CN107316978A - Conductive slurry of a kind of lithium battery special graphite alkene and preparation method thereof - Google Patents
Conductive slurry of a kind of lithium battery special graphite alkene and preparation method thereof Download PDFInfo
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- CN107316978A CN107316978A CN201710467707.7A CN201710467707A CN107316978A CN 107316978 A CN107316978 A CN 107316978A CN 201710467707 A CN201710467707 A CN 201710467707A CN 107316978 A CN107316978 A CN 107316978A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 provides conductive slurry of a kind of lithium battery special graphite alkene containing network structure and preparation method thereof.Pass through the means by mechanical stripping, graphite is set to be thinned to the graphene of Nano grade, by being modified and being crosslinked to graphenic surface under enough fineness and homogeneous condition, obtain the graphene of network structure, and dispersant formation graphene conductive slurry is used in thinning process, the graphene conductive slurry is used to be easily dispersed in anode material of lithium battery, significantly enhance the electric conductivity and rate charge-discharge performance of electrode material, the generation of irreversible capacity is reduced, the cyclical stability of battery is added.
Description
Technical field
The invention belongs to anode material of lithium battery field, and in particular to a kind of conductive slurry of lithium battery special graphite alkene and its
Preparation method.
Background technology
As natural resources is reduced, environmental pollution is aggravated, and energy-saving and emission-reduction are assign as the breakthrough adjusted economic structure in country
In the case of mouthful, the new energy for seeking substitute fossil fuels has become focus of concern.Need of the modern society to the energy
Ask, the development of energy storage technology is greatly facilitated, lithium battery is as most successful energy storage device, because its energy density is high, use the longevity
Life is long, self-discharge rate is low, environmental suitability is strong, good cycle, high safety coefficient many advantages, such as, more and more into people
The visual field, be widely used in every field, how to prepare high-performance lithium battery have become researchers concern heat
Point, it is however generally that, in each part of lithium battery, positive electrode plays critical effect, and the performance of positive electrode is fine or not,
Directly affect the performance indications of final lithium battery.Therefore searching novel anode material is mostly important, and it will have boundless
DEVELOPMENT PROSPECT and the ever-increasing market demand.
Positive electrode should typically meet following condition：1. the compatibility with electrolyte is good, 2. good reversibility, 3. stability
It is good.Currently used for the positive electrode multiselect transition-metal oxide or transition metal phosphate of lithium battery（Such as ferric phosphate
Lithium）.The oxide of arteriopathy metal system, because on the one hand metallic atom has mixed valence, is on the other hand not susceptible to disproportionation
Reaction, in the presence of outer making alive, can quickly occur greatly redox reaction, but be due to that different metal redox is anti-
Answer current potential different, so its preparation method and use condition are widely different；Transition metal phosphate such as LiFePO4 have environmental protection,
The advantages of cyclicity is good, is considered as the good anode material of lithium battery of development prospect, but be due to that it is mostly semiconductor or exhausted
Edge body, electric conductivity is poor, it is necessary to add conductive agent to improve electric conductivity.In order to improve the electric conductivity of anode material of lithium battery, mesh
It is preceding that graphite is used for the research of conductive agent, but due to the influence such as particle diameter, pattern, surface area, dispersiveness, cause leading for graphite
Electrical property can not give full play to.
Chinese patent discloses (bulletin) number 103236290A, a kind of entitled electrocondution slurry using electrically conductive graphite powder as major ingredient
And preparation method thereof patent of invention, the disclosure of the invention is a kind of using electrically conductive graphite powder as the electrocondution slurry of major ingredient and its preparation side
Method.Modified Nano carbon is with the addition of in electrocondution slurry described in it, but electrocondution slurry prepared by the test method still can not fully be sent out
Wave its electric conductivity.
Chinese patent discloses (bulletin) number 104659334A, entitled a kind of pulp of lithium ion battery and preparation method thereof and
The patent of invention of purposes, a kind of pulp of lithium ion battery of the disclosure of the invention and its production and use.The test method system
Standby pulp of lithium ion battery, above for conductive agent, does not have with one or both of carbon black, carbon fiber, CNT or graphite
There is network structure, electric conductivity is poor.
