CN106159266B - A kind of negative electrode slurry preparation method reducing lithium ion battery expansion - Google Patents
A kind of negative electrode slurry preparation method reducing lithium ion battery expansion Download PDFInfo
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- CN106159266B CN106159266B CN201610798757.9A CN201610798757A CN106159266B CN 106159266 B CN106159266 B CN 106159266B CN 201610798757 A CN201610798757 A CN 201610798757A CN 106159266 B CN106159266 B CN 106159266B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention discloses a kind of negative electrode slurry preparation method of reduction lithium ion battery expansion comprising:Negative electrode active material and conductive agent is pre- dry-mixed;Sodium carboxymethylcellulose is dissolved in deionized water, obtains the CMC glue that concentration is 1.0-2.0%;Part CMC glue is added to negative electrode active material, in conductive agent mixture, high-speed stirred 0.5-1h;Residue CMC glue, high-speed stirred 1-3h is added;Modified SBR binder is added, moderate-speed mixer 0.3-1h adjusts viscosity.The present invention by artificial graphite and conductive agent it is pre- it is dry-mixed, glue is added in two portions and use method of the modification SBR as binder, artificial graphite arch formation is reduced, pole piece structure is changed, improves the cohesive force between particle, cathode expansion is reduced, while artificial graphite being inhibited to close slurry sedimentation.The present invention is for ternary lithium electricity, especially to the processing performance of high capacity power battery, capacity and the safety is improved is of great significance.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of negative electrode slurry system for reducing lithium ion battery expansion
Preparation Method.
Background technique
High capacity ternary battery has higher requirement to negative electrode material, such as high capacity, high-pressure solid, low bounce-back.Negative electrode material
High rebound rate keeps rectangular aluminum-shell battery firmly swollen, causes the appearance of battery product not up to standard always, becomes lithium battery industry and is badly in need of solution
One of certainly the problem of.
Through high temperature storage and circulation bulging often occurs for rectangular aluminum-shell battery in the market, and thickness increases 6-20%, wherein just
Pole expansion rate is 4%, and cathode expansion rate is 20% or more, therefore, it is considered that cathode expansion is the main reason for battery is firmly swollen.Cathode
Expansion cause core to deform, between positive and negative anodes and diaphragm formed cavity, cathode particle formed micro-crack, SEI film rupture with again
Group consumes electrolyte, so that battery electrochemical impedance increases, cycle performance is deteriorated, and the performance and safety belt to battery are come important
It influences.
Ningxin Zhang research shows that graphite cathode expansion mainly due to generated after embedding lithium it is irrecoverable expansion and
Cause, and thinks that this demi-inflation is mainly related with the structure of particle size, binder and pole piece.Pole piece structure is come
It says, most important influence factor is to close slurry mode.J.Christensen has studied stress point during graphite removal lithium embedded simultaneously
Cloth shows smaller with isotropism negative electrode material stress.But for isotropic artificial graphite, because generating frame between particle
Bridge, conjunction slurry is easily settled, is difficult to solve using traditional binder and conjunction slurry mode.
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, a kind of bearing for reduction lithium ion battery expansion is provided
Pole slurry preparation method.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of negative electrode slurry preparation method reducing lithium ion battery expansion, negative electrode slurry include the following steps:
(1) negative electrode active material and conductive agent is pre- dry-mixed;
(2) sodium carboxymethylcellulose is dissolved in deionized water, obtains the CMC glue that concentration is 1.0-2.0%;
(3) part CMC glue is added to negative electrode active material, in conductive agent mixture, high-speed stirred 0.5-1h;
(4) residue CMC glue, high-speed stirred 1-3h is added;
(5) modified SBR binder is added, moderate-speed mixer 0.3-1h adjusts viscosity, homogenate, sieving, adjust viscosity to
2000-6000mPa·s。
Further scheme, the step (3) and the stirring of (4) high speed are rotation revolving speed 2500-4000rpm, and revolve revolving speed
40-64rpm;Step (5) moderate-speed mixer rotation revolving speed 2000-2500rpm, revolve revolving speed 32-40rpm.
Further scheme, step (1) negative electrode active material are the pure artificial stones of isotropism formed through secondary granulation
Ink.
Further scheme, the amount of CMC glue is 10-35% in the step (3).
Further scheme, step (3) conductive agent are conductive black Sp.
Further scheme, modified SBR binder mass percentage content is 1-3% in the negative electrode slurry.
Beneficial effects of the present invention:The present invention by artificial graphite and conductive agent it is pre- it is dry-mixed, be added in two portions glue and
Use modified SBR as the method for binder, reduce artificial graphite arch formation, change pole piece structure, improves between particle
Cohesive force reduces cathode expansion, while artificial graphite being inhibited to close slurry sedimentation.The present invention is for ternary lithium electricity, especially to Gao Rong
It measures the processing performance of power battery, capacity and the safety is improved is of great significance.
Detailed description of the invention
Fig. 1 is negative electrode slurry preparation technology flow chart of the present invention.
Fig. 2 is embodiment 1 and comparative example 3,4 cathode expansion rate of comparative example.
