CN110289388A - Cathode manufacture manufacturing method, the manufacturing method of negative electrode battery electrode, battery and negative electrode battery electrode of slurry - Google Patents

Cathode manufacture manufacturing method, the manufacturing method of negative electrode battery electrode, battery and negative electrode battery electrode of slurry Download PDF

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Publication number
CN110289388A
CN110289388A CN201910206422.7A CN201910206422A CN110289388A CN 110289388 A CN110289388 A CN 110289388A CN 201910206422 A CN201910206422 A CN 201910206422A CN 110289388 A CN110289388 A CN 110289388A
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slurry
negative electrode
cathode
manufacturing
thickener
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高松秀明
堀龙太郎
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Envision AESC Energy Devices Ltd
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Envision AESC Energy Devices Ltd
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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
    • 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
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • H01M4/0435—Rolling or calendering
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/06—Electrodes for primary cells
    • H01M4/08—Processes of manufacture
    • 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
    • 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
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • H01M4/137—Electrodes based on electro-active polymers
    • 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
    • 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
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • 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
    • H01M4/1399—Processes of manufacture of electrodes based on electro-active polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M6/00—Primary cells; Manufacture thereof
    • H01M6/14—Cells with non-aqueous electrolyte
    • H01M6/16—Cells with non-aqueous electrolyte with organic electrolyte
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The manufacturing method of cathode manufacture slurry of the invention includes: by mixing negative electrode active material and the 1st thickener, to prepare the process (A) of the mixture (M1) including at least the negative electrode active material and the 1st thickener；By the liquid component of one or more of the aqueous emulsion of addition selected from water-medium and comprising water-based binder in the mixture (M1) and wet mixed is carried out, to prepare the process (B) of slurry presoma；With by further adding the liquid component in the slurry presoma and carrying out wet mixed, prepare the process (C) of cathode manufacture slurry, the process (B) at least successively includes: to obtain the process (B1) of mixture (M2) and making the liquid component penetrate into mixture (M1)；The process (B2) of mixture (M3) is obtained by the 2nd thickener of mixing in the mixture (M2) and the liquid component；The process (B3) of the slurry presoma is obtained with by the way that the mixture (M3) is done thick mixing.

Description

Cathode manufacture manufacturing method, negative electrode battery electrode, battery and the battery of slurry With the manufacturing method of negative electrode
Technical field
The present invention relates to the manufacturing method of cathode manufacture slurry, negative electrode battery electrode, battery and negative electrode batteries The manufacturing method of electrode.
Background technique
In general negative electrode used in battery is mainly made of negative electrode active material layer and current collector layer.Cathode is living Property material layer can be for example, by will include that the cathode manufacture of negative electrode active material, thickener and water-based binder etc. is applied with slurry It is distributed in the current collector layers such as metal foil surface and drying and obtains.
As the manufacturing method of negative electrode battery, for example, method described in Patent Document 1.
In the manufacture for recording a kind of lithium ion secondary battery in patent document 1 (No. 5396989 bulletins of Japanese Patent No.) The manufacturing method of the slurry used puts into carbon dust 1a and CMC powder 1b, generates powder mixing with the state mixing of only powder After object 1, based on each related to the viscosity of slurry, granularity and peel strength, determine the input amount of decentralized medium and do thick mixing Time is divided into thick refining process and does thick compounding procedure two stages, puts into the water as decentralized medium.
Existing technical literature
Patent document
Patent document 1: No. 5396989 bulletins of Japanese Patent No.
Summary of the invention
Problems to be solved by the invention
The research of people etc. according to the present invention, the negative electrode battery electrode obtained by previous manufacturing method are removed by force sometimes Spend low, the cementability of current collector layer and negative electrode active material layer is clearly present room for improvement.
In the case where the peel strength of negative electrode battery electrode is low, electrode is worried, the productivity of battery reduces, Huo Zhe The powder falling of negative electrode active material layer occurs in the process of assembled battery, as a result the quality deterioration of battery, cycle characteristics of battery etc. It leads to the problem of.
The present invention in view of the above situation completes, and current collector layer and negative electrode active material can be stably obtained by providing one kind The cathode manufacture of the negative electrode battery electrode excellent in adhesion of the layer manufacturing method of slurry.
The means used to solve the problem
The inventors of the present invention further investigate repeatedly in order to reach the above subject.Itself as a result, it has been found that, by using by thickener The manufacturing method of the cathode manufacture slurry mixed in two stages, can stably obtain current collector layer and negative electrode active material layer Negative electrode battery electrode excellent in adhesion so that complete the present invention.
That is, according to the present invention, providing a kind of manufacturing method of cathode manufacture slurry comprising:
By mixing negative electrode active material and the 1st thickener, to prepare including at least above-mentioned negative electrode active material and upper State the process (A) of the mixture (M1) of the 1st thickener；
By being added in the aqueous emulsion selected from water-medium and comprising water-based binder in said mixture (M1) One or more kinds of liquid components and carry out wet mixed, to prepare the process (B) of slurry presoma；With
By further adding aforesaid liquid ingredient in above-mentioned slurry presoma and carrying out wet mixed, to prepare cathode The manufacture process (C) of slurry；
Above-mentioned operation (B) at least successively includes:
The process (B1) of mixture (M2) is obtained and making aforesaid liquid ingredient penetrate into said mixture (M1)；
The work of mixture (M3) is obtained by the 2nd thickener of mixing in said mixture (M2) and aforesaid liquid ingredient Sequence (B2)；With
The process (B3) of above-mentioned slurry presoma is obtained by the way that said mixture (M3) is done thick mixing.
In addition, according to the present invention, providing a kind of negative electrode battery electrode, it includes current collector layer and it is set to above-mentioned current collection At least one side of body layer and the negative electrode active material layer formed by the solid component of cathode manufacture slurry of the invention.
In addition, according to the present invention, a kind of battery is provided,
It is the battery at least having anode, electrolyte and cathode,
Above-mentioned cathode includes negative electrode battery electrode of the invention.
According to the present invention, a kind of manufacturing method of negative electrode battery electrode is provided comprising:
The cathode that the manufacturing method of cathode manufacture slurry through the invention obtains is manufactured and is coated on current collection with slurry Body layer and drying remove above-mentioned water-medium, thus the process for forming above-mentioned negative electrode active material layer in above-mentioned current collector layer.
Invention effect
According to the present invention it is possible to which the excellent in adhesion of current collector layer and negative electrode active material layer can be stably obtained by providing Negative electrode battery electrode cathode manufacture use slurry.
Detailed description of the invention
Above-mentioned purpose and other objects, features and advantages according to preferred embodiment described below and are attached to The following drawings definitely.
Fig. 1 is the sectional view for indicating an example of the structure of negative electrode battery electrode of embodiment of the present invention.
Fig. 2 is the sectional view for indicating an example of the structure of battery of embodiment of the present invention.
Specific embodiment
Hereinafter, being illustrated for embodiments of the present invention using attached drawing.It should be noted that in all the appended drawings, Same symbol is assigned for same constituent element, is suitably omitted the description.In addition, each component is schematically shown in figure It will be appreciated that the shape of degree of the invention, size and configuration relation, different from actual size.
It should be noted that in present embodiment unless otherwise specified, the layer comprising negative electrode active material is known as The substance that negative electrode active material layer is formd in current collector layer is known as electrode by negative electrode active material layer.In addition, this embodiment party " A~B " of numberical range unless otherwise specified, indicates A or more and B or less in formula.
<manufacturing method that slurry is used in cathode manufacture>
The manufacturing method of cathode manufacture slurry of the present embodiment includes: by by negative electrode active material and the 1st Thickener mixing, to prepare the process (A) of the mixture (M1) including at least negative electrode active material and the 1st thickener；By Addition is selected from one or more of water-medium and the aqueous emulsion comprising water-based binder in mixture (M1) Liquid component simultaneously carries out wet mixed, to prepare the process (B) of slurry presoma；With by further adding in slurry presoma Add liquid component and wet mixed, to prepare the process (C) of cathode manufacture slurry.