Chinese patent is disclosed（Bulletin）Number 102263265A, entitled lithium ion battery conductive additive and preparation method thereof
Patent of invention, a kind of lithium ion battery conductive additive of the disclosure of the invention and preparation method thereof.Its described lithium ion battery
Conductive additive is graphene, is black powder of the particle diameter distribution between 10nm-100 μm, is parallel by -1000 layers of individual layer
Or the carbonaceous material constituted close to parallel graphene sheet layer, specific surface area is 50-1500m2/ g, electrical conductivity is 1 × 104-9
×104S/m.The preparation method of its lithium ion battery conductive additive, including the oxidation of graphite, the stripping of graphite oxide and
Three steps of reduction of graphene oxide, but the graphene of experimental method synthesis still contains oxygen-containing functional group, defect, sp3
Graphite oxide can not possibly be reduced to crystallize perfect graphene by the factors such as carbon hydridization, the i.e. experimental method completely, and prepare
Graphene be difficult to disperse, it is impossible to form good conductive network, electric conductivity is poor.
In summary, the positive electrode active materials currently used for lithium ion battery are generally transition metal oxide or transition gold
Belong to phosphate, because transition-metal oxide different metal redox reaction current potential is different, its preparation method and use condition
It is widely different；Because transition metal phosphate such as most of LiFePO4 is all semiconductor or insulator, electric conductivity is poor, because
And have to add conductive agent to improve electric conductivity, graphite has been used for conductive agent at present, but due to particle diameter, pattern, surface
Product, dispersiveness etc. influence, and causing the electric conductivity of graphite can not give full play to.
The content of the invention
The problem of for current anode material of lithium battery electric conductivity difference, the present invention provides a kind of lithium containing network structure
Battery special graphite alkene conduction slurry and preparation method thereof.By the means by mechanical stripping, graphite is set to be thinned to nanoscale
Other graphene, by being modified and being crosslinked to graphenic surface under enough fineness and homogeneous condition, obtains the stone of network structure
Black alkene, and using dispersant formation graphene conductive slurry in thinning process, the graphene conductive slurry is being used for lithium battery just
It is easily dispersed in the material of pole, significantly enhances the electric conductivity and rate charge-discharge performance of electrode material, reduce irreversible appearance
The generation of amount, adds the cyclical stability of battery.
To achieve these goals, the present invention uses following technical scheme：
The conductive slurry of a kind of lithium battery special graphite alkene, it is characterised in that be a kind of graphene dispersing solution containing network structure,
It is prepared from by weight by following raw material：
10-20 parts of electrically conductive graphite；
1-3 parts of dispersant；
1-3 parts of modifying agent；
1-2 parts of crosslinking agent；
70-80 parts of solvent；
Wherein, described electrically conductive graphite is crystalline flake graphite, compact crystal shape graphite, expanded graphite, thermal cracking graphite, highly oriented stone
One or more in ink；Described dispersant be Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, gelatin,
One or more in benzalkonium chloride；Described modifying agent is stearic acid, titanate coupling agent, silane coupler, Aluminate idol
Join the one or more in agent；Described crosslinking agent is acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinyl
One or more and the mixture of sulphur in benzene, N hydroxymethyl acrylamide, DAAM；Described solvent is tetrahydrochysene
Furans, 1-METHYLPYRROLIDONE, N- cyclohexyl pyrrolidones, NOP, NVP or N- 12
Alkyl pyrrolidone.
Described crosslinking agent is acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinylbenzene, N- methylols
One or more in acrylamide, DAAM are with sulphur with mass ratio 1:0.5-1 is prepared.
Further preferably, described crosslinking agent is acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinyl
One or more in benzene, N hydroxymethyl acrylamide, DAAM are with sulphur with mass ratio 1:0.5 prepares.