Fig. 3 is 1 rheological curve of comparative example.
Specific embodiment
Present invention is further described in detail in the following with reference to the drawings and specific embodiments.
" the pure artificial graphite of isotropism is made through secondary granulation " used in the present invention and " the modified SBR binder " city Jun Ke
By being commercially available on field.
Embodiment 1
The pure artificial graphite of isotropism is made through secondary granulation in negative electrode active material use, and binder is modified SBR bonding
Agent, conductive agent are conductive black Sp, and glue is CMC aqueous solution, modified SBR binder mass percentage content in negative electrode slurry
It is 3%.
Negative electrode slurry preparation includes the following steps:(1) artificial graphite is pre- dry-mixed with conductive black Sp;(2) carboxymethyl is fine
It ties up plain sodium and is dissolved in deionized water, obtain the CMC glue that concentration is 1.0%;(3) the CMC glue that 10% is made in (2) is added mixed
It closes in material, sets rotation revolving speed 4000rpm, revolve revolving speed 64rpm, stirs 0.5h;(4) the CMC glue of residue 90% is added, if
Determine rotation revolving speed 4000rpm, revolve revolving speed 64rpm, stirs 3h;(5) modified SBR binder is added, sets rotation revolving speed
2000rpm, revolve revolving speed 40rpm, stirs 0.3h;(6) viscosity, homogenate, sieving are adjusted.Coating, roll pressing obtain pole piece.Stock discharge
When viscosity it is more uniform, viscosity 4851mPas, slurry shelve 48h viscosity be 4915mPas.Normal temperature shelf after pole piece roll-in
After 48h, expansion rate 1%;Full electric state cathode expansion rate is 17% after battery is made in pole piece, and empty electricity state cathode expansion rate is
9.6%.
Comparative example 1
This comparative example negative electrode active material is natural graphite, and binder is untreated SBR binder, and conductive agent is conductive charcoal
Black, glue is CMC aqueous solution, and untreated SBR binder mass percentage content in negative electrode slurry is 3%.
Negative electrode slurry preparation process is as follows:(1) sodium carboxymethylcellulose is dissolved in deionized water, and obtaining concentration is 1.0%
CMC glue;(2) conductive black Sp is added in (1), sets rotation revolving speed 4000rpm, and revolve revolving speed 64rpm, stirs 0.5h;
(3) natural graphite is added in (2), sets rotation revolving speed 4000rpm, revolve revolving speed 64rpm, stirs 3h;(5) it is added and does not locate
SBR binder is managed, rotation revolving speed 2000rpm is set, revolve revolving speed 40rpm, stirs 0.3h;(6) viscosity, homogenate, sieving are adjusted;Slurry
There is serious sedimentation phenomenon when material sieving.Slurry upper, middle and lower-ranking viscosity difference is larger, and upper layer viscosity is 500-1000mPa
S, lower layer's viscosity are up to 5000mPas or so, rheological curve such as Fig. 3.
Comparative example 2
The pure artificial graphite of isotropism is made through secondary granulation in the use of this comparative example negative electrode active material, and binder is to be modified
SBR binder, modified SBR binder mass percentage content in negative electrode slurry is 3%, and conductive agent is conductive black Sp, glue
Liquid is CMC aqueous solution.
Negative electrode slurry preparation process is as follows:(1) sodium carboxymethylcellulose is dissolved in deionized water, and obtaining concentration is 1.0%
CMC glue;(2) conductive black is added in (1), sets rotation revolving speed 4000rpm, and revolve revolving speed 64rpm, stirs 0.5h;(3)
Natural graphite is added in (2), rotation revolving speed 4000rpm is set, revolve revolving speed 64rpm, stirs 3h;(5) carboxylated is added
SBR binder is handled, rotation revolving speed 2000rpm is set, revolve revolving speed 40rpm, stirs 0.3h;(6) viscosity, homogenate, sieving are adjusted.
There is serious sedimentation phenomenon when being sieved in slurry.
Comparative example 3
The pure artificial graphite of isotropism is made through secondary granulation in the use of this comparative example negative electrode active material, and binder is not locate
SBR is managed, untreated SBR binder mass percentage content in negative electrode slurry is 3%, and conductive agent is conductive black Sp, glue
For CMC aqueous solution.
Negative electrode slurry preparation includes the following steps:(1) artificial graphite is pre- dry-mixed with conductive black;(2) carboxymethyl cellulose
Plain sodium is dissolved in deionized water, obtains the CMC glue that concentration is 1.0%;(3) mixing is added in the CMC glue that 10% is made in (2)
In material, rotation revolving speed 4000rpm is set, revolve revolving speed 64rpm, stirs 0.5h;(4) the CMC glue of residue 90%, setting is added
Rotation revolving speed 4000rpm, revolve revolving speed 64rpm, stirs 3h;(5) untreated SBR, moderate-speed mixer, rotation revolving speed is added
2000rpm, revolve revolving speed 40rpm, stirs 0.3h;(6) viscosity, homogenate, sieving are adjusted.Coating, roll pressing obtain pole piece.Stock discharge
When viscosity be 1512mPas, after slurry shelves 48h, slurry is settled.After pole piece roll-in after normal temperature shelf 48h, expansion rate
It is 6%;Full electric state cathode expansion rate is 24% after battery is made in pole piece, and empty electricity state cathode expansion rate is 17%.
