CN115763802A - Positive electrode slurry, positive plate and lithium ion secondary battery - Google Patents
Positive electrode slurry, positive plate and lithium ion secondary battery Download PDFInfo
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- CN115763802A CN115763802A CN202211336184.XA CN202211336184A CN115763802A CN 115763802 A CN115763802 A CN 115763802A CN 202211336184 A CN202211336184 A CN 202211336184A CN 115763802 A CN115763802 A CN 115763802A
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Abstract
The invention discloses a positive electrode slurry, a positive plate and a lithium ion secondary battery, and relates to the technical field of lithium ion secondary batteries. The positive electrode slurry contains a nickel-rich positive electrode active substance and a sulfonic group modified 1,1-difluoroethylene copolymer binder, and through the reaction of a sulfonic group and residual alkali on the surface of a nickel-rich positive electrode material, the HF elimination reaction of the residual alkali and 1,1-difluoroethylene polymer is inhibited, the formation of a conjugated polyene structure is prevented, the gelation of the positive electrode slurry is avoided, and the viscosity and the electrical properties of the positive electrode slurry are improved. The positive electrode slurry is suitable for preparing positive plates and lithium ion secondary batteries, and the obtained batteries have low internal resistance and good constant current charging ratio.
Description
Technical Field
The invention relates to the technical field of lithium ion secondary batteries, in particular to a positive electrode slurry, a positive plate and a lithium ion secondary battery.
Background
With the rapid development of new energy industry, lithium ion secondary batteries are receiving much attention as important chemical energy in the field of new energy. The positive electrode in the lithium ion secondary battery is one of the core components, the higher the energy density is, the larger the capacity is, the better the dynamic performance of the battery is, and the nickel-rich positive electrode active material has high energy density, and is more and more popular with long-endurance automobiles. However, with the increase of nickel content in the positive active material, the surface residual alkali of the positive active material is high, and the elimination reaction of HF elimination between the positive active material and 1,1-difluoroethylene copolymer forms a conjugated polyene structure, so that a gel phenomenon is generated when the slurry is finally prepared, and the pole piece coating cannot be smoothly carried out.
The prior art discloses a positive electrode mixture for a secondary battery, which comprises a lithium nickel composite oxide positive electrode active material, a vinylidene fluoride binder and an organic acid, and inhibits the gelation of high nickel positive electrode slurry by introducing carboxylic acid groups. However, the binding energy between carboxylic acid groups and lithium ions is larger, the lithium ions are not easy to dissociate, the internal resistance is larger, the conductivity is poorer, the constant current charging ratio is low, the rapid charge and discharge is not facilitated, and the dynamic performance of the battery still needs to be improved.
Disclosure of Invention
The invention aims to solve the technical problems of large internal resistance, low constant current charging ratio and insufficient dynamic performance of the battery of the conventional positive electrode slurry of the lithium ion secondary battery, and provides the positive electrode slurry.
The invention also aims to provide application of the positive electrode slurry in the positive electrode plate.
It is still another object of the present invention to provide a use of the positive electrode slurry in a lithium ion secondary battery.
The above purpose of the invention is realized by the following technical scheme:
the positive electrode slurry comprises solid matters and a solvent, wherein the solid matters comprise a nickel-rich positive electrode active substance, a conductive agent and a binder, the mass content of the nickel-rich positive electrode active substance in the solid matters is 90-98%, and the mass content of the binder is 0.5-5%;
the adhesive is 1,1-difluoroethylene copolymer with sulfonic acid groups, and has the following structural unit containing sulfonic acid groups:
wherein R is 1 、R 2 、R 3 Each independently represents a hydrogen atom, a fluorine atom or an alkyl group having 1 to 2 carbon atoms; x is selected from one or more of ester, amide and ether structures with a main chain of 2-20 carbon atoms;
the structural formula of the nickel-rich positive electrode active material is as follows: li x Ni y M 1-y O 2 Wherein X is more than or equal to 0.9 and less than or equal to 1.1,0.6 and less than or equal to 1,M is selected from one or more of Co, mn and Al.