Also, in the manufacturing method of cathode manufacture slurry of the present embodiment, above-mentioned operation (B) is at least successively It include: to obtain the process (B1) of mixture (M2) and making aforesaid liquid ingredient penetrate into said mixture (M1)；By upper It states the 2nd thickener of mixing and aforesaid liquid ingredient in mixture (M2) and obtains the process (B2) of mixture (M3)；With pass through by Said mixture (M3) does thick mixing and obtains the process (B3) of above-mentioned slurry presoma.
Here, 1st thickener and the 2nd thickener are manufactured in cathode in cathode manufacture slurry of the present embodiment It is dissolved in slurry, rather than pulverulence.
In addition, battery of the present embodiment be such as lithium ion one-shot battery or lithium ion secondary battery, preferably Lithium ion secondary battery.
As previously mentioned, the research of people etc. according to the present invention, the negative electrode battery electrode obtained by previous manufacturing method Sometimes peel strength is low, and the cementability of current collector layer and negative electrode active material layer is clearly present room for improvement.
In the case where the peel strength of negative electrode battery electrode is low, electrode is worried, the productivity of battery reduces, Huo Zhe The powder falling of negative electrode active material layer occurs in the process of assembled battery, as a result the quality deterioration of battery, cycle characteristics of battery etc. It leads to the problem of.
The inventors of the present invention further investigate repeatedly in order to reach the above subject.As a result, it has been found that by carrying out the dry of slurry In stage before the process (B3) of thick mixing, it is divided into the 1st thickener and the 2nd the two stages of thickener to mix thickener, it can The negative electrode battery electrode excellent in adhesion for stably obtaining current collector layer and negative electrode active material layer, so that completing this hair It is bright.
Here, by the 2nd the two stages of thickener in the 1st thickener and process (B2) that are divided into process (A) come Thickener is mixed, the negative electrode battery electrode excellent in adhesion of current collector layer and negative electrode active material layer can be stably obtained The reasons why it is not necessarily clear, but be contemplated that following reason.
Firstly, passing through mixing negative electrode active material and the 1st thickener, it is believed that the 1st thickener is adsorbed in process (A) The surface of negative electrode active material.
Additionally, it is believed that passing through mixing the 2nd after by making liquid component penetrate into mixture (M1) to obtain mixture (M2) Thickener, can in the state that the 1st thickener is adsorbed in the surface of negative electrode active material by the 2nd thickener be scattered in liquid at In point.
Think in the obtained cathode manufacture slurry presoma, the major part of negative electrode active material on surface to inhale The form of the attached aggregate of 1st thickener excellent with the adsorptivity of water-based binder exists, and the 2nd thickener is not adsorbed in negative The surface of pole active material and exist in liquid component with free state.Water-based binder is efficiently adsorbed in above-mentioned as a result, The three-dimensional network of aggregate, the interaction based on each storeroom is flourishing, and unadsorbed the 2nd thickening in negative electrode active material Agent is moderately dispersed in a liquid with free state.
Therefore, followed by, cathode manufacture is coated on current collector layer and drying with slurry, and then remove above-mentioned Water-medium is formed in above-mentioned current collector layer in the process of above-mentioned negative electrode active material layer, it is believed that with trip in above-mentioned slurry Water-based binder is mobile to negative electrode active material layer surface when the 2nd thickener from state dispersion inhibits dry.It is also thought that by Flourishing in the three-dimensional network of the interaction based on each storeroom, water-based binder is to negative electrode active material when further suppressing dry Matter layer surface is mobile.Their synergistic effect as a result, be regarded to inhibit water-based binder in negative electrode active material layer It is biased to exist in surface.
Also, there are repressed as a result, being regarded to the surface of negative electrode active material layer deviation for water-based binder The amount for increasing the water-based binder of the interface of current collector layer and negative electrode active material layer, can be improved current collector layer and cathode is living Cementability, the i.e. peel strength of property material layer.
That is, the manufacturing method for the cathode manufacture slurry being related to according to the present embodiment, by be divided into process (A) The 2nd the two stages of thickener in 1 thickener and process (B2) mix thickener, are able to suppress water-based binder to cathode The deviation of active material layer surface exists, and cementability, the i.e. peel strength of current collector layer and negative electrode active material layer can be made to mention It is high.
By the above, according to the present embodiment, can provide can stably obtain current collector layer and negative electrode active material Slurry is used in the cathode manufacture of the negative electrode battery electrode excellent in adhesion of layer.
From the viewpoint of make cathode manufacture slurry dispersion stabilization it is good, cathode of the present embodiment manufacture It is, for example, 6.0 or more and 8.0 hereinafter, preferably 6.5 or more and 7.5 hereinafter, more preferably 6.8 or more and 7.2 with the pH of slurry Below.
The method of adjustment of the pH of cathode manufacture slurry of the present embodiment is not particularly limited, for example, can lead to Cross the compounding ratio of each material of adjustment composition cathode manufacture slurry, composition cathode is manufactured with type of each material of slurry etc. To be adjusted.
<constituent material that slurry is used in cathode manufacture>
Then, each material for constituting cathode manufacture slurry of the present embodiment is illustrated.Present embodiment The cathode manufacture slurry being related to includes negative electrode active material, water-based binder, thickener (by the 1st thickener and the 2nd thickener Also referred to collectively as thickener.) and water-medium, it further as needed include conductive auxiliary agent.
(negative electrode active material)
In present embodiment, use negative electrode active material as electrode active material, cathode manufacture is for shape with slurry At the cathode of battery slurry when, more particularly to effectively obtain the peel strength improvement effect of present embodiment.
As negative electrode active material, if the common negative electrode active material being able to use in the cathode of battery then without spy It does not limit.In the case that above-mentioned battery is lithium ion battery, it can be cited for example that natural graphite, artificial graphite, resin carbon, carbon fiber The carbon materials such as dimension, active carbon, hard carbon, soft carbon；The lithiums such as lithium metal, lithium alloy system metal；The metals such as silicon, tin；Polyacene, poly- second Electric conductive polymers such as alkynes, polypyrrole etc..Preferred carbon material among these, the graphite such as particularly preferred natural graphite, artificial graphite Material.
Negative electrode active material can be used singly or in combination of two or more.
When the total amount of the solid component of cathode manufacture slurry is set as 100 mass parts, the content of negative electrode active material is excellent 70 mass parts or more and 99.97 are selected as below the mass, more than more preferably 85 mass parts and 99.85 below the mass.
As graphite material, do not limited especially then if the common graphite material being able to use in the cathode of battery It is fixed.Above-mentioned battery be lithium ion battery in the case where, it can be cited for example that natural graphite, by petroleum and coal system coke The artificial graphite etc. for being heat-treated and being manufactured.
Here, natural graphite refers to, the graphite as the natural output of ore.The day that core material as present embodiment uses The place of production of right graphite, character, type are not particularly limited.
In addition, artificial graphite refers to, the graphite that is made using artificial gimmick and close to the graphite of graphite being fully crystallized. Such artificial graphite can be for example, by tar, the coke to be obtained by the distillation bring residue etc. of the destructive distillation of coal, crude oil Charcoal is raw material, is obtained by firing process, graphitization process.
In addition, graphite material is preferably using powdered graphite as core material, and at least part on the surface of above-mentioned powdered graphite It is coating (hereinafter, also referred to as surface is coated graphite by the carbon material lower than the crystallinity of above-mentioned powdered graphite.).Particularly preferred graphite powder The edge part at end is coated by above-mentioned carbon material.Edge part by powdered graphite is coated, and edge part and electrolyte are able to suppress Irreversible reaction, be as a result able to suppress the reduction of the efficiency for charge-discharge at initial stage caused by the increase of irreversible capacity.
In addition, can be improved the bonding with binder compared with the independent situation of graphite if being coated graphite using surface Property, therefore the amount of binder can be reduced.As a result the battery behavior of the battery enabled to improves.
Here, the carbon material lower than the crystallinity of above-mentioned powdered graphite refers to the amorphous carbon such as soft carbon, hard carbon.
As be used as core material powdered graphite, it can be cited for example that natural graphite, by petroleum and coal system coke The artificial graphite etc. for being heat-treated and being manufactured.In present embodiment, these powdered graphites be can be used alone, can also be with It is applied in combination two or more.Among these, from cost aspect, preferred natural graphite.