The conductive slurry of described lithium battery special graphite alkene, is the means fully peeled off by mechanical shearing, subtracts graphite
The graphene of Nano grade is as thin as, by being modified and being crosslinked to graphenic surface under enough fineness and homogeneous condition, is obtained
To the graphene of network structure, and the conductive slurry of lithium battery special graphite alkene in thinning process using dispersant formation, should
The specific preparation method of lithium battery special graphite conduction slurry is as follows：
（1）By electrically conductive graphite, dispersant into abrasive, it is put into grinder and is ground, further in 40-60KHz frequencies
Ultrasonic disperse 20-40min under rate, obtains dispersed mixture A；
（2）Modifying agent is added in mixture A, continuation grinds 30-60min in grinder, obtains mixture B；
（3）Crosslinking agent is added in mixture B, 30-60min is ground in continuation in grinder, while pressure is controlled in 2-3MPa,
Temperature maintains 1-2h at 120-125 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；
（4）Mixture C is well mixed with solvent, 30-40min is disperseed in homogenizer, lithium battery special graphite alkene is produced and leads
Plasma-based body.
It is preferred that, step（1）The described grinding control time is 15-45min.
It is preferred that, described grinder is disc grinder, rotary shaft grinder or gear lapping machine.
Most of positive electrode active materials currently used for lithium ion battery are all semiconductor or insulator, electric conductivity compared with
Difference, it is necessary to which adding conductive agent improves electric conductivity, improves the research of electric conductivity by adding graphite, but due to particle diameter, shape
Looks, surface area, dispersiveness etc. influence, and the electric conductivity of graphite can not give full play to.Graphene has excellent electric conductivity, but limit
In lacking network structure, therefore, the present invention provides a kind of lithium battery special graphite alkene conductive slurry, the characteristics of it is protruded is by stone
Graphene platelet is set to be cross-linked to form network by special sulfur-bearing cross-linking system in further grinding stripping process after ink stripping
Structure, and form graphene conductive slurry using dispersant in thinning process.The graphene conductive slurry is being used for lithium battery just
It is easily dispersed in the material of pole, good conductive network can be formed, Li is more beneficial for during high-multiplying power discharge+Fortune in the electrodes
It is defeated, provide convenient passage for the transport of electronics in the electrodes, and then increase the electrical conductivity of whole lithium battery anode system,
The cyclical stability of battery is added simultaneously.Consumption of this graphene conductive slurry when preparing lithium ion battery is only existing
The 50-60% of conductive agent consumption, but 2C multiplying powers improve 6-10%, save cost so that and lithium ion battery has more city
Field competitiveness.
Compared with prior art, it is as follows that it protrudes achievement to the present invention：
1st, the present invention adds modifying agent and specifically contains sulfur crosslinking agent, graphene platelet is cross-linked into network structure, the stone of preparation
The conductive slurry of black alkene is used in anode material of lithium battery the electric conductivity and rate charge-discharge performance for significantly enhancing electrode material,
The generation of irreversible capacity is reduced, the cyclical stability of battery is added.
2nd, the present invention gives full play to the electric conductivity of graphene, led so as to reduce in lithium battery by graphene networking
The application amount of electric agent.
3rd, the preparation method that the present invention is provided, the requirement ratio to equipment and raw material etc. is relatively low, and preparation process is simple and easy to apply, throws
Enter less, cost is low, be adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the network sweep electron microscope after the graphene of embodiment 1 is crosslinked.
Embodiment
Below by way of specific embodiment, the present invention will be further explained, but this should not be interpreted as into the scope of the present invention
It is only limitted to following embodiment.In the case where not departing from above method thought of the present invention, according to ordinary skill knowledge
The various replacements or change made with customary means, should be included in the scope of the present invention.
Embodiment 1
（1）The dispersant Sodium Polyacrylate of the expanded graphite of 20 parts by weight, 1 parts by weight is mixed into abrasive, disc type is put into
It is ground in grinder, further the ultrasonic disperse 20min under 40-60KHz frequencies, obtains dispersed mixture A；
（2）1 part by weight modified dose of stearic acid is added in mixture A, continuation grinds 30min in grinder, obtains mixture
B；
（3）2 parts by weight of crosslinking agent are added in mixture B, 30min is ground in continuation in grinder, while controlling pressure to exist
2MPa, temperature maintains 1h at 120 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；Crosslinking agent is propylene
Acid is with sulphur with mass ratio 1:0.5 prepares.
