731A CN110364731A CN201810312296.9A CN201810312296A CN110364731A CN 110364731 A CN110364731 A CN 110364731A CN 201810312296 A CN201810312296 A CN 201810312296A CN 110364731 A CN110364731 A CN 110364731A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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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 present invention proposes a kind of graphene conductive slurry, is made of graphene and solvent, and the graphene thickness has 1-10 layers, and a small amount of alkali metal or alkali metal compound are contained in graphene, and the quality of alkali metal accounts for the 0.01-10% of the graphene quality of the alkali metal containing；The alkali metal is one or more of lithium, sodium, potassium.The present invention also proposes the application of the graphene conductive slurry.The graphene that the present invention uses alkali metal graft process to prepare is raw material；Electrocondution slurry component is simple, does not need other additives, and electrocondution slurry preparation method is simple, environmental-friendly, and gained electrocondution slurry preparation method is suitable for large scale preparation.
Description
Technical field
The invention belongs to field of energy source materials, and in particular to a kind of electrocondution slurry and its application for secondary cell.
Background technique
The electrode active material of secondary cell lower for conductivity, low conductivity can greatly limit secondary cell
High magnification under charge-discharge performance.Therefore, usually required when preparing electrode by these active materials be added conductive agent
Improve its electric conductivity.Electrode material preferable for some electric conductivity undergoes generally existing volume after multiple charge and discharge swollen
Swollen blockage effect reduces the contact between electrode material granules, it is thus typically necessary to which amount of conductive agent is added to maintain it
Structural stability.
Searching electric conductivity is excellent and the conductive agent of perfect conductive network can be constructed in active material for realizing
Chemical property under higher energy density and high magnification is particularly important.Graphene is a kind of New Two Dimensional nano material, tool
There are excellent electric conductivity, the electron mobility of superelevation, thermal conductivity, and specific surface area is larger, after it disperses in active material
It will be a kind of conductive agent of great application prospect.Dispersed to prepare electrocondution slurry, good three-dimensional conductive can be formed
Network, can effectively shorten the transmission path of battery charge and discharge process intermediate ion and electronics, the transmission speed both accelerated, this for
High rate performance, cycle life, the charging rate for improving battery are of great significance.But there are stronger π-π between graphene layer
Interaction force, the graphene peeled away can usually reunite in storage and use process, therefore the dispersion one of graphene
It is directly a great problem for hindering its application.It in summary it can be seen, the complete graphene of preparation structure and be stably dispersed in slurry
It is key point of the graphene as lithium ion battery conductive agent in material.
Summary of the invention
For shortcoming existing for this field, the purpose of the present invention is to provide a kind of graphene conductive slurries.
Second object of the present invention is to propose the application of the graphene conductive slurry.
Realize the technical solution of above-mentioned purpose of the present invention are as follows:
A kind of graphene conductive slurry, is made of graphene and solvent, and the graphene thickness has 1~10 layer, graphene
In contain a small amount of alkali metal or alkali metal compound, the quality of alkali metal account for the graphene quality of the alkali metal containing 0.01~
10%；The alkali metal is one or more of lithium, sodium, potassium.
Wherein, the solvent is N-Methyl pyrrolidone, dimethylformamide, water, ethyl alcohol, methanol, one in isopropanol
Kind is a variety of.
Wherein, the mass ratio of the graphene and solvent is 1~10:99~90.
Preferably, the mass ratio of the graphene and solvent is 1~5:99~95.
In the graphene conductive slurry, the graphene is prepared by the following method:
(1) in inert environments, graphite-like raw material and alkali metal are mixed, obtain uniformly mixed graphite-like carbon
Material-alkali metal composite material, and stood in inert environments, make that metal intercalation reaction occurs, until composite material is by black
Become golden yellow；
(2) resulting composite material is put into the liquid medium that can be reacted and is reacted, remove intercalation object,
By shaking or removing, clean, separate, grapheme material is obtained.
Wherein, in step (1), the alkali metal is one or more of lithium, sodium, potassium；The graphite-like former material
Material is natural or artificial graphite, is particularly preferred as graphite paper, graphite powder, crystalline flake graphite, expanded graphite, spherical graphite, height
One of directional thermal decomposition graphite is a variety of.
Wherein, in step (1), the inert environments are argon atmosphere or helium atmosphere, are stood in inert environments to sample
Product become golden yellow, and time of repose is in 10h or more.
Wherein, in step (2), the liquid medium be water, methanol, ethyl alcohol, propyl alcohol, n-butanol, ethylene glycol, formic acid,
One of acetic acid, propionic acid, hydrochloric acid are a variety of.
The graphene conductive slurry is to obtain graphene dispersion in a solvent, and dispersing method includes stirring, surpasses
One of sound, concussion are a variety of.