Surface of the present embodiment is coated graphite and can make by the following method: will be carbonized by firing process And after becoming the organic compound of the carbon material lower than the crystallinity of above-mentioned powdered graphite, being mixed with above-mentioned powdered graphite, to upper It states organic compound and carries out firing carbonization.
If the organic compound mixed with above-mentioned powdered graphite be carbonized by firing it is available than above-mentioned graphite powder The organic compound of the low carbon material of the crystallinity at end, is not particularly limited, it can be cited for example that petroleum tar, coal system The tar such as tar；The pitches such as petroleum pitch, coal system pitch；Polyvinyl chloride, polyvinyl acetate, polyvinyl butyral, The thermoplastic resins such as polyvinyl alcohol, Vingon, polyacrylonitrile；The thermosetting resins such as phenolic resin, furfuryl alcohol resin；Cellulose Equal natural resins；Aromatic hydrocarbons such as naphthalene, alkylnaphthalene, anthracene etc..
In present embodiment, these organic compounds be can be used alone, and can also be applied in combination two or more.Separately Outside, these organic compounds, which can according to need, is dissolved by solvent or is dispersed to use.
Among above-mentioned organic compound, from the preferred tar of price aspect and pitch.
When negative electrode active material is set as 100 mass %, surface of the present embodiment is coated having by oneself in graphite The ratio (hereinafter referred to as " amount of coating " of the carbon material of machine compound.) it is preferably 0.7 mass % or more and 8.0 mass % or less.
By the amount of coating of carbon material is set as above-mentioned upper limit value hereinafter, absorb release lithium ion area become larger, can The multiplying power property of the lithium ion battery made improves.
By the way that the amount of coating of carbon material is set as above-mentioned lower limit value or more, it is able to suppress caused by the increase of irreversible capacity The reduction of the efficiency for charge-discharge at initial stage.In addition, being enabled to by the way that the amount of coating of carbon material is set as above-mentioned lower limit value or more Cathode manufacture improved with the stability of slurry.
Here, above-mentioned amount of coating can be calculated by thermogravimetric analysis.More specifically, thermogravimetric analysis meter (example can be used Such as Perkin-Elmer corporation TGA7 analysis meter), under oxygen atmosphere, with 5 DEG C/min of heating rate by negative electrode active material liter When temperature is to 900 DEG C, it is by the temperature since Mass lost to the Mass lost ratio temperature that then Mass lost accelerates that slows down Reduction quality only is as amount of coating.
The specific surface area based on N2 adsorption BET method of negative electrode active material is preferably 1.0m2/ g or more and 6.0m2/ g hereinafter, More preferably 2.0m2/ g or more and 5.0m2/ g or less.
By the way that specific surface area is set as above-mentioned upper limit value hereinafter, being able to suppress initial stage caused by the increase of irreversible capacity The reduction of efficiency for charge-discharge.In addition, by the way that specific surface area is set as above-mentioned upper limit value hereinafter, the cathode manufacture enabled to is used The stability of slurry improves.
By the way that specific surface area is set as above-mentioned lower limit value or more, the area for absorbing releasing lithium ion becomes larger, and enables to Lithium ion battery multiplying power property improve.
In addition, the caking property of water-based binder can be made to improve by the way that specific surface area to be set as in above range.
Side reaction when inhibiting charge and discharge and the reduction aspect for inhibiting efficiency for charge-discharge, negative electrode active material Average grain diameter is preferably 1 μm or more, more preferably 3 μm or more, further preferably 5 μm or more, particularly preferably 8 μm or more, Viewpoint in terms of inputting out power characteristic and electrode fabrication (put down by the) such as flatness of electrode surface, negative electrode active material Equal partial size be preferably 50 μm hereinafter, more preferably 40 μm hereinafter, particularly preferably 30 μm or less.Here, average grain diameter refers to base Partial size (the median particle diameter: d under accumulated value 50% in the size distribution (volume reference) of laser diffraction scattering method50)。
(water-based binder)
If water-based binder is able to carry out electrode forming and there is sufficient electrochemical stability to be not particularly limited, example Rubber series binder resin, acrylic acid series system binder resin such as can be used.It should be noted that in present embodiment, Water-based binder resin refers to, is dispersed in water the substance for being capable of forming aqueous emulsion.
Water-based binder of the present embodiment is formed by latex particle, is preferably dispersed in water it as emulsified water Solution uses.That is, water-based binder of the present embodiment is preferably formed by the latex particle of water-based binder.As a result, can It reaches between not hindering negative electrode active material, the contact between conductive auxiliary agent, between negative electrode active material and conductive auxiliary agent, and keeps cathode living Property material layer in contain water-based binder resin.
As rubber series binder resin, it can be cited for example that styrene-butadiene copolymer rubber etc..
As acrylic binder resin, it can be cited for example that including acrylic acid, methacrylic acid, acrylate, first Polymer (the homopolymer of the unit (hereinafter referred to as " acrylic acid units ") of base acrylate, acrylates or methacrylate Or copolymer) etc..As the copolymer, the copolymer comprising acrylic acid units and styrene units can be enumerated, comprising propylene Acid unit and the copolymer of silicon unit etc..
These water-based binder resins can be used alone, and can also be applied in combination two or more.Among these, from Caking property is set out with excellent aspects such as the compatibilities, price and electrochemical stability of electrolyte, particularly preferred styrene-fourth Diene copolymers rubber.
When the total amount of the solid component of cathode manufacture slurry is set as 100 mass parts, the content of water-based binder is preferred For more than 0.01 mass parts and 10.0 below the mass, more than more preferably 0.05 mass parts and 5.0 below the mass.If water system Within the above range, then cathode is manufactured with the coating of slurry, the caking property of binder and battery behavior the content of binder It balances more excellent.
Water-based binder for example makes powdered binder be scattered in water-medium and use in the form of aqueous emulsion. Thereby, it is possible to not hinder between negative electrode active material, the contact between conductive auxiliary agent, between negative electrode active material and conductive auxiliary agent, and Improve the dispersibility of water-based binder.
About the water-medium for dispersing water-based binder, do not have then if the water-medium that can disperse water-based binder It is particularly limited to, distilled water, ion exchange water, city can be used for tap water, industrial water etc..Among these, preferably distilled water, Ion exchange water.In addition, solvent that can be high with water hydrophily with mixed alcohol etc. in water.
Styrene-butadiene copolymer rubber is using styrene and 1,3-butadiene as the copolymer of principal component.Here, main Ingredient refers to, in styrene-butadiene copolymer rubber, structural unit from styrene and from 1,3 one butadiene Total content of structural unit is the feelings of 50 mass % or more in whole polymerized units of styrene-butadiene copolymer rubber Condition.
Structural unit from styrene is (hereinafter, also referred to as St.) with from 1,3-butadiene structural unit (hereinafter, Claim BD.) mass ratio (St/BD) be, for example, 10/90~90/10.
It can also make the monomer component other than styrene and 1,3-butadiene in styrene-butadiene copolymer rubber Copolymerization.For example, conjugate diene monomer, unsaturated carboxylic acid monomer, other well known monomers that can be copolymerized etc. can be enumerated.
As conjugate diene monomer, it can be cited for example that isoprene, 2,3- dimethyl -1,3-butadiene, 1,3- penta Diene, pentadiene etc..
As unsaturated carboxylic acid monomer, it can be cited for example that acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid Deng.
The manufacturing method of styrene-butadiene copolymer rubber is not particularly limited, and is preferably manufactured by emulsion polymerization. If can be obtained in the form of the latex particle comprising styrene-butadiene copolymer rubber using emulsion polymerization.
As emulsion polymerization, previously known method can use.For example, can by by styrene, 1,3-butadiene, And the above-mentioned various monomer components that can be copolymerized add polymerization initiator in the case where preferably there is emulsifier, in water Emulsion polymerization is carried out to manufacture.
(thickener)
Thickener is not particularly limited if the thickener that the coating of cathode manufacture slurry can be made to improve.As Thickener, it can be cited for example that cellulose-based water soluble polymer；Polycarboxylic acids；Polyethylene oxide；Polyvinylpyrrolidone；Poly- third The polyacrylates such as olefin(e) acid sodium；Polyvinyl alcohol；Equal water-soluble polymers.These thickeners can be used alone, can also group It closes and uses two or more.