（4）Mixture C is well mixed with the solvents tetrahydrofurane of 70 parts by weight, 30min is disperseed in homogenizer, is produced
Lithium battery special graphite alkene conduction slurry.
The step of the present embodiment 1（3）Graphene after crosslinking connects and forms network as shown in Figure 1, between graphene film
Structure.
The present embodiment slurry is used for positive electrode LiFePO4 with 5%, is uniformly coated on metal aluminum foil, positive pole electricity is prepared
Pole, after tested, with preferable cycle life and high-rate discharge ability, such as table 1：
Embodiment 2
（1）The polyethylene of dispersing agent pyrrolidones of the crystalline flake graphite of 15 parts by weight, 1 parts by weight is mixed into abrasive, is put into and grinds
It is ground in grinding machine, further the ultrasonic disperse 40min under 60KHz frequencies, obtains dispersed mixture A；
（2）2 part by weight modified doses of titanate coupling agents are added in mixture A, continuation is ground 60min in grinder, obtained
Mixture B；
（3）1 parts by weight are added to enter crosslinking agent in mixture B, 30min is ground in continuation in grinder, while controlling pressure to exist
3MPa, temperature maintains 2h at 125 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；Crosslinking agent is N- hydroxyls
Methacrylamide is with sulphur with mass ratio 1:0.8 prepares.
（4）Mixture C is well mixed with 80 parts by weight solvent 1-METHYLPYRROLIDONEs, 40min is disperseed in homogenizer,
Produce the conductive slurry of lithium battery special graphite alkene.
The present embodiment slurry is used for positive electrode LiFePO with 5%4, it is uniformly coated on metal aluminum foil, prepares positive pole electricity
Pole, after tested, with preferable cycle life and high-rate discharge ability, such as table 1：
Embodiment 3
（1）10 parts by weight electrically conductive graphites, 2 parts per weight dispersing agent sodium carboxymethylcelluloses are mixed into abrasive, gear is put into and grinds
It is ground in grinding machine, further the ultrasonic disperse 25min under 40KHz frequencies, obtains dispersed mixture A；
（2）3 part by weight modified doses of aluminate coupling agents are added in mixture A, continuation is ground 40min in grinder, obtained
Mixture B；
（3）2 parts by weight of crosslinking agent are added in mixture B, 30min is ground in continuation in grinder, while controlling pressure to exist
2MPa, temperature maintains 1h at 120 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；Crosslinking agent is diethyl
Alkenyl benzene is with sulphur with mass ratio 1:0.5 prepares.
（4）Mixture C is well mixed with 75 parts by weight solvent NOPs, 30- is disperseed in homogenizer
40min, produces the conductive slurry of lithium battery special graphite alkene.
The present embodiment slurry is used for positive electrode LiFePO with 5%4, it is uniformly coated on metal aluminum foil, prepares positive pole electricity
Pole, after tested, with preferable cycle life and high-rate discharge ability, such as table 1：
Embodiment 4
（1）15 parts by weight expanded graphites, 2 parts per weight dispersing agent gelatin are mixed into abrasive, is put into grinder and is ground,
Further the ultrasonic disperse 40min under 60KHz frequencies, obtains dispersed mixture A；
（2）2 part by weight modified doses are added in mixture A, 60min is ground in continuation in grinder, obtains mixture B；
（3）2 parts by weight of crosslinking agent are added in mixture B, 60min is ground in continuation in grinder, while controlling pressure to exist
3MPa, temperature maintains 2h at 125 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；Connection agent is methyl-prop
Olefin(e) acid is with sulphur with mass ratio 1:0.5 prepares.
（4）Mixture C is well mixed with 80 parts by weight solvent NVPs, disperseed in homogenizer
35min, produces the conductive slurry of lithium battery special graphite alkene.