Application of the graphene conductive slurry of the present invention in secondary cell preparation.
Compared with prior art, the present invention has following major advantage:
(1) graphene that the present invention uses alkali metal graft process to prepare is raw material；(2) electrocondution slurry component is simple, is not required to
Want other additives；(3) electrocondution slurry preparation method is simple, environmental-friendly；(4) gained electrocondution slurry preparation method is suitable for big
Scale preparation.
To sum up, graphene conductive slurry of the invention has good electric conductivity, is easy to be formed with active material good
Conductive network improves electrocondution slurry stability, so that battery has the electrochemistries such as excellent cycle life, energy density
Energy；In addition, electrocondution slurry preparation method repeatability is high, process is simple, it is time-consuming less, it is environmental-friendly, be suitable for industrialized production.
Detailed description of the invention
Fig. 1 is graphene conductive slurry material object photo in the present invention.
Fig. 2 is the SEM figure of the graphene conductive slurry of embodiment 1.
Fig. 3 is that the atom of graphene in the graphene conductive slurry of embodiment 1 is tried hard to.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip
Part or according to the normal condition proposed by manufacturer.Unless otherwise stated, otherwise percentage and number are calculated by weight.
Unless otherwise defined, it anticipates known to all professional and scientific terms as used herein and one skilled in the art
Justice is identical.In addition, any method similar to or equal to what is recorded and material can be applied to the method for the present invention.Wen Zhong
The preferred implement methods and materials are for illustrative purposes only.
Embodiment 1:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) graphite powder and lithium metal are mixed in argon atmosphere with the ratio of mass ratio 6:1, first passing through heating will
Lithium adds graphite powder and is stirred after melting, until graphite powder and lithium metal are placed in after evenly mixing in argon atmosphere, to place 24 small
When, gained mixture becomes golden yellow；
(2) above-mentioned golden yellow composite material is taken out from argon atmosphere, is put into ethyl alcohol (analysis is pure), intercalation metal is fast
Speed and ethanol synthesis generate gas, and composite material expands rapidly, and dispersion is in ethanol.Solution is ultrasonically treated one after the reaction was completed
Solution is cleaned repeatedly after hour, filters isolated grapheme material.
(3) it by 5 parts of above-mentioned graphene additions, 95 parts of (mass ratio) N-Methyl pyrrolidones, is then ultrasonically treated, obtains
Uniform solution, as gained electrocondution slurry.Change the ratio of graphene and solvent, 1~10 part and 90~99 parts N- of graphene
The slurry of methyl pyrrolidone has same performance.
The pattern of resulting materials is characterized, as a result referring to Fig. 1 and Fig. 2.Fig. 1 is the appearance photo of slurry, graphene
It is evenly dispersed in a solvent and to stablize and kept for 6 months or more, no sedimentation phenomenon.Fig. 2 shows graphene, and there is no stacking, rulers
Very little size is several microns.Fig. 3 shows that the thickness of graphene in this experiment, thickness are about 3nm.
Embodiment 2
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) graphite powder and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 6:1, first passes through and adds
Heat is added graphite powder after melting lithium and is stirred, until graphite powder and lithium metal are placed in inert atmosphere place 24 after evenly mixing
Object to be mixed becomes golden yellow after hour；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into ethyl alcohol (analysis is pure), intercalation metal is fast
Speed and ethanol synthesis generate gas, and composite material expands rapidly, and dispersion is in ethanol.Solution is ultrasonically treated one after the reaction was completed
Solution is cleaned repeatedly after hour, filters isolated grapheme material.
(3) it by 2 parts of above-mentioned graphene additions, 98 parts of N-Methyl pyrrolidones, then stirs, obtains uniform solution, i.e.,
For gained electrocondution slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.Change graphene and solvent
Ratio, the slurry of 1~10 part and 90~99 parts N-Methyl pyrrolidone of graphene has same performance.
Embodiment 3
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) graphite powder and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 6:1, first passes through and adds
Heat is added graphite powder after melting lithium and is stirred, until graphite powder and lithium metal are placed in inert atmosphere place 24 after evenly mixing
Become golden yellow to said mixture after hour；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into ethyl alcohol (analysis is pure), intercalation metal is fast
Speed and ethanol synthesis generate gas, and composite material expands rapidly, and dispersion is in ethanol.Solution is ultrasonically treated one after the reaction was completed
Solution is cleaned repeatedly after hour, filters isolated grapheme material.
(3) by 10 parts of above-mentioned graphene additions, 90 parts of N-Methyl pyrrolidones, then concussion is handled, and is obtained uniform molten
Liquid, as gained electrocondution slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.
