CN108183223A - A kind of electrocondution slurry of carbon nanotube, graphene and conductive black compounding and preparation method thereof - Google Patents

A kind of electrocondution slurry of carbon nanotube, graphene and conductive black compounding and preparation method thereof Download PDF

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Publication number
CN108183223A
CN108183223A CN201711482716.XA CN201711482716A CN108183223A CN 108183223 A CN108183223 A CN 108183223A CN 201711482716 A CN201711482716 A CN 201711482716A CN 108183223 A CN108183223 A CN 108183223A
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graphene
carbon nanotube
preparation
electrocondution slurry
conductive black
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CN108183223B (en
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王昆明
张晓鸿
耿超
杨兴振
于大周
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Qingdao Haoxin New Energy Technology Co Ltd
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Qingdao Haoxin New Energy Technology Co Ltd
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Priority to PCT/CN2018/125008 priority patent/WO2019129228A1/en
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • 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

Electrocondution slurry the invention discloses a kind of carbon nanotube, graphene and conductive black compounding and preparation method thereof, wherein preparation method includes the following steps：In the solvent containing dispersant, graphene, carbon nanotube and conductive black are added in, and disperseed, obtain the electrocondution slurry；The dispersant is by high molecular polymer, anion surfactant, non-ionic wetting agent and antifoaming agent with weight ratio 1：0.3~0.7：0.3~0.7：0.05~0.1 mixture forms.The electrocondution slurry of carbon nanotube provided by the invention, graphene and conductive black compounding, preparation method is simple, at low cost, and stability is good, and electric conductivity is good.