Preferred cellulose system water soluble polymer among these.
As cellulose-based water soluble polymer, if the cellulose that the coating of cathode manufacture slurry can be made to improve It is that water soluble polymer is not particularly limited.As cellulose-based water soluble polymer, can be used for example selected from carboxymethyl Cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, methyl ethyl hydroxy cellulose, methylcellulose, hydroxypropyl cellulose etc. In cellulose-based polymer salts such as the ammonium salt and alkali metal salt of cellulose-based polymer and these cellulose-based polymer etc. It is one or more kinds of.
It is preferably comprised among these selected from least one of carboxymethyl cellulose and carboxymethyl cellulose salt, is more preferably wrapped Containing the sylvite for being selected from carboxymethyl cellulose, the ammonium salt of carboxymethyl cellulose, the sodium salt of carboxymethyl cellulose and carboxymethyl cellulose One or more of.
From can make cellulose-based water soluble polymer to the dissolubility of water-medium improve, improve cathode manufacture slurry The aspect of solid component concentration, the aspect that improves of elasticity modulus of the cathode manufacture slurry enabled to etc. set out, it is fine The degree of etherification falling for tieing up prime system water soluble polymer is preferably 0.50 or more and 1.0 hereinafter, more preferably 0.70 or more and 0.90 or less.
Here, degree of etherification falling refers to, the hydroxyl of every 1 anhydrous grape sugar unit in cellulose-based water soluble polymer is to carboxylic The degree of substitution of the substituents such as methyl.
Pass through weight average molecular weight Mw (the poly- second two of gel permeation chromatography (GPC) measurement, cellulose-based water soluble polymer Alcohol scaled value) it is preferably 100000 or more, more preferably 200000 or more.If the Weight-average molecular of cellulose-based water soluble polymer Measuring Mw is above-mentioned lower limit value or more, then can effectively improve the energy storage mould of cathode manufacture slurry of the present embodiment Amount.
In addition, passing through the weight average molecular weight Mw (polyethylene glycol scaled value) of GPC measurement, cellulose-based water soluble polymer Preferably 900000 hereinafter, more preferably 800000 or less.If the weight average molecular weight Mw of cellulose-based water soluble polymer is upper Upper limit value is stated hereinafter, then cellulose-based water soluble polymer can be improved cathode manufacture and use to the raising of the dissolubility of water-medium As a result the solid component concentration of slurry can effectively improve the energy storage mould of cathode manufacture slurry of the present embodiment Amount.
When the total amount of the solid component of cathode manufacture slurry is set as 100 mass parts, content (the 1st thickening of thickener Total content of agent and the 2nd thickener) be preferably 0.01 mass parts or more and 10.0 below the mass, more preferably 0.05 mass Part or more and 5.0 below the mass.If the content of thickener is in above range, the coating of cathode manufacture slurry glues The balance of the caking property and battery behavior of tying agent is more excellent.
(conductive auxiliary agent)
From the viewpoint of the raising of the electric conductivity of the electrode made, cathode manufacture of the present embodiment is excellent with slurry Choosing also contains conductive auxiliary agent.
The conductive auxiliary agent that conductive auxiliary agent is improved if electric conductivity that is conductive, making electrode is not particularly limited.Make For conductive auxiliary agent of the present embodiment, it can be cited for example that acetylene black, Ketjen black, carbon black, carbon nano-fiber, than as work The carbon materials such as the small graphite of the partial size of the graphite of property substance migration.These conductive auxiliary agents can be used alone, and can also combine Use two or more.
When the total amount of the solid component of cathode manufacture slurry is set as 100 mass parts, the content of conductive auxiliary agent is preferably More than 0.01 mass parts and 10.0 below the mass, more than more preferably 0.05 mass parts and 5.0 below the mass.
If the content of conductive auxiliary agent is the coating of cathode manufacture slurry and the caking property of binder in above range Balance it is more excellent.
From the conductive balance aspect of the coating of cathode manufacture slurry and electrode, conductive auxiliary agent based on The specific surface area of N2 adsorption BET method is preferably 50m2/ g or more and 1000m2/ g or less.
(water-medium)
Water-medium of the present embodiment is not particularly limited, distilled water, ion exchange can be used for example Water, city are for tap water, industrial water etc..Among these, preferably distilled water, ion exchange water.In addition, can be with mixed alcohol etc. in water The high solvent with water hydrophily.
Cathode manufacture of the present embodiment is set as with the total amount of the solid component of slurry with slurry manufacturing cathode When 100 mass parts, the content of negative electrode active material be preferably 70 mass parts or more and 99.97 below the mass, more preferably 85 More than mass parts and 99.85 below the mass.In addition, the content of water-based binder is preferably 0.01 mass parts or more and 10.0 matter Part is measured hereinafter, more than more preferably 0.05 mass parts and 5.0 below the mass.In addition, thickener content (the 1st thickener and Total content of 2nd thickener) be preferably 0.01 mass parts or more and 10.0 below the mass, more preferably 0.05 mass parts with It is upper and 5.0 below the mass.In addition, the content of conductive auxiliary agent be preferably 0.01 mass parts or more and 10.0 below the mass, more More than preferably 0.05 mass parts and 5.0 below the mass.
If the content of each ingredient of composition cathode manufacture slurry is within the above range, the cathode manufacture quality of slurry The balance of the battery behavior of stability and obtained battery is especially excellent.
<manufacturing method that slurry is used in cathode manufacture>
Then, the manufacturing method of water system cathode manufacture slurry of the present embodiment is illustrated.
The manufacturing method of cathode manufacture slurry of the present embodiment is bonded comprising negative electrode active material, water system Agent, thickener, water-medium, further the negative electrode battery comprising conductive auxiliary agent manufactures the manufacturer for using slurry as needed Method includes at least process below (A)~(C).
Process (A): by mixing negative electrode active material and the 1st thickener, to prepare including at least negative electrode active material With the process of the mixture (M1) of above-mentioned 1st thickener
Process (B): by being added in said mixture (M1) selected from water-medium and including the emulsification of water-based binder The liquid component of one or more of aqueous solution simultaneously carries out wet mixed, the process to prepare slurry presoma
Process (C): by further adding aforesaid liquid ingredient in above-mentioned slurry presoma and carrying out wet mixed, come The process for preparing cathode manufacture slurry
In process (A), by mixing negative electrode active material and the 1st thickener, to prepare including at least negative electrode active material The mixture (M1) of matter and the 1st thickener.At this point it is possible to which conductive auxiliary agent is mixed together.
In process (A), the various powders shape substance of negative electrode active material and the 1st thickener will be preferably included at least with powder State dry type mixing.By that with powder state dry type mixing, can prepare negative electrode active material and the 1st thickener comprising cathode The mixture of the powder of active material and the 1st thickener.At this point it is possible to which conductive auxiliary agent together powder is mixed.Present embodiment In, by carrying out process (A), the 1st thickener can be made to be adsorbed in the surface of negative electrode active material.
Here, can carry out process (A) with wet mixed, the solid component concentration of process (A) is for example preferably 95 matter Measure % or more and 100 mass % or less.By making the solid component concentration in process (A) within the above range, the 1st increasing can be made The thick dose of surface for being more effectively adsorbed in negative electrode active material.
As the mixing machine for carrying out process (A), it is preferable to use planetary motion type mixer, more preferably uses planetary motion type Planetary-type mixer.By using such mixing machine, it is able to suppress dispersing for negative electrode active material and the 1st thickener, simultaneously It is sufficiently mixed negative electrode active material and the 1st thickener.It should be noted that planetary motion type mixer refers to as agitating device Mixer with rotation and revolution function.Planetary motion type planetary-type mixer refers to that having as agitating device has certainly Turn and revolution function blade mixer.
Mixed shear velocity in process (A) is preferably 1.0sec-1Above and 26.0sec-1In following range, more Preferably 6.5sec-1Above and 19.5sec-1In following range.
If the mixed shear velocity in process (A) is within the above range, it is able to suppress negative electrode active material and the 1st and increases Thick dose disperses, while being sufficiently mixed negative electrode active material and the 1st thickener.
Incorporation time in process (A) is not particularly limited, and for example, 5 minutes or more and 120 minutes hereinafter, preferably 10 Minute or more and 60 minutes or less.