Embodiment 4
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) graphite powder and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 6:1, first passes through and adds
Heat is added graphite powder after melting lithium and is stirred, until graphite powder and lithium metal are placed in inert atmosphere place 24 after evenly mixing
Become golden yellow to said mixture after hour；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into ethyl alcohol (analysis is pure), intercalation metal is fast
Speed and ethanol synthesis generate gas, and composite material expands rapidly, and dispersion is in ethanol.Solution is ultrasonically treated one after the reaction was completed
Solution is cleaned repeatedly after hour, filters isolated grapheme material.
(3) it by 5 parts of above-mentioned graphene additions, 95 parts of deionized waters, is then ultrasonically treated, obtains uniform solution, as
Gained electrocondution slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.Change graphene and solvent
Ratio, the slurry of 1~10 part and 90~99 parts water of graphene has same performance.
Embodiment 5:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) crystalline flake graphite and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 5:1, is rolled over repeatedly
Folded roll-in, becomes until crystalline flake graphite and lithium metal are placed in inert atmosphere after evenly mixing after placing 48 hours to said mixture
It is golden yellow；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into the aqueous hydrochloric acid solution of 0.1mol/L, inserts
Layer metal is quickly and solution reaction generates gas, and composite material is expanded rapidly, is dispersed in aqueous hydrochloric acid solution.After the reaction was completed will
Solution cleans solution after being ultrasonically treated one hour repeatedly, filters isolated grapheme material.
(3) it by 5 parts of above-mentioned graphene additions, 95 parts of dimethylformamides, then stirs, obtains uniform solution, as
Gained electrocondution slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.Change graphene and solvent
Ratio, the slurry of 1~10 part and 90~99 parts dimethylformamide of graphene has same performance.
Embodiment 6:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) expanded graphite and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 3:1, is rolled over repeatedly
Folded roll-in, becomes until crystalline flake graphite and lithium metal are placed in inert atmosphere after evenly mixing after placing 48 hours to said mixture
It is golden yellow；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into acetic acid (analysis is pure), intercalation metal is fast
Speed and acetic acidreaction generate gas, and composite material is expanded rapidly, is dispersed in acetic acid.Solution is ultrasonically treated one after the reaction was completed
Solution is cleaned repeatedly after hour, filters isolated grapheme material.
(3) it by 4 parts of above-mentioned graphene additions, 96 parts of dimethylformamides, then stirs, obtains uniform solution, as
Gained electrocondution slurry.
Embodiment 7:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) crystalline flake graphite and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 5:1, uses roll-in
The folding roll-in of machine, until crystalline flake graphite and lithium metal are placed in inert atmosphere after placing 48 hours after evenly mixing to above-mentioned mixed
It closes object and becomes golden yellow；
(2) above-mentioned golden yellow composite material is taken out from inert environments, into the water, intercalation metal is quickly reacted with water
Gas is generated, composite material is expanded rapidly, is dispersed in water.It reacts after solution is ultrasonically treated one hour by 30s after the completion to molten
Liquid is cleaned repeatedly, filters isolated grapheme material.
(3) it by 2 parts of above-mentioned graphene additions, 98 parts of ethyl alcohol, then stirs, obtains uniform solution, as gained is conductive
Slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.
Embodiment 8:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) graphite powder and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 8:1, it is folding
Roll-in, until graphite powder and lithium metal, which are placed in inert atmosphere after evenly mixing after placing 48 hours, becomes golden yellow to said mixture
Color；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into flask, water is slowly introducing into flask
Steam is further expanded after vapor and volume after the raw lithium hydroxide of intercalation metal slow reaction, is about taken out after 2h；
(3) above-mentioned product is put into formic acid (analysis is pure), intercalation reacts with formic acid, and composite material expansion exists
30s in formic acid.Solution is cleaned repeatedly after solution is ultrasonically treated one hour after the reaction was completed, filters isolated graphite
Alkene material.
(4) it by 5 parts of above-mentioned graphene additions, 95 parts of ethyl alcohol, then stirs, obtains uniform solution, as gained is conductive
Slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.
Embodiment 9:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) expanded graphite and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 10:1, repeatedly
Rolling is folded, is become until expanded graphite and lithium metal are placed in inert atmosphere after evenly mixing after placing 48 hours to said mixture
At golden yellow；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into flask, argon is slowly introducing into flask
Gas-acetic acid gaseous mixture (acetic acid is brought into Ar, estimates the total charge volume ratio of acetic acid Zhan between 1%~10%), it is to be mixed
Acetic acid is further expanded with volume after the raw lithium acetate of intercalation metal slow reaction in gas；
(3) into the water by above-mentioned product, intercalation reacts with water, and composite material expansion is in water after about 1min
In.Solution is cleaned repeatedly after solution is ultrasonically treated one hour after the reaction was completed, filters isolated grapheme material.