Description

A kind of carbon nanotube, the electrocondution slurry of graphene and conductive black compounding and its preparation Method
Technical field
The present invention relates to conductive material technical fields, and in particular to a kind of carbon nanotube, graphene and conductive black compounding Electrocondution slurry and preparation method thereof.
Background technology
In the prior art, when carbon nanotube is applied in lithium ion battery, since carbon nanotube is in threadiness, lithium-ion electric The positive electrode in pond is in granular form, and there is only point contacts between carbon nanotube and positive electrode, influence the conduction of lithium ion battery Performance.
Further, carbon nanotube and traditional conductive agent, such as carbon black, acetylene black, electrically conductive graphite etc. are compounded, Although electrocondution slurry can be made, Stability of Slurry is poor, and electric conductivity is also undesirable.
At present, the dispersion report about carbon nanotube, graphene and conductive black is limited.
Invention content
The present invention provides the electrocondution slurries of a kind of carbon nanotube, graphene and conductive black compounding, and preparation method is simple, At low cost, stability is good, and electric conductivity is good.
A kind of preparation method of the electrocondution slurry of carbon nanotube, graphene and conductive black compounding, which is characterized in that including Following steps：
In the solvent containing dispersant, graphene, carbon nanotube and conductive black are added in, is mixed to get slurry；It will slurry Abrasive lapping to fineness is less than 40 μm, obtains the electrocondution slurry；
The dispersant is by high molecular polymer, anion surfactant, non-ionic wetting agent and antifoaming agent with weight Than 1：0.3~0.7：0.3~0.7：0.05~0.1 mixture forms.
In the present invention, electrocondution slurry is made using the dispersant of mixture, to improve dispersion performance, obtains property stable homogeneous Electrocondution slurry.
The carbon nanotube has one dimension fibre shape structure, and line-face conductive network, graphene can be formed with composite material With two-dimensional layered structure, surface-to-surface conductive network can be formed with composite material, conductive black has zero dimension dots structure, with Composite material can form point-face conductive network, by the compounding of different carbon structures, compounding electrocondution slurry can be made to have than list The conductive network of only a kind of carbonaceous conductive agent more horn of plenty, so as to higher electrical efficiency.
Preferably, the solvent is N-Methyl pyrrolidone, deionized water, N-N dimethylacetylamides, dimethyl sulfoxide (DMSO) At least one of.
Further preferably, the solvent is water.Using water as solvent, the production cost of electrocondution slurry can be reduced, is fitted Close large-scale industrial production.
Preferably, in the solvent containing dispersant, sequentially add graphene, carbon nanotube and conductive black or Sequentially add graphene, conductive black and carbon nanotube.
The charging sequence of carbon nanotube, graphene and conductive black is carried out preferably in the present invention, first, adds in graphite Alkene, graphene carries out secondary stripping in a solvent under shearing force, obtains the lower graphene sheet layer of the number of plies, jitter time Longer, obtained graphene sheet layer is thinner, and conductive effect is better；Then carbon nanotube is added in, using high shear force to carbon nanometer Pipe is disperseed, and is effectively opened carbon nanotube aggregate, is eventually adding conductive black.
The jitter time of carbon nanotube is long, it will the length of truncating carbon nano-tubes influences electric conductivity, therefore, should not make It is added in the solvent containing dispersant for the first sequence material.
The charging sequence of conductive black and carbon nanotube can be interchanged, and not influence the performance of electrocondution slurry.
Further preferably, the dispersion linear velocity of the graphene is 10~15m/s, the jitter time of graphene for 60~ 180min；The dispersion linear velocity of the carbon nanotube is 10~15m/s, and the jitter time of carbon nanotube is 20~60min；It is described The dispersion linear velocity of conductive black is 6~12m/s, and the jitter time of conductive black is 20~30min.
In dispersion process, different material assigns optimum dispersion state in different dispersion linear velocities, graphene it is best Dispersion linear velocity is 10~15m/s, and linear velocity is too low can not to remove graphene, the excessively high sheet knot for destroying graphene of linear velocity Structure reduces electric conductivity.
Carbon nanotube optimum dispersion linear velocity is 10~15m/s, and linear velocity is too low can not to open carbon nanotube aggregate, line The excessively high destroying carbon nanometer tube length of speed reduces electric conductivity.
Conductive black optimum dispersion linear velocity is 6~12m/s, and linear velocity is too low can not to open conductive black aggregate, line Speed is excessively high to destroy conductive black branch conductive network, reduce electric conductivity.
In dispersion process, there is best requirement to jitter time, more than certain jitter time, caused under dispersion electric conductivity Drop, jitter time is very few to lead to disperse insufficient, electric conductivity decline.
During practical operation, a kind of material is often added in, i.e., according to the optimum dispersion linear velocity of the material and optimum dispersion time Disperseed, for sequentially adding graphene, carbon nanotube and conductive black, after adding in graphene, with point of 10~15m/s 60~180min of loose wire Rate Dispersion；After adding in carbon nanotube, with 20~60min of discrete lines Rate Dispersion of 10~15m/s；Add After entering conductive black, with 20~30min of discrete lines Rate Dispersion of 6~12m/s.
Type and ratio to dispersant are carried out preferably, to reach best dispersion effect.Preferably, the dispersant By high molecular polymer, anion surfactant, non-ionic wetting agent and antifoaming agent with weight ratio 1：0.3~0.7：0.3~ 0.4：0.05~0.1 mixture forms.
The high molecular polymer can be adsorbed effectively as main dispersant and wrap up carbon nanotube, graphene and lead The surface of electric carbon black prevents the cohesion between each component, dispersion is made to be in stable state.
Preferably, the high molecular polymer is polyethylene glycol, Sodium Polyacrylate, polyvinylpyrrolidone, polyphenyl sulphur At least one of sour sodium, polyimides.
The anion surfactant can be adsorbed rapidly on the surface of carbon nanotube, graphene and conductive black, High molecular polymer is assisted to be effectively disperseed.
Preferably, the anion surfactant is lauryl sodium sulfate, cetyl trimethylammonium bromide, carboxylic At least one of sodium carboxymethylcellulose pyce, naphthalene sulfonate salt.
The non-ionic wetting agent is accelerated the sympathy of conductive black surface and solvent, is improved for reducing surface tension Dispersion efficiency, and significantly improve pulp surface glossiness.
Preferably, the non-ionic wetting agent is high-carbon fatty alcohol polyoxyethylene ether.
The proportioning of each component in electrocondution slurry, for the stability of electrocondution slurry, viscosity and electric conductivity have an impact, Preferably, the carbon nanotube, graphene, conductive black, dispersant, solvent weight be 1~1.5：1.5~3：1 ~2：1~1.25：80~95.Further preferably, the carbon nanotube, graphene, conductive black, dispersant, solvent weight Part proportioning is 1.5：1.5~3：1~2：1~1.25：80~95.
In order to improve the stability of electrocondution slurry, ensure that electrocondution slurry has suitable viscosity, it is preferable that the carbon nanometer The specific surface area of pipe is not less than 270m2/g；The specific surface area of the graphene is not less than 350m2/g。
Preferably, the D of the graphene sheet layer size50It is 10~20 μm.Graphene sheet layer size is blocked up, and graphene adds Enter amount it is identical under the premise of, influence the network density of conductive grid structure, and then influence electric conductivity, graphene sheet layer size mistake It is thin, it is easily broken, conductive grid structure is equally influenced, reduces electric conductivity.
Preferably, the conductive black is at least one of acetylene black, furnace black, coke, Ketjen black.It is further excellent Choosing, the conductive black are acetylene black.
It is stirred preferably, being added in the solvent containing dispersant after carbon nanotube with the rotating speed of 180~250r/min Then at least 30min adds in graphene and stirs at least 20min with the rotating speed of 280~380r/min, is eventually adding conductive black, At least 20min is stirred with the rotating speed of 280~380r/min, obtains slurry.
Preferably, in dispersion process, slurry temperature is kept to be less than 40 DEG C.
Graphene, carbon nanotube and conductive black can be effectively scattered in the solvent containing dispersant by grinding, be formed The stable and uniform electrocondution slurry of property, electrocondution slurry is mixed with composite material (such as positive electrode of battery), in composite wood Material, carbon nanotube, graphene and between formed be provided simultaneously with point-line-surface contact conductive network, improve electric conductivity.
The present invention also provides the electrocondution slurry of a kind of carbon nanotube, graphene and conductive black compounding, using described Preparation method obtains.
The electrocondution slurry of carbon nanotube provided by the invention, graphene and conductive black compounding, stability is good, electric conductivity Good and easy to operate, production efficiency is high, it is easy to accomplish industrialized production.
Specific embodiment
Examples 1 to 6
(1) proportioning as shown in table 1 weighs each embodiment and the corresponding raw material of comparative example.
(2) under normal-temp.-dehumidifying environment (i.e. 10~30 DEG C of temperature, humidity are less than 30%R.Hs), successively by solvent and dispersion Agent is poured slowly into stirred tank, while lasting stirring, until dispersant is completely dissolved, obtains solution.
(3) first graphene is added in step (2) acquired solution and stirred, carried out after premix is uniform using high-speed dispersion equipment Dispersion, dispersion linear velocity are 12m/s, and jitter time is as shown in table 1, obtains graphene dispersing solution；
(4) in graphene dispersing solution obtained by step (3), carbon nanotube is added in, after premix is uniform, is set using high speed dispersion Standby to be disperseed, dispersion linear velocity is 15m/s, and jitter time is as shown in table 1, obtains graphene, carbon nanotube composite mortar；
(5) in graphene, carbon nanotube composite mortar obtained by step (4), conductive black is added in, after premix is uniform, is made Disperseed with high-speed dispersion equipment, dispersion linear velocity is 15m/s, and jitter time is as shown in table 1, obtains compounding electrocondution slurry.
In step (3), (4), (5), dispersion process temperature is controlled below 40 DEG C by condensing water cooling.
Table 1
In table 1, in Examples 1 to 4 and comparative example 1~2, the specific surface area of carbon nanotube is 270m2/g；Graphene Specific surface area is 350m2/g；High molecular polymer is PVP；Conductive black is Super-P conductive blacks；Anionic dispersing agents are SDS；Nonionic surfactant is OP-10；Antifoaming agent is silicone oil.