The present embodiment slurry is used for positive electrode LiFePO with 5%4, it is uniformly coated on metal aluminum foil, prepares positive pole electricity
Pole, after tested, with preferable cycle life and high-rate discharge ability, such as table 1：
Table 1：
Obviously, when using cross-linking system, acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinylbenzene, N- hydroxyls
One or more in Methacrylamide, DAAM are with sulphur with mass ratio 1:0.5 prepares, with preferable capacity
Conservation rate and high rate capability, further show that the present invention makes graphene be cross-linked to form the excellent of network for piece and led by crosslinking
Electrical property.
Those skilled in the art can to the present invention carry out it is various change and modification without departing from the present invention spirit and
Scope.So, if these modifications and variations of the present invention belong within the scope of the claims in the present invention and its equivalent technologies,
Then the present invention is also intended to comprising including these changes and modification.
Claims (5)
1. the conductive slurry of a kind of lithium battery special graphite alkene, it is characterised in that be a kind of graphene dispersion containing network structure
Liquid, is prepared from by weight by following raw material：
10-20 parts of electrically conductive graphite；
1-3 parts of dispersant；
1-3 parts of modifying agent；
1-2 parts of crosslinking agent；
70-80 parts of solvent；
Wherein, described electrically conductive graphite is crystalline flake graphite, compact crystal shape graphite, expanded graphite, thermal cracking graphite, highly oriented stone
One or more in ink；Described dispersant be Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, gelatin,
One or more in benzalkonium chloride；Described modifying agent is stearic acid, titanate coupling agent, silane coupler, Aluminate idol
Join the one or more in agent；Described crosslinking agent is acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinyl
One or more and the mixture of sulphur in benzene, N hydroxymethyl acrylamide, DAAM；Described solvent is tetrahydrochysene
Furans, 1-METHYLPYRROLIDONE, N- cyclohexyl pyrrolidones, NOP, NVP or N- 12
Alkyl pyrrolidone；
The conductive slurry of described lithium battery special graphite alkene, is prepared by the following method：
（1）By electrically conductive graphite, dispersant into abrasive, it is put into grinder and is ground, further in 40-60KHz frequencies
Ultrasonic disperse 20-40min under rate, obtains dispersed mixture A；
（2）Modifying agent is added in mixture A, continuation grinds 30-60min in grinder, obtains mixture B；
（3）Crosslinking agent is added in mixture B, 30-60min is ground in continuation in grinder, while pressure is controlled in 2-3MPa,
Temperature maintains 1-2h at 120-125 DEG C, graphene platelet is cross-linked into network structure, obtains mixture C；
（4）Mixture C is well mixed with solvent, 30-40min is disperseed in homogenizer, lithium battery special graphite alkene is produced and leads
Plasma-based body.
2. the conductive slurry of a kind of lithium battery special graphite alkene according to claim 1, it is characterised in that：Described crosslinking agent is
Acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM
In one or more with sulphur with mass ratio 1:0.5-1 is prepared.
3. the conductive slurry of a kind of lithium battery special graphite alkene according to claim 1, it is characterised in that：Described crosslinking agent is
Acrylic acid, methacrylic acid, hydroxyethyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM
In one or more with sulphur with mass ratio 1:0.5 prepares.
4. the conductive slurry of a kind of lithium battery special graphite alkene according to claim 1, it is characterised in that：Step（1）Described
The grinding control time is 15-45min.
5. the conductive slurry of a kind of lithium battery special graphite alkene according to claim 1, it is characterised in that：Described grinder is
Disc grinder, rotary shaft grinder or gear lapping machine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109147988A (en) * | 2018-08-02 | 2019-01-04 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of thin graphene slurry |
| CN112768691A (en) * | 2020-12-31 | 2021-05-07 | 宁波杉杉新材料科技有限公司 | Coating agent, coating modified graphite negative electrode material, preparation method and application thereof, and lithium ion battery |
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| CN109147988A (en) * | 2018-08-02 | 2019-01-04 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of thin graphene slurry |
| CN112768691A (en) * | 2020-12-31 | 2021-05-07 | 宁波杉杉新材料科技有限公司 | Coating agent, coating modified graphite negative electrode material, preparation method and application thereof, and lithium ion battery |
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| CN107316978B (en) | 2020-04-17 |
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