(4) it by 5 parts of above-mentioned graphene additions, 95 parts of methanol, then stirs, obtains uniform solution, as gained is conductive
Slurry.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.
Embodiment 10:
Present embodiments provide a kind of graphene conductive slurry.The operation for preparing this graphene conductive slurry is as follows:
(1) expanded graphite and lithium metal are mixed in inert environments argon gas with the ratio of mass ratio 10:1, repeatedly
Rolling is folded, is become until expanded graphite and lithium metal are placed in inert atmosphere after evenly mixing after placing 48 hours to said mixture
At golden yellow；
(2) above-mentioned golden yellow composite material is taken out from inert environments, is put into flask, argon is slowly introducing into flask
Gas-ethyl alcohol gaseous mixture (the total charge volume ratio of acetic acid Zhan be 1%~10% between), ethyl alcohol and intercalation metal are slow in gas to be mixed
Volume further expands after reacting raw lithium ethoxide；
(3) into the water by above-mentioned product, intercalation reacts with water, and composite material expansion is in water.It has reacted
Solution is cleaned repeatedly after being ultrasonically treated solution one hour after, filters isolated grapheme material.
(4) it by 5 parts of above-mentioned graphene additions, 95 parts of isopropanols, then stirs, obtains uniform solution, as gained is led
Plasma-based material.
Graphene uniform disperses in a solvent and stablizes holding 6 months or more, no sedimentation phenomenon.
The present invention is difficult to disperse for graphene conductive agent in existing electrocondution slurry, need to add dispersing agent, electrocondution slurry system
The problem of standby complex process, obtains having good electric conductivity by using graphene prepared by alkali metal graft process, be easy to
Active material forms good conductive network, improves electrocondution slurry stability, so that battery has excellent cycle life, energy
The chemical properties electrocondution slurry such as metric density；Meanwhile electrocondution slurry preparation method repeatability is high, process is simple, it is time-consuming less, ring
Border is friendly, is suitable for industrialized production.This has very heavy to the development for pushing secondary cell and the problems such as solving energy shortage
The meaning wanted.
Above embodiment be only preferred embodiments of the present invention will be described, not to the scope of the present invention into
Row limits, and without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to technical side of the invention
The all variations and modifications that case is made, should fall within the scope of protection determined by the claims of the present invention.
Claims (10)
1. a kind of graphene conductive slurry, which is characterized in that be made of graphene and solvent, the graphene thickness has 1~10
Layer, a small amount of alkali metal or alkali metal compound are contained in graphene, the quality of alkali metal accounts for the graphene matter of the alkali metal containing
The 0.01~10% of amount；The alkali metal is one or more of lithium, sodium, potassium.
2. graphene conductive slurry according to claim 1, which is characterized in that the solvent be N-Methyl pyrrolidone,
One of dimethylformamide, water, ethyl alcohol, methanol, isopropanol are a variety of.
3. graphene conductive slurry according to claim 1, which is characterized in that the mass ratio of the graphene and solvent
For 1~10:99~90.
4. graphene conductive slurry according to claim 3, which is characterized in that the mass ratio of the graphene and solvent
For 1~5:99~95.
5. graphene conductive slurry according to any one of claims 1 to 4, which is characterized in that the graphene by with
The preparation of lower section method:
(1) in inert environments, graphite-like raw material and alkali metal are mixed, obtain uniformly mixed graphite-like carbon materials
Material-alkali metal composite material, and stood in inert environments, make that metal intercalation reaction occurs, until composite material is become by black
At golden yellow；
(2) resulting composite material is put into the liquid medium that can be reacted and is reacted, remove intercalation object, passed through
Concussion or removing, cleaning, separation, obtain graphene.
6. graphene conductive slurry according to claim 5, which is characterized in that in step (1), the alkali metal be lithium,
One or more of sodium, potassium；The graphite-like raw material are natural or artificial graphite, preferably graphite paper, stone
One of ink powder, crystalline flake graphite, expanded graphite, spherical graphite, highly oriented pyrolytic graphite are a variety of.
7. graphene conductive slurry according to claim 5, which is characterized in that in step (1), the inert environments are argon
Gas atmosphere or helium atmosphere stand to sample in inert environments and become golden yellow, and time of repose is in 10h or more.
8. graphene conductive slurry according to claim 5, which is characterized in that in step (2), the liquid medium is
One of water, methanol, ethyl alcohol, propyl alcohol, n-butanol, ethylene glycol, formic acid, acetic acid, propionic acid, hydrochloric acid are a variety of.
9. described in any item graphene conductive slurries according to claim 1~8, which is characterized in that be that graphene dispersion exists
It is obtained in solvent, dispersing method includes one of stirring, ultrasound, concussion or a variety of.
10. the application of graphene conductive slurry according to any one of claims 1 to 9 in the secondary battery.
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Application publication date: 20191022 |