In process (B), by adding in the mixture (M1) obtained using process (A) selected from water-medium and comprising water It is the liquid component of one or more of aqueous emulsion of binder and carries out wet mixed, prepares slurry forerunner Body.
Mixing machine as the wet mixed in progress process (B) is, it is preferable to use planetary motion type mixer, more preferably makes With planetary motion type planetary-type mixer.By using such mixing machine, it is able to suppress and constitutes each of cathode manufacture slurry Material disperses, while improving the dispersibility of each material.
Here, process (B) at least successively includes: to obtain mixture and making aforesaid liquid ingredient penetrate into mixture (M1) (M2) process (B1)；By the 2nd thickener of mixing in mixture (M2) and aforesaid liquid ingredient to obtain mixture (M3) process (B2)；By the way that mixture (M3) is done thick mixing to obtain the process (B3) of slurry presoma, it is set as three The process more than stage.
Obtaining the process (B1) of mixture (M2) and making aforesaid liquid ingredient penetrate into mixture (M1) is made selected from water It is liquid component infiltration mixture (M1) of one or more of medium and the aqueous emulsion comprising water-based binder Process.Mixture (M2) obtained in process (B1) is the state for the powder that such as liquid component penetrates into negative electrode active material, It is not argillaceous, and the state in flowing.That is, preferably with the state compounding mixture (M1) of flowing, and being obtained in process (B1) To the mixture (M2) for being in flow regime.By including the infiltration process (B1), mixture can be inhibited in a certain range Swarm the edge of mixing machine in wet mixed, moistening of mixture has deviation, mixture disperses when being kneaded.
The shear velocity of wet mixed in process (B1) is preferably 6.5sec-1Above and 55.5sec-1Range below It is interior, more preferably 26.0sec-1Above and 40.0sec-1In following range.
If the shear velocity of the wet mixed in process (B1) is within the above range, it can more effectively inhibit mixture Swarm the edge of mixing machine in wet mixed, the wet of mixture has deviation, mixture disperses when being kneaded, while making liquid Body ingredient is fully infiltrated into mixture.
The incorporation time of wet mixed in process (B1) is not particularly limited, such as preferably 0.5 minute or more and 60 Minute is hereinafter, more preferably 10 minutes or more and 30 minutes or less.
In process (B1), the solid component concentration of mixture (M2) is preferably adjusted to 71 mass % or more and 95 mass % Hereinafter, being more preferably adjusted to 73 mass % or more and 94 mass % hereinafter, being further preferably adjusted to 74 mass % or more and 91 Quality % is hereinafter, be particularly preferably adjusted to 77 mass % or more and 86 mass % or less.
In process (B1), by the way that the solid component concentration of mixture (M2) is set as above-mentioned lower limit value or more, the 1st thickener The surface for being adsorbed in negative electrode active material is become easy, therefore further suppresses surplus of the 1st thickener into water-medium Dispersion.Think negative electrode active material it is most of followed by process (B2) and process (B3) in, also thickened by the 1st Agent disperses in the state of being adsorbed in the aggregate on surface into water-medium.1st thickener is compared with negative electrode active material itself It is excellent with the adsorptivity of water-based binder, therefore, it is considered that water-based binder is efficiently adsorbed in above-mentioned aggregate, it is based on each material Between interaction three-dimensional network it is flourishing.As a result, above-mentioned cathode manufacture is then coated on collector simultaneously with slurry In negative electrode obtained from drying, cementability, the i.e. peel strength of current collector layer and negative electrode active material layer can be made into one Step improves.
In the manufacturing method of cathode of the present embodiment manufacture slurry, by by the mixture in process (B1) (M2) solid component concentration is set as above-mentioned upper limit value and exists hereinafter, the mixture comprising negative electrode active material can be effectively inhibited Swarm mixing machine edge when mixing, therefore the cathode manufacture slurry of stable viscosity, mixing ratio can be obtained.
In addition, process (B2) is mixed by the 2nd thickener of mixing in mixture (M2) and aforesaid liquid ingredient The process for closing object (M3).
In process (B2), the 2nd thickener is mixed with powder state preferably in mixture (M2).In this way, Neng Gouyi Side inhibits reduction one side compounding mixture (M2) of the solid component concentration of mixture (M2), can apply higher shearing on one side One side compounding mixture (M2).
The 2nd thickener mixed in the 1st thickener and process (B2) mixed in preferable process (A) is one species.It is logical It crosses in this way, the design of cathode manufacture slurry, the management of thickener become to be more easier.
Water system cathode manufacture of the present embodiment is used in the manufacturing method of slurry, preferably the combined amount of the 2nd thickener More than the combined amount of the 1st thickener.
More specifically, when total combined amount of the 1st thickener and the 2nd thickener being set as 100 mass %, the 1st thickening The combined amount of agent is preferably 45 mass % hereinafter, more preferably 40 mass % are hereinafter, further preferably 35 mass % are hereinafter, spy It You Xuanwei not 30 mass % or less.In this way, it can increase and increase in cathode manufacture slurry with the 2nd of free state dispersion the Thick dose of amount, therefore water-based binder is mobile to negative electrode active material layer surface when can further suppress dry.As a result can It further suppresses water-based binder and is biased to exist on the surface of negative electrode active material layer, therefore current collector layer and cathode can be increased The amount of the water-based binder of the interface of active material layer can further increase the viscous of current collector layer and negative electrode active material layer Connecing property, i.e. peel strength.
In addition, the 1st thickener mixes when total combined amount of the 1st thickener and the 2nd thickener is set as 100 mass % Resultant is preferably 1 mass % or more, more preferably 5 mass % or more, further preferably 10 mass % or more.In this way, The amount in the 1st thickener of the adsorption of negative electrode active material can be increased, the interaction as a result based on each storeroom Three-dimensional network is further flourishing, and water-based binder is mobile to negative electrode active material layer surface when can further suppress dry.Its It is biased to exist on the surface of negative electrode active material layer as a result, it is possible to further suppress water-based binder, therefore collection can be increased The amount of the water-based binder of the interface of electrics layer and negative electrode active material layer, can further increase current collector layer and cathode is living Cementability, the i.e. peel strength of property material layer.
In addition, slurry occurs in the stage of process (B) in the case where not mixing the 1st thickener completely in process (A) The cohesion of presoma cannot prepare desired cathode manufacture slurry.The reasons why cohesion of such slurry presoma occurs It is not necessarily clear, if not mixing the 1st thickener completely, become the state that negative electrode active material and thickener are not uniformly mixed, A large amount of negative electrode active materials are not in the aggregate of adsorption 1st thickener excellent with the adsorptivity of water-based binder Form exists, and the 2nd thickener put into process (B2) becomes only is biased to exist on the periphery of the negative electrode active material of a part State.So, in the stage that water-based binder is added, it is believed that the absorption of water-based binder is preferentially in above-mentioned thickener It is biased to carry out in existing negative electrode active material.
In addition, process (B3) is to obtain slurry forerunner by the way that mixture (M3) obtained in process (2) is done thick mixing The process of body.Slurry presoma obtained in process (B3) is in such as clay state.That is, in process (B3), mixture (M3) Become clay state with progress is kneaded, as a result preferably obtains the slurry presoma in clay state.
Here, it is preferred that the solid component concentration of the slurry presoma in process (B3) is set below mixed in process (B1) Close the solid component concentration of object (M2).Thus mixture (M3) becomes clay state as mixing is in progress, and as a result can apply more High shearing, being capable of abundant compounding mixture (M3).
In process (B3), the solid component concentration of mixture (M3) is preferably adjusted to 55 mass % more than and less than 75 matter % is measured, is more preferably adjusted to 56 mass % or more and 72 mass % hereinafter, being further preferably adjusted to 57 mass % or more and 70 Quality % is hereinafter, be particularly preferably adjusted to 59 mass % or more and 66 mass % or less.