Comparative example 4
This comparative example negative electrode active material is natural graphite, and binder is modified SBR, modified SBR matter in negative electrode slurry
Measuring degree is 3%, and conductive agent is conductive black Sp, and glue is CMC aqueous solution.
Slurry preparation includes the following steps:(1) artificial graphite is pre- dry-mixed with conductive black;(2) sodium carboxymethylcellulose
It is dissolved in deionized water, obtains the CMC glue that concentration is 1.0%;(3) mixture is added in the CMC glue that 10% is made in (2)
In, rotation revolving speed 4000rpm is set, revolve revolving speed 64rpm, stirs 0.5h;(4) glue of residue 90% is added, sets rotation
Revolving speed 4000rpm, revolve revolving speed 64rpm, stirs 3h;(5) carboxylated SBR is added, moderate-speed mixer sets rotation revolving speed
2000rpm, revolve revolving speed 40rpm, stirs 0.3h;(6) viscosity, homogenate, sieving are adjusted.Coating, roll pressing obtain pole piece.Pole piece roll-in
Afterwards after normal temperature shelf 48h, expansion rate 8.1%;Full electric state cathode expansion rate is 30% after battery is made in pole piece, and empty electricity state is negative
Pole expansion rate is 21%.
Embodiment 2
The pure artificial graphite of isotropism is made through secondary granulation in negative electrode active material use in the present embodiment, and binder is to change
Property SBR, modified SBR mass percentage content in negative electrode slurry is 1%, and conductive agent is conductive black, and glue is that CMC is water-soluble
Liquid.
Negative electrode slurry preparation includes the following steps:(1) artificial graphite is pre- dry-mixed with conductive black;(2) carboxymethyl cellulose
Plain sodium is dissolved in deionized water, obtains the CMC glue that concentration is 2.0%;(3) mixing is added in the CMC glue that 35% is made in (2)
In material, rotation revolving speed 4000rpm is set, revolve revolving speed 64rpm, stirs 1h;(4) glue of residue 65% is added, sets rotation
Revolving speed 2500rpm, revolve revolving speed 40rpm, stirs 1h;(5) hydroxylating SBR is added, moderate-speed mixer sets rotation revolving speed
2000rpm, revolve revolving speed 32rpm, stirs 1h;(6) viscosity, homogenate, sieving are adjusted.Coating, roll pressing obtain pole piece.When stock discharge
Viscosity is more uniform, viscosity 5023mPas, and it is 5137mPas that slurry, which shelves 48h viscosity,.Normal temperature shelf 48h after pole piece roll-in
Afterwards, expansion rate 1.1%;Full electric state cathode expansion rate is 16.8% after battery is made in pole piece, and empty electricity state cathode expansion rate is
10.2%.
Fig. 1 is negative electrode slurry preparation technology flow chart of the present invention.Fig. 2 is that embodiment 1 and comparative example 3,4 cathode of comparative example are swollen
Swollen rate.Fig. 3 is 1 rheological curve of comparative example.By the above embodiments and comparative example as it can be seen that artificial graphite and conductive agent it is pre- it is dry-mixed,
Glue is repeatedly added and cathode expansion can be effectively reduced using the method for modified SBR, while it is heavy to inhibit artificial graphite to close slurry
Drop.
Claims (6)
1. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion, which is characterized in that negative electrode slurry includes following step
Suddenly:
(1)Negative electrode active material and conductive agent is pre- dry-mixed;
(2)Sodium carboxymethylcellulose is dissolved in deionized water, obtains the CMC glue that concentration is 1.0-2.0%;
(3)Part CMC glue is added to negative electrode active material, in conductive agent mixture, high-speed stirred 0.5-1h;
(4)Residue CMC glue, high-speed stirred 1-3h is added;
(5)Modified SBR binder is added, moderate-speed mixer 0.3-1h adjusts viscosity, homogenate, sieving, adjusts viscosity to 2000-
6000mPa·s。
2. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion according to claim 1, which is characterized in that
The step(3)With(4)High speed stirring is rotation revolving speed 2500-4000rpm, and revolve revolving speed 40-64rpm;Step(5)Middling speed
Rotation revolving speed 2000-2500rpm is stirred, revolve revolving speed 32-40rpm.
3. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion according to claim 1, which is characterized in that
The step(1)Negative electrode active material is the pure artificial graphite of isotropism formed through secondary granulation.
4. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion according to claim 1, which is characterized in that
The step(3)The amount of middle CMC glue is step(2)In CMC adhesive liquid quantity obtained 10-35%.
5. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion according to claim 1, which is characterized in that
The step(3)Conductive agent is conductive black Sp.
6. a kind of negative electrode slurry preparation method for reducing lithium ion battery expansion according to claim 1, which is characterized in that
Modified SBR binder mass percent is 1-3% in the negative electrode slurry.
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