Claims (10)

1. the preparation method of the electrocondution slurry of a kind of carbon nanotube, graphene and conductive black compounding, which is characterized in that including such as Lower step：
In the solvent containing dispersant, graphene, carbon nanotube and conductive black are added in, and disperseed, obtain described lead Plasma-based material；
The dispersant is by high molecular polymer, anion surfactant, non-ionic wetting agent and antifoaming agent with weight ratio 1： 0.3~0.7：0.3~0.7：0.05~0.1 mixture forms.
2. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the solvent is N- crassitudes At least one of ketone, deionized water, N-N dimethylacetylamides, dimethyl sulfoxide (DMSO)；The conductive black for acetylene black, furnace black, At least one of coke, Ketjen black.
3. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the high molecular polymer is poly- second two At least one of alcohol, Sodium Polyacrylate, polyvinylpyrrolidone, polyphenyl sodium sulfonate, polyimides.
4. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the anion surfactant is ten At least one of sodium dialkyl sulfate, cetyl trimethylammonium bromide, sodium carboxymethylcellulose, naphthalene sulfonate salt.
5. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the non-ionic wetting agent is high-carbon fat Fat alcohol polyoxyethylene ether.
6. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the carbon nanotube, graphene, conduction Carbon black, dispersant, solvent weight be 1~1.5：1.5~3：1~2：1~1.25：80~95.
7. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that in dispersion process, keep slurry temperature Degree is less than 40 DEG C.
8. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that in the solvent containing dispersant, according to Secondary addition graphene, carbon nanotube and conductive black sequentially add graphene, conductive black and carbon nanotube.
9. the preparation method of electrocondution slurry as described in claim 1, which is characterized in that the dispersion linear velocity of the graphene is 10~15m/s, the jitter time of graphene is 60~180min；The dispersion linear velocity of the carbon nanotube be 10~15m/s, carbon The jitter time of nanotube is 20~60min；The dispersion linear velocity of the conductive black be 6~12m/s, the dispersion of conductive black Time is 20~30min.
10. the electrocondution slurry of a kind of carbon nanotube, graphene and conductive black compounding, which is characterized in that using such as claim 1 ~9 any one of them preparation methods obtain.
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