In process (B3), by the way that the solid component concentration of mixture (M3) is set as above-mentioned lower limit value or more, it is able to maintain that The adsorbed state of the 1st thickener adsorbed in negative electrode active material, therefore superfluous dispersion of the 1st thickener into water-medium It is suppressed.The water-based binder added in cathode manufacture slurry preparation section (C) later, which is efficiently adsorbed in, to be adsorbed with The three-dimensional network of the active material for stating the 1st thickener, the interaction based on each storeroom is flourishing.As a result, then will In negative electrode obtained from above-mentioned cathode manufacture is coated on collector and is dried with slurry, current collector layer and cathode can be made living Cementability, the i.e. peel strength of property material layer further increases.
By the way that the solid component concentration of mixture (M3) is set as above-mentioned lower limit value or more, it is able to suppress solid mixture change At the state of so-called agglomeration, uniform slurry is made.
By the way that the solid component concentration of mixture (M3) is set as above-mentioned upper limit value hereinafter, can be uniform by the 2nd thickener Ground further disperses well into water-medium.As a result, it is continuing, cathode manufacture is coated on collector with slurry Layer is simultaneously dry, and then removes above-mentioned water-medium, is formed in the process of above-mentioned negative electrode active material layer in above-mentioned current collector layer, Think that water-based binder is moved to negative electrode active material layer surface when the 2nd thickener dispersed in above-mentioned slurry further suppresses dry It is dynamic, it as a result can further suppress water-based binder and be biased to exist on the surface of negative electrode active material layer.
In addition, by the way that the solid component concentration of mixture (M3) is set as above-mentioned upper limit value hereinafter, can effectively inhibit Mixture (M3) swarms the edge of mixing machine, therefore available stable viscosity, the cathode system of mixing ratio in wet mixed It makes and uses slurry.
Process (B3) is preferably carried out from the viewpoint of simplifying manufacturing process or shortening manufacturing time with 1 stage.That is, The solid component concentration of mixture (M3) is identical as the solid component concentration of slurry presoma in preferable process (B3).
The incorporation time of above-mentioned wet mixed in process (B3) is not particularly limited, and for example, 5 minutes or more and 120 points Below clock.
The shear velocity of wet mixed in process (B3) is preferably 10.0sec-1Above and 70.0sec-1Range below It is interior, preferably 20.0sec-1Above and 65.0sec-1In following range, more preferably 30.0sec-1Above and 60.0sec-1With Under range in.
Cathode manufacture is used in slurry preparation section (C), above-mentioned by obtaining in the process (B) by preparing slurry presoma Further addition is selected from one or both of water-medium and the aqueous emulsion comprising water-based binder in slurry presoma Above liquid component and wet mixed, to prepare above-mentioned cathode manufacture slurry.
As the mixing machine for carrying out wet mixed of the cathode manufacture in slurry preparation section (C), it is preferable to use planet is transported Ejector half mixer more preferably uses planetary motion type planetary-type mixer.It, can be on one side with low by using such mixing machine Speed stirring is sufficiently mixed on one side.Therefore, the cutting of the strand of thickener caused by being stirred can be inhibited on one side and inhibited The mutual cohesion of water-based binder improves the dispersibility for constituting each material of cathode manufacture slurry on one side.Also, as its knot Fruit can obtain the more excellent cathode manufacture slurry of quality stability.
In addition, the dispersibility of obtained cathode manufacture slurry is more excellent, if therefore manufacturing use using such cathode Slurry can then obtain negative electrode active material layer more evenly.As a result, the more excellent electricity of battery behavior can be obtained Pond.
In addition, there there is no cathode manufacture with the shear velocity of the wet mixed in slurry preparation section (C) in present embodiment It is particularly limited to, for example, 5.0sec-1Above and 60.0sec-1In following range.
Cathode manufacture is not particularly limited with the incorporation time of the above-mentioned wet mixed in slurry preparation section (C), such as It is 5 minutes or more and 60 minutes or less.
It should be noted that cathode manufacture is manufactured with the cathode in slurry preparation section (C) and uses the solid component of slurry dense Degree can adjust by adjusting the concentration of aforesaid liquid ingredient, additive amount.
The manufacturing method of cathode manufacture slurry of the present embodiment can also carry out bubble removal step (D): vacuum is de- The process of bubble.Thereby, it is possible to remove the bubble being involved in slurry, the coating of slurry can be made to improve.
Vacuum defoamation can container to mixing machine, axle portion implement encapsulation process to remove bubble, can also move into other It is carried out after container.
<negative electrode battery electrode>
Fig. 1 is the sectional view for indicating an example of the structure of negative electrode battery electrode 100 of embodiment of the present invention. Negative electrode battery electrode 100 of the present embodiment includes current collector layer 101 and at least one side set on current collector layer 101 And the negative electrode active material layer 103 formed by the solid component of cathode manufacture slurry of the present embodiment.
Current collector layer 101 used in manufacture as negative electrode battery electrode 100 of the present embodiment, such as can To use the common collector being able to use in battery.
In the case that above-mentioned battery is lithium ion battery, as negative electrode collector, can be used for example copper, stainless steel, nickel, Titanium or their alloy, particularly preferred copper among these.
Shape about collector is not particularly limited, for example, can make in the range of with a thickness of 0.001~0.5mm With the collector of foil-like.
The thickness and density of negative electrode active material layer 103 of the present embodiment is appropriate according to usage of battery etc. It determines, therefore is not particularly limited, it generally can be according to well known information setting.
<manufacturing method of negative electrode battery electrode>
Then, the manufacturing method of negative electrode battery electrode 100 of the present embodiment is illustrated.
The manufacturing method of negative electrode battery electrode 100 of the present embodiment includes: by that will be related to by present embodiment And the obtained cathode of manufacturing method of cathode manufacture slurry manufacture and be coated on current collector layer 101 and dry with slurry, remove Water-medium, thus the process for forming negative electrode active material layer 103 in current collector layer 101.It is possible thereby to stably obtain collection The negative electrode battery electrode 100 excellent in adhesion of electrics layer 101 and negative electrode active material layer 103.
That is, negative electrode battery electrode 100 of the present embodiment can be by by cathode system of the present embodiment It makes and is coated in current collector layer 101 and is dried with slurry, remove water-medium, so that it is living to form cathode in current collector layer 101 Property material layer 103 and obtain.
Cathode manufacture of the present embodiment generally can use with the method that slurry is coated in current collector layer 101 Well known method.It is applied for example, reverse roll method, direct roller method, scraping blade method, scraper method, extrusion molding, curtain coating method, intaglio plate can be enumerated Cloth method, stick coating method, dip coating and extrusion etc..
Cathode manufacture of the present embodiment can only be coated on the single side of current collector layer 101 with slurry or be coated with In two sides.In the case where the two sides for being coated on current collector layer 101, it can be gradually coated with, can also be applied simultaneously with two sides with each single side Cloth.Furthermore it is possible to be continually or intermittently coated on the surface of current collector layer 101.The thickness of coating layer, length, width can be with It is suitably determined according to the size of battery.
The drying means of the cathode manufacture slurry of coating generally can use well known method.Such as it can independent or group It closes and uses hot wind, vacuum, infrared ray, far infrared, electron ray and low warm wind.Drying temperature is, for example, 30 DEG C or more and 350 DEG C range below.
Negative electrode battery electrode 100 of the present embodiment, which can according to need, to be suppressed.As the method for compacting, It generally can use well known method.For example, mold pressing, calender pressing etc. can be enumerated.Compacting pressure is not special It limits, for example, 0.2~3t/cm2Range.
The thickness of negative electrode battery electrode 100 of the present embodiment, density are appropriate according to usage of battery etc. It determines, therefore is not particularly limited, it generally can be not fixed according to well known information.
<battery>
Next, being illustrated to battery 150 of the present embodiment.Fig. 2 is to indicate embodiment party of the present invention The sectional view of an example of the structure of the battery 150 of formula.
Battery 150 of the present embodiment at least has anode 120, electrolyte 110 and cathode 130, cathode 130 Negative electrode battery electrode 100 of the present embodiment.In addition, battery 150 of the present embodiment can according to need packet Containing spacer.
Battery 150 of the present embodiment includes negative electrode battery electrode of the present embodiment due to cathode 130 100, therefore the powder falling of negative electrode active material layer when assembled battery is suppressed, the quality of battery, the cycle characteristics etc. of battery are good It is good.
Battery 150 of the present embodiment can make according to known methods.