Wherein, it is required to be noted that:
the nickel-rich positive active material has high nickel content, so that the residual alkali on the surface of the active material is increased, a conjugated polyene structure which is easy to crosslink is formed after the nickel-rich positive active material reacts with the 1,1-difluoroethylene copolymer, the finally obtained positive slurry has a gelation phenomenon, and a positive plate cannot be prepared. The nickel-rich positive active material in the positive slurry is rich in nickel and has high energy density, and the binder is 1,1-difluoroethylene copolymer with sulfonic acid groups and can react with residual alkali on the surface of the nickel-rich positive active material, so that the HF elimination reaction between the residual alkali and 1,1-difluoroethylene polymer is inhibited, the formation of a conjugated polyolefin structure is prevented, and the occurrence of chemical crosslinking is avoided, so that the gel phenomenon caused by the increase of the nickel content in the positive slurry is avoided.
In the binder, the length of X can influence the swing degree of sulfonic acid groups, when the main chain of X is a plurality of atoms, sulfonic acid groups are easy to swing and easily migrate to an aluminum foil interface, and the binding power of the binder is enhanced, but when the atoms of the main chain of X are too many and the main chain is too long, the content of the sulfonic acid groups in the binder with the same quality is too small, so that the gelation of positive electrode slurry is not favorably prevented, and when the content of the sulfonic acid groups is too small, lithium sulfonate groups which are converted into lithium ion conductivity by reacting with an electrolyte are also less, so that the internal resistance of a battery is not favorably reduced, and the constant current charging ratio is not favorably improved.
In addition, when the mass content of the binder is too low or the content of the positive active material is too high, the sulfonic acid group cannot completely react residual alkali on the surface of the nickel-rich positive active material, the binding force between the active material and the conductive agent is poor, and the active material of the battery is easy to fall off from a current collector in the circulation process, so that the battery is subjected to circulation and water jumping; when the mass content of the binder is too high or the content of the nickel-rich cathode active material is too low, the effective contact between the nickel-rich cathode active material and the conductive agent is reduced, the obtained cathode slurry is used in the battery, the capacity of the battery is reduced, the internal resistance is increased, the dynamic performance of the battery is also reduced, and when the mass content of the binder is too high, molecular chains are mutually entangled, and the gelation phenomenon also occurs.
The solvent of the positive electrode slurry is preferably N-methyl pyrrolidone; the conductive agent of the positive electrode slurry is preferably one or more of conductive graphite, conductive carbon black, acetylene black, carbon nanotubes and graphene, wherein the mass content of the conductive agent in solid substances is preferably 0.1-5%.
The binder may be copolymerized from 1,1-difluoroethylene with one or more of 2-acrylamido-2-methylpropanesulfonic acid, 2-methyl-2-sulfoethyl 2-acrylate, 2-trifluoromethyl-2-sulfoethyl 2-acrylate, 3-allyl-2-hydroxy-1-propanesulfonic acid, and perfluoro (4-methyl-3,6-dioxa-7-octene) sulfonic acid.
Preferably, the mass content of the nickel-rich positive electrode active material in the solid matter is 95-98%, and the mass content of the binder is 1-2%.
Preferably, the molar content of the sulfonic acid group-containing structural unit in the binder is 0.1 to 5%.
The content of sulfonic acid groups in the binder is too low to fully react with residual alkali, so that the gelation of the positive electrode slurry is inhibited; and the content of the sulfonic acid group is too high, so that the crystallinity of 1,1-difluoroethylene copolymerization is reduced, the electrolyte corrosion resistance of the adhesive in the battery is reduced, and the long-term cycle performance is not facilitated.
More preferably, the molar content of the sulfonic acid group-containing structural unit in the binder is 0.8 to 1.5%, still more preferably 1 to 1.2%.
Specifically, the weight average molecular weight of the binder is 65 to 300 ten thousand.
More preferably, the weight average molecular weight of the binder is 100 to 150 ten thousand, and still more preferably 122 ten thousand.
The binder is 1,1-difluoroethylene copolymer with sulfonic acid groups, and when the molecular weight of the binder is too low, the length of a molecular chain is low, so that the binder is not beneficial to the improvement of binding power; when the molecular weight is too large, the copolymer is slowly dissolved, which affects the production efficiency.
Preferably, the viscosity of the positive electrode slurry is 5000 to 15000mPa · s, more preferably 6000 to 8000mPa · s.
The viscosity of the slurry is low, the slurry is easy to settle, the content of general solvents is high, the energy consumption for volatilizing the solvents is high, and the production benefit is influenced; the viscosity of the slurry is too high, the fluidity of the slurry in the pipeline is poor, and the production efficiency is not favorable. In addition, the performance of the prepared battery can be controlled by controlling the viscosity of the positive electrode slurry, the viscosity of the positive electrode slurry is low, the stripping force of the generally obtained positive electrode plate is low, and the service life and the stability of the battery are influenced.