Laminated body, coiling body can be used for example in electrode.As external packing body, can be properly used metal external packing body, Aluminium layer folds external packing body.The shape of battery can be the arbitrary shapes such as Coin shape, coin shape, piece type, cylinder type, square, platypelloid type Shape.
The anode 120 of battery can use well known manufacturing method manufacture.For example, using that will include at least just Pole active material and binder, the slurry further as needed comprising conductive auxiliary agent, thickener are coated on positive electrode collector simultaneously The anode of dry etc. method manufacture.
As a positive electrode active material, if the common positive active material for the anode that can be used in battery then without special It limits.Above-mentioned battery be lithium ion battery in the case where, it can be cited for example that lithium nickel composite oxide, lithium cobalt composite oxide, The composite oxides of the lithiums and transition metal such as complex Li-Mn-oxide, lithium-manganese-ni compound oxide；TiS2、FeS、MoS2It waited Cross metal sulfide；MnO,V2O5、V6O13、TiO2Equal transition metal oxides, olivine-type lithium phosphate etc..
Olivine-type lithium phosphate is including, for example, being selected from Mn, Cr, Co, Cu, Ni, V, Mo, Ti, Zn, Al, Ga, Mg, B, Nb and Fe In at least one kind of element, lithium, phosphorus and oxygen.Their compound can be in order to improve its characteristic and by the element portion of a part It is replaced into the compound of other elements with dividing.
Among these, preferably olivine-type iron lithium phosphate, lithium cobalt composite oxide, lithium nickel composite oxide, lithium manganese are compound Oxide, lithium-manganese-ni compound oxide.The high working potential and capacity of these positive active materials are also big, have big energy Metric density.Positive active material can be used singly or in combination of two or more.
Binder resin used in anode suitably selects depending on the application.It is, for example, possible to use the fluorine that can be dissolved in solvent It is binder resin, the water-based binder that can be dispersed in water etc..
As fluorine system binder resin, if being capable of forming electrode and do not limit especially if there is sufficient electrochemical stability It is fixed, it can be cited for example that Kynoar system resin, fluorubber etc..These fluorine system binder resins can be used alone, It can also be applied in combination two or more.Among these, preferred Kynoar system resin.Fluorine system binder resin for example can be molten It is used in N- methyl-pyrrolidon (NMP) equal solvent.
In addition, can be used as water-based binder resin, thickener, conductive auxiliary agent and constitute this above-mentioned embodiment party The identical material of each material for the cathode manufacture slurry that formula is related to.
As positive electrode collector, aluminium, stainless steel, nickel, titanium or their alloy etc. can be used, among these particularly preferably Aluminium.
As the electrolyte in the electrolyte of battery, well known lithium salts be can be used, and be selected according to the type of active material It selects.It can be cited for example that LiClO4、LiBF6、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiB10Cl10、 LiAlCl4、LiCl、LiBr、LiB(C2H5)4、CF3SO3Li、CH3SO3Li、LiCF3SO3、LiC4F9SO3、Li(CF3SO2)2N, low Grade fatty acid carboxylate lithium etc..
As the solvent of dissolution electrolyte, do not have then if the usually used solvent of the liquid component as dissolution electrolyte It is particularly limited to, ethylene carbonate (EC), propylene carbonate (PC), butylene carbonate (BC), dimethyl carbonate can be enumerated (DMC), the carbonates such as diethyl carbonate (DEC), methyl ethyl carbonate (MEC), vinylene carbonate (VC)；Gamma-butyrolacton, The lactones such as gamma-valerolactone；Trimethoxy-methane, 1,2- dimethoxy-ethane, diethyl ether, 2- Ethoxyethane, tetrahydrofuran, The ethers such as 2- methyltetrahydrofuran；The sulfoxide types such as dimethyl sulfoxide；1,3-dioxolane, 4- methyl-1, the oxa-s such as 3- dioxolanes Cyclopentanes；The nitrogenous class such as acetonitrile, nitromethane, formamide, dimethylformamide；Methyl formate, methyl acetate, acetic acid second The organic acid esters such as ester, butyl acetate, methyl propionate, ethyl propionate；Phosphotriester, diethylene glycol dimethyl ethers；Triethylene glycol diformazan Ethers；The sulfolane class such as sulfolane, methyl sulfolane；The oxazolidinones such as 3- methyl -2- oxazolidone；1, in 3-N-morpholinopropanesulfonic acid Sultone classes such as ester, Isosorbide-5-Nitrae-butyl sultone, naphthalene sulfonic acids lactone etc..These can be used alone, and electricity can be applied in combination 2 Kind or more.
As spacer, it can be cited for example that porosity spacer.The form of spacer can enumerate film, film, nonwoven Cloth etc..
As porosity spacer, it can be cited for example that the polyolefin-based porous spacer such as polypropylene-based, polyethylene-based； By the porosity interval of the formation such as Kynoar, polyethylene oxide, polyacrylonitrile, Kynoar hexafluoropropylene copolymer Part.
More than, embodiments of the present invention are described, but these are illustration of the invention, can also be used above-mentioned Various compositions in addition.
In addition, the present invention is not limited to embodiment above-mentioned, the deformation in the range of the purpose of the present invention can be reached, changed It is good equal comprising in the present invention.
Embodiment
Hereinafter, by embodiment and comparative example, the present invention will be described, but the present invention is not restricted to these.
(embodiment 1)
<production that slurry is used in the manufacture of water system cathode>
(1) process (A)
In luck of being expert at ejector half planetary-type mixer (size of kettle: 5L), the stone that surface is coated by amorphous carbon is put into Ink (average grain diameter d50: 16 μm, the specific surface area based on N2 adsorption BET method: 3.4m2/ g) 1500g, carboxymethyl cellulose powder (the MAC series of Nippon Paper corporation Sunrose (registered trademark), degree of etherification falling: 0.73, weight average molecular weight Mw:300000 is (poly- Ethylene glycol scaled value)) 1 particle coacervation of 2.95g and the about 30nm as conductive auxiliary agent (is based on nitrogen at the carbon black of chain shape Adsorb the specific surface area of BET method: 60m2/g)6.2g.It then, is 13.1sec in shear velocity-1, temperature: under conditions of 25 DEG C into 20 minutes dry type mixings of row, obtain powder mixture.
Hereinafter, average grain diameter d50It is measured by Microtrac corporation, MT3000 device, specific surface area uses Quantachrome Corporation corporation, Quanta Sorb, are found out by N2 adsorption BET method.
Here, surface is made in the following way by the graphite that amorphous carbon is coated.
By average grain diameter d50For 16 μm, specific surface area 3.4m2The natural graphite of/g is used as core material.
99.0 mass parts of natural graphite powder and 1.0 mass parts of coal system asphalt powder are passed through using V-Mixer Simple mixing is with solid phase mixing.Obtained mixed-powder is put into graphite crucible, under nitrogen flowing with 1300 DEG C of heat treatments 1 Hour, obtain the graphite that surface is coated by amorphous carbon.
(2) process (B1)
Then, in the planetary motion type planetary-type mixer for finishing above-mentioned dry type mixing process (A), according to what is obtained The solid component concentration of mixture (M2) adds water as the mode of 80 mass %.It thereafter, is 32.7sec in shear velocity-1, temperature Degree: 25 DEG C, carries out 20 minutes wet mixeds under conditions of atmospheric pressure, make to obtain mixture (M2) in water infiltration powder mixture.
(3) process (B2)
Then, in mixture (M2), carboxymethyl cellulose powder (Nippon Paper corporation Sunrose (registrar is added Mark) MAC series, degree of etherification falling: 0.73, weight average molecular weight Mw:300000 (polyethylene glycol scaled value)) 12.58g, then, according to The solid component concentration of obtained mixture (M3) adds water as the mode of 63 mass %, obtains mixture (M3).
(4) process (B3)
It then, is 52.3sec in shear velocity-1, temperature: 25 DEG C, under conditions of atmospheric pressure, mixture (M3) is carried out 30 minutes wet mixeds obtain cathode manufacture slurry presoma.
(5) process (C)
Then, preparation is by styrene-butadiene copolymer rubber (SBR) as water-based binder resin dispersion Yu Shuizhong's The SBR aqueous emulsion of 71 mass % of solid component concentration.Obtained SBR aqueous emulsion 77.64g is made an addition to and is finished In the planetary motion type planetary-type mixer of process (B3).