The positive electrode slurry can be prepared by the following preparation method:
the nickel-rich positive electrode active substance, the conductive agent and the sulfonic acid monomer copolymer 1,1-difluoroethylene are uniformly mixed, and the mixture is stirred to synthesize the slurry after the solvent is added.
The invention also protects the application of the positive electrode slurry in the preparation of the positive electrode plate.
The invention particularly protects a positive plate which is prepared from the positive electrode slurry.
The binder in the positive electrode slurry is 1,1-difluoroethylene copolymer with sulfonic acid groups, and the sulfonic acid groups in the positive electrode slurry react with residual alkali to inhibit the gelation of the positive electrode slurry, so that the positive electrode sizing material can be smoothly used for pole piece coating. The content of the binder in the positive electrode slurry and the length of X in the binder are controlled, so that the obtained binder is strong in binding power, and the prepared positive electrode plate is good in stripping performance.
The invention particularly relates to a lithium ion secondary battery, and the lithium ion secondary battery is a positive plate prepared from the positive electrode slurry.
According to the invention, sulfonic acid groups are introduced into the 1,1-difluoroethylene copolymer as a binder, and can react with residual alkali on the surface of a nickel-rich positive active material, so that the formation of a conjugated polyene structure is prevented, chemical crosslinking is avoided, the gelation phenomenon of positive slurry is avoided, and the sulfonic acid groups can react with an electrolyte and are converted into lithium sulfonate groups with high lithium ion conductivity, so that the prepared battery has lower internal resistance and higher constant current charge ratio, and the battery can be endowed with better dynamics.
Compared with the prior art, the invention has the beneficial effects that:
the binder of the anode slurry disclosed by the invention has a sulfonic acid group side chain with a certain length, so that the gelation phenomenon can be avoided, the anode slurry does not gelate after standing for 12 hours, the slurry can flow, the peel strength of an anode plate prepared from the anode slurry is 68-168N/m, the capacity of the prepared lithium ion secondary battery is more than 2.28Ah, the internal resistance is lower than 4.96m omega, and the constant current charging ratio is more than 80.4%.
Drawings
FIG. 1 is a picture of the positive electrode slurry of example 1 after standing for 12 hours;
fig. 2 is a picture of the positive electrode slurry of comparative example 1 after being left standing for 12 hours.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
The positive electrode slurry comprises a solid substance and a solvent, wherein the solid substance is a positive electrode active substance, a conductive agent and a binder, and the positive electrode active substance is LiNi 0.8 Co 0.1 Mn 0.1 O 2 The binder is 2-acrylamide-2-methylpropanesulfonic acid modified 1,1-difluoroethylene copolymer, the conductive agent is high-purity conductive carbon black (ultra high SUPER P Li), the solvent is N-methylpyrrolidone, and the balance of the solid matter is the conductive agent except the nickel-rich positive electrode active substance and the binder;
the parameters of the cathode slurry are detailed in table 1.
TABLE 1 anode slurry parameter Table of example 1
The positive electrode slurry can be prepared by the following method comprising the following steps:
adding LiNi into a double-planet stirrer 0.8 Co 0.1 Mn 0.1 O 2 The active substance, the conductive agent and the binder are gradually added with a plurality of N-methyl pyrrolidone (NMP), the mixture is stirred at high speed of 1500rpm to synthesize slurry, and finally the initial viscosity of the positive electrode slurry is adjusted to 7230 mPas by adding NMP solvent and testing by adopting a Bohler Fei rotary viscometer.
Examples 2 to 9
A positive electrode slurry, which is different from example 1 in the following point in table 2.
TABLE 2 parameter tables of positive electrode pastes of examples 1 to 9
The preparation method of the cathode slurry is the same as that of example 1.
Comparative example 1
A positive electrode slurry, the preparation method of which is the same as that in example 1, except that 2-acrylamido-2-methylpropanesulfonic acid monomer is not added in the preparation of 1,1-difluoroethylene copolymer, and the molecular weight Mw of the binder is 118 ten thousand.
Comparative example 2
A positive electrode slurry is different from the examples in that the binder used is Acomata Kynar HSV900.
Comparative example 3
A positive electrode slurry, which is different from example 1 in that the binder is acrylic acid copolymerized PVDF, wherein the molecular weight of the binder is Mw 116 ten thousand.