It thereafter, is 32.7sec in shear velocity-1, temperature: 15 minutes wet mixeds are carried out under conditions of 25 DEG C.
(6) process (D)
Then, vacuum defoamation is carried out, cathode manufacture slurry is obtained.
It should be noted that the final solid component concentration of cathode manufacture slurry by prepare cathode manufacture with slurry Water is added in the process (C) of material to be adjusted to 51 mass %.
<production of cathode>
It uses slurry that die coating machine is used to be coated on as the two sides of the copper foil of current collector layer obtained cathode manufacture and does It is dry.Then, obtained electrode is suppressed, obtains cathode.
<evaluation>
(1) the cathode manufacture viscosimetric analysis of slurry
Using Brookfield viscometer (Brookfield corporation, rotational viscometer), in 25 DEG C, shear velocity 3.4s-1Condition The lower measurement cathode manufacture viscosity of slurry.
(2) peeling strength test
The peel strength of obtained cathode is measured by following step.Cathode is cut into out wide 20mm, long 10cm, it will The single side of cathode is attached on the plate for having pasted double faced adhesive tape.Then, plate is fixed, by cathode with the speed edge of 100mm/min 90 ° of direction removings.3 peel strengths (mN/mm) at this time are measured, using its average value as peel strength.Here, the stripping of cathode It is measured from two sides of the intensity to cathode.Here, using the side of initial coating sizing-agent and drying as the face A in table 1, it will be with A The opposite side in face is as the face B.
Will be obtained evaluation result is shown in table 1.
(embodiment 2~4)
In addition to making the mixed proportion of the 1st thickener and the 2nd thickener (by total mixing of the 1st thickener and the 2nd thickener Amount be set as 100 mass %) and the solid component concentration of mixture (M2) become other than value shown in table 1 respectively, with embodiment 1 together Water system cathode manufacture slurry is prepared to sample respectively, carries out each evaluation respectively.Obtained result is shown in table 1.
(comparative example 1)
It does not add carboxymethyl cellulose powder in process (A), and adds carboxymethyl cellulose powder in process (B2) (the MAC series of Nippon Paper corporation Sunrose (registered trademark), degree of etherification falling: 0.73, weight average molecular weight Mw:300000 is (poly- Ethylene glycol scaled value)) 15.53g, attempts to make water system cathode manufacture slurry, the situation similarly to Example 1 in addition to this The cohesion of lower negative electrode active material largely occurs, and can not adjust water system cathode manufacture slurry.
(comparative example 2)
Carboxymethyl cellulose powder (the MAC of Nippon Paper corporation Sunrose (registered trademark) is added in process (A) Series, degree of etherification falling: 0.73, weight average molecular weight Mw:300000 (polyethylene glycol scaled value)) 15.53g, and in process (B2) not Carboxymethyl cellulose powder is added, prepares water system cathode manufacture slurry similarly to Example 1 in addition to this, is carried out respectively each Evaluation.The results obtained are shown in tables 1.
[table 1]
This application claims preferential based on Japanese publication Patent 2018-50411 filed on March 19th, 2018 Power, is disclosed full content and is incorporated herein.

Claims (23)

1. a kind of cathode manufacture manufacturing method of slurry,
Comprising:
By mixing negative electrode active material and the 1st thickener, to prepare including at least the negative electrode active material and the described 1st The process A of the mixture M 1 of thickener；
One of water-medium and the aqueous emulsion comprising water-based binder are selected from by adding in the mixture M 1 Or two or more liquid components and wet mixed is carried out, to prepare the process B of slurry presoma；With
By further adding the liquid component in the slurry presoma and carrying out wet mixed, to prepare cathode manufacture With the process C of slurry,
The process B at least successively includes:
The process B 1 of mixture M 2 is obtained and making the liquid component penetrate into mixture M 1；
The process B 2 of mixture M 3 is obtained and mixing the 2nd thickener and the liquid component in the mixture M 2；With
By the way that the dry thick mixing of the mixture M 3 is obtained the process B 3 of the slurry presoma.
2. the manufacturing method that slurry is used in cathode manufacture according to claim 1, wherein
In the process A, by the various powders shape substance for including at least the negative electrode active material and the 1st thickener with Powder state dry type mixing.
3. the manufacturing method that slurry is used in cathode manufacture according to claim 1 or 2, wherein
The 1st thickener that mixes in the process A with the 2nd thickener mixed in the process B 2 is same Class.
4. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 3, wherein
In the process B 2, the 2nd thickener is mixed with powder state.
5. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 4, wherein
The combined amount of 2nd thickener is more than the combined amount of the 1st thickener.
6. the manufacturing method that slurry is used in cathode manufacture according to claim 5, wherein
When total combined amount of 1st thickener and the 2nd thickener is set as 100 mass %, the 1st thickener Combined amount is 1 mass % or more and 45 mass % or less.
7. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 6, wherein
The solid component concentration of mixture M 3 described in the process B 3 is identical as the solid component concentration of the slurry presoma.
8. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 7, wherein
The solid component concentration of the slurry presoma in the process B 3 is set below described mixed in the process B 1 Close the solid component concentration of object M2.
9. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 8, wherein
The solid component concentration of the mixture M 2 in the process B 1 is 71 mass % or more and 95 mass % or less.
10. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 9, wherein
The solid component concentration of the mixture M 3 in the process B 3 is 55 mass % more than and less than 75 mass %.
11. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 10, wherein
The shear velocity of wet mixed in the process B 3 is set in 10.0sec-1Above and 70.0sec-1Range below It is interior.
12. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 11, wherein
The pH of the cathode manufacture slurry is 6.0 or more and 8.0 or less.
13. the manufacturing method that slurry is used in cathode manufacture according to any one of claim 1 to 12, wherein
The thickener includes cellulose-based water soluble polymer.
14. the manufacturing method that slurry is used in cathode manufacture according to claim 13, wherein
The degree of etherification falling of the cellulose-based water soluble polymer is 0.50 or more and 1.0 or less.
15. the manufacture of cathode described in 3 or 14 manufacturing method of slurry according to claim 1, wherein
The weight average molecular weight Mw of the cellulose-based water soluble polymer is 100000 or more.
16. according to claim 1 to the manufacturing method of cathode manufacture slurry described in any one of 15, wherein
The water-based binder includes styrene-butadiene copolymer rubber.
17. according to claim 1 to the manufacturing method of cathode manufacture slurry described in any one of 16, wherein
When the total amount of the solid component of the cathode manufacture slurry is set as 100 mass parts,
The content of the negative electrode active material is 70 mass parts or more and 99.97 below the mass,
Total content of 1st thickener and the 2nd thickener is 0.01 mass parts or more and 10.0 below the mass,
The content of the water-based binder is 0.01 mass parts or more and 10.0 below the mass.
18. according to claim 1 to the manufacturing method of cathode manufacture slurry described in any one of 17, wherein
The negative electrode active material includes carbon material.
19. according to claim 1 to the manufacturing method of cathode manufacture slurry described in any one of 18, wherein
The cathode manufacture also contains the conductive auxiliary agent being made of the material comprising carbon material with slurry.
20. the manufacturing method that slurry is used in cathode manufacture according to claim 19, wherein
The specific surface area based on N2 adsorption BET method of the conductive auxiliary agent is 50m2/ g or more.
21. a kind of negative electrode battery electrode,
It includes current collector layer and set on the current collector layer at least one side and as described in any one of claims 1 to 20 The negative electrode active material layer that is formed with the solid component of slurry of cathode manufacture.
22. a kind of battery,
It is the battery at least having anode, electrolyte and cathode,
The cathode includes negative electrode battery electrode described in claim 21.
23. a kind of manufacturing method of negative electrode battery electrode comprising following process:
The cathode obtained by the manufacturing method of cathode manufacture slurry described in any one of claims 1 to 20 is manufactured into use Slurry is coated on current collector layer and drying, removes the water-medium, to form negative electrode active material in the current collector layer Matter layer.
CN201910206422.7A 2018-03-19 2019-03-18 Cathode manufacture manufacturing method, the manufacturing method of negative electrode battery electrode, battery and negative electrode battery electrode of slurry Pending CN110289388A (en)

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