Comparative example 4
A positive electrode slurry was different from example 1 in that the mass content of the binder in the positive electrode slurry was 0.1%.
Comparative example 5
A positive electrode slurry was different from example 1 in that the mass content of the binder in the positive electrode slurry was 7%.
Result detection
5363 and detecting the content of sulfonic acid groups of the 1,1-difluoroethylene copolymer:
acid-base titration method: 0.2g of 1, 1-difluoroethylene copolymer was dissolved in 19.8g of acetone at about 80 ℃ and 1g of pure water was added to prepare a titrated 1,1-difluoroethylene copolymer solution. Neutralization titration was carried out at room temperature using 0.01mol/L aqueous sodium hydroxide solution using phenolphthalein as an indicator.
Detecting the weight average molecular weight of the adhesive:
the weight average molecular weight of the copolymer was measured by Gel Permeation Chromatography (GPC), and the mobile liquid was N, N-dimethylacetamide (DMAc) in terms of polymethyl methacrylate.
And (3) testing the viscosity of the positive electrode slurry:
120g of the slurry is placed in a 150ml beaker, sealed by a sealing film and placed in a 2520.2 ℃ water bath and kept stand for 1h. The viscosity was measured using a Bohler fly rotary viscometer, model DV2TLVTJ0, model 63, at a speed of 12 rpm.
And (3) testing the stripping force of the positive plate:
and (3) uniformly coating the two sides of the slurry on an aluminum foil with the thickness of 12um by using a scraper, baking the aluminum foil in a blast oven at 120 ℃ for 40min, wherein the density of the single-side coated surface is 160g/m & lt 2 & gt, the density of the double-side coated surface is 320g/m & lt 2 & gt, rolling the aluminum foil by using a roller press, and controlling the compaction density to be 3.5g/cm & lt 3 & gt to obtain the positive pole piece. Then, one side of 3M HVB double-sided tape (19mm × 60mm) was attached to one end of the steel plate, then the negative electrode sheet was cut into 20mm × 200mm strips, one side of the positive electrode active layer was attached to the double-sided tape, and the adhesion was measured as the stress at which the aluminum foil was peeled off at a speed of 100mm/min in the 180 ° direction in an atmosphere of 25 ℃ and a relative humidity of 50%.
Testing the performance of the lithium ion secondary battery:
(1) Preparation of lithium ion secondary battery:
and fully stirring and uniformly mixing the artificial graphite serving as the negative electrode material, acetylene black serving as a conductive agent, styrene-butadiene emulsion serving as a bonding agent and a carboxymethyl cellulose sodium deionized water solvent system serving as a dispersing agent, and coating the mixture on a copper foil of a negative current collector to obtain a negative electrode sheet. The diaphragm adopts a porous PE diaphragm, the electrolyte of the diaphragm is 1mol/L LiPF6 solution, and the solvents are ethylene carbonate, diethyl carbonate and ethyl methyl carbonate. And finally assembling the positive plate, the negative plate and the diaphragm containing the positive electrode slurry into a soft-package battery with the volume of about 3Ah (1C constant volume).
(2) Testing internal resistance:
and when the battery core is charged to 50% of capacity, detecting the internal resistance of the battery by using a 1kHz voltage internal resistance tester.
(3) Constant current charge ratio:
discharging the battery cell to 3.0V at a constant current of 0.33C at 25 ℃ and 5 ℃, standing for 10min, and then charging to 4.35V at a constant current of 2C; then changing constant voltage charging until the charging current is less than or equal to 0.02C; and the capacity of the charging stage in the constant current stage is C1, and the capacity of the charging stage in the constant voltage stage is C2, so that the constant current charging ratio = C1/(C1 + C2).
(4) Battery capacity:
discharging the battery cell to 3.0V at a constant current of 0.33C at 25 ℃ and 5 ℃, and standing for 10min; then charging to 4.35V at a constant current of 1.0C; then changing constant voltage charging until the charging current is less than or equal to 0.02C; and the capacity of the constant-current charging stage is Q1, the capacity of the constant-voltage charging stage is Q2, and the capacity of the battery is Q1+ Q2. The test results are detailed in tables 3 and 4.
TABLE 8978 molecular weight of zxft 8978-difluoroethylene copolymer and molar content of sulfonic acid group-containing structural units
TABLE 4 performances of the positive electrode slurry, the positive electrode sheet and the lithium ion secondary battery
As can be seen from table 3 and table 4, in the positive electrode slurry prepared according to the present invention, the content of the nickel-rich positive electrode active material and the binder, the source of the sulfonic acid group in the binder, the molar content of the sulfonic acid group-containing structural unit, and the molecular weight of the binder all affect the performance of the obtained positive electrode slurry, the positive electrode sheet, and the lithium ion secondary battery. As can be seen from the data in table 4, the greater the viscosity of the positive electrode slurry, the greater the peel strength of the positive electrode sheet is not necessarily (as in examples 1 and 3), which indicates that the viscosity of the positive electrode slurry does not have a simple linear trend in the influence on the peel force of the positive electrode sheet. Whereas the binders in comparative examples 1 and 2 did not contain a sulfonic acid group, gelation occurred in the positive electrode slurry. Comparative example 3 is modified by carboxylic acid group, the obtained lithium ion secondary battery has higher internal resistance and poorer constant current charging ratio, and the lower the internal resistance of the battery, the higher the constant current charging ratio, which shows that the dynamic performance of the battery is better, and is more beneficial to quick charge and discharge, namely the battery is modified by carboxylic acid group, and the dynamic performance of the battery is not as good as that of sulfonic acid group. The slurry in comparative example 5 was left to stand for 12 hours, causing gelation, and it was difficult to coat the positive electrode sheet in actual production.
Fig. 1 and 2 are diagrams showing the positive electrode slurry of example 1 and comparative example 1 after being left to stand for 12 hours, and it can be seen that the positive electrode slurry of example 1 is ungelled and in a flowable state, and can be coated with a positive electrode sheet, while the positive electrode slurry of comparative example 1 is gelled and cannot flow, and it is difficult to coat a positive electrode sheet in actual production.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The positive electrode slurry comprises solid matters and a solvent, wherein the solid matters comprise a nickel-rich positive electrode active substance, a conductive agent and a binder, and the positive electrode slurry is characterized in that the mass content of the nickel-rich positive electrode active substance in the solid matters is 90-98%, and the mass content of the binder is 0.5-5%;
the adhesive is 1,1-difluoroethylene copolymer with sulfonic acid groups, and has the following structural units containing sulfonic acid groups:
wherein R is 1 、R 2 、R 3 Each independently represents a hydrogen atom, a fluorine atom or an alkyl group having 1 to 2 carbon atoms; x is selected from one or more of ester, amide and ether structures with a main chain of 2-20 carbon atoms;
the structural formula of the nickel-rich positive electrode active material is as follows: li x Ni y M 1-y O 2 Wherein X is more than or equal to 0.9 and less than or equal to 1.1,0.6 and less than or equal to 1,M is selected from one or more of Co, mn and Al.
2. The positive electrode slurry according to claim 1, wherein the solid material contains the nickel-rich positive electrode active material in an amount of 95 to 98% by mass and the binder in an amount of 1 to 2% by mass.
3. The positive electrode slurry according to claim 1, wherein the binder contains a sulfonic acid group-containing structural unit in an amount of 0.1 to 4.5 mol%.
4. The positive electrode slurry according to claim 3, wherein the binder contains the sulfonic acid group-containing structural unit in an amount of 0.8 to 1.5 mol%.
5. The positive electrode slurry according to claim 1, wherein the weight average molecular weight of the binder is 65 to 300 ten thousand.
6. The positive electrode slurry according to claim 5, wherein the weight average molecular weight of the binder is 100 to 150 ten thousand.
7. The positive electrode slurry according to claim 6, wherein the viscosity of the positive electrode slurry is 5000 to 15000 mPas.
8. Use of the positive electrode slurry according to any one of claims 1 to 7 for the preparation of a positive electrode sheet.
9. A positive electrode sheet, characterized in that it is produced from the positive electrode slurry according to claims 1 to 7.
10. A lithium ion secondary battery comprising a positive electrode sheet prepared from the positive electrode slurry according to claims 1 to 7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116613321A (en) * | 2023-07-18 | 2023-08-18 | 宁德时代新能源科技股份有限公司 | Composite cathode material, additive, cathode plate, secondary battery and electricity utilization device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116613321A (en) * | 2023-07-18 | 2023-08-18 | 宁德时代新能源科技股份有限公司 | Composite cathode material, additive, cathode plate, secondary battery and electricity utilization device |
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