CN111244454A - High-proportion silicon cathode water system composite binder and application thereof - Google Patents
High-proportion silicon cathode water system composite binder and application thereof Download PDFInfo
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- CN111244454A CN111244454A CN201910958226.5A CN201910958226A CN111244454A CN 111244454 A CN111244454 A CN 111244454A CN 201910958226 A CN201910958226 A CN 201910958226A CN 111244454 A CN111244454 A CN 111244454A
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- 239000011230 binding agent Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 30
- 239000010703 silicon Substances 0.000 title claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229920000642 polymer Polymers 0.000 claims abstract description 51
- 229920003048 styrene butadiene rubber Polymers 0.000 claims abstract description 18
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims abstract description 17
- 239000004642 Polyimide Substances 0.000 claims abstract description 13
- 229920001721 polyimide Polymers 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 11
- 229910052744 lithium Inorganic materials 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000006258 conductive agent Substances 0.000 claims description 9
- 239000002210 silicon-based material Substances 0.000 claims description 9
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000006230 acetylene black Substances 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000011889 copper foil Substances 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229910021426 porous silicon Inorganic materials 0.000 claims description 2
- 239000006183 anode active material Substances 0.000 claims 1
- 239000002174 Styrene-butadiene Substances 0.000 abstract description 16
- 238000010438 heat treatment Methods 0.000 abstract description 6
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000004816 latex Substances 0.000 abstract description 3
- 229920000126 latex Polymers 0.000 abstract description 3
- 239000011115 styrene butadiene Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000007773 negative electrode material Substances 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 239000006245 Carbon black Super-P Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000007719 peel strength test Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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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- Electrochemistry (AREA)
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Abstract
The invention relates to a high-proportion silicon negative pole aqueous composite binder, which is prepared by mixing a polymer A, a polymer B and a polymer C, mixing the mixture into a negative pole piece, and then heating the negative pole piece in vacuum; the polymer A is water-soluble Polyimide (PI), the polymer B is at least one of polyacrylic acid (PAA) or polymethacrylic acid (PMAA), the polymer C is water-soluble styrene-butadiene latex (SBR), the water-based composite binder combines good cohesiveness of the PI, the PAA (PMAA) and the SBR, shows good tensile property, can form a cross-linked network after being heated, improves the binding effect, can well adapt to the expansion of the volume of the silicon negative electrode, and improves the cycle stability of the silicon negative electrode.
Description
Technical Field
The application belongs to the field of lithium battery manufacturing, and particularly relates to the field of lithium battery silicon cathodes.
Background
At present, graphite is a commonly used negative electrode material in lithium ion batteries, the theoretical specific capacity (372 mAh/g) of the graphite is low, the application requirement of high-energy density batteries cannot be met, a new negative electrode material is needed to be replaced, and a silicon-based material is the most promising replacement option: for example, the silica material has extremely high theoretical specific capacity (more than 2100 mAh/g) when being used as the negative electrode material of the lithium battery. However, in the process of charging and discharging of the silicon-based material, when lithium ions are inserted into the silicon crystal, the silicon particles generate huge volume change, the volume expansion rate of the silicon-oxygen material can reach more than 150%, and the volume expansion rate of the pure silicon material can even reach more than 360%. Along with the insertion and the extraction of lithium, the silicon-based material can expand and contract continuously, so that the separation of part of the silicon-based material from the conductive agent and the current collector is easily caused by the huge volume change, and the material pulverization phenomenon is caused; causing the capacity to decline rapidly and seriously hindering the commercial application of the capacity.
The requirements on the performance of the binder are stricter aiming at the fact that the silicon-based negative electrode material undergoes huge volume change in the charging and discharging processes, and the existing binders such as polyvinylidene fluoride (PVDF), carboxymethyl cellulose (CMC), styrene butadiene latex (SBR) and the like can not meet the application requirements of the silicon negative electrode. Therefore, the development of a high-performance aqueous binder which is compatible with the existing mass production process is urgently needed to maintain the stable structure of the silicon-based negative electrode in the charging and discharging processes and prolong the cycle life of the battery.
Disclosure of Invention
The purpose of the invention is as follows: the problem of pole piece pulverization caused by volume expansion and contraction of the negative electrode in the charging and discharging process of the silicon negative electrode of the lithium battery is solved.
The technical scheme is as follows: a high-proportion silicon negative pole water system composite binder is characterized in that a polymer A, a polymer B and a polymer C are mixed and then mixed into a negative pole piece, and then the negative pole piece is heated in vacuum; the polymer A is water-based polyimide PI, the polymer B is polyacrylic acid PAA and/or polymethacrylic acid (PMAA), and the polymer C is water-based styrene-butadiene rubber (SBR).
Preferably, the polymer A, the polymer B and the polymer C are mixed in the following mixing ratio: the polymer A accounts for 10-50% of the total mass of the composite binder; the polymer B accounts for 25-75% of the total mass of the composite binder; the polymer C accounts for 5-25% of the total mass of the composite binder.
Preferably, the molecular weights of the polymers are respectively as follows: the molecular weight of the polymer A and the polymer B is more than 15w, and the particle size of the polymer C is between 50nm and 300 nm.
A high-proportion silicon negative pole water system composite binder is used for preparing a negative pole of a lithium battery, and comprises the following specific steps: s1: the three polymers A, B, C need to be respectively prepared into aqueous solutions with certain mass ratios and then mixed, the polymer A needs to be prepared into 1-10% aqueous solution, the polymer B needs to be prepared into 10-30% aqueous solution, and the polymer C needs to be prepared into 1-10% aqueous solution;
s2: mixing the three aqueous solutions to prepare a composite binder, and adjusting the pH value of the composite binder to 5-8 by using alkali liquor;
s3, adding a negative electrode active substance and a conductive agent into the aqueous solution of the binder in a certain sequence, coating the mixed slurry on a copper foil, and then drying in vacuum to cut into electrode plates;
s4: and putting the cut electrode slice into a vacuum drying furnace again to be heated at 140-200 ℃.
Preferably, the negative electrode active material is a silicon-based material:
preferably, the silicon-based material is silicon oxide (SiOx), nano silicon, micro silicon or porous silicon.
Preferably, the conductive agent is one or more of graphite, acetylene black, Super P, Super S, graphene and carbon nanotubes.
The preferable scheme is that the usage amount of the composite binder accounts for 1-20% of the total mass of the negative pole piece.
The preferable scheme is that the prepared negative electrode battery is subjected to vacuum heating at the temperature of 140-200 ℃ for 2-6h, and then three polymers are subjected to crosslinking reaction.
Has the advantages that: the polymer A is water-soluble Polyimide (PI), the polymer B is at least one of polyacrylic acid (PAA) or polymethacrylic acid (PMAA), the polymer C is water-soluble styrene-butadiene latex (SBR), the water-based composite binder combines good cohesiveness of the PI, the PAA (PMAA) and the SBR, shows good tensile property, can form a cross-linked network after being heated, improves the binding effect, can well adapt to the expansion of the volume of the silicon negative electrode, and improves the cycle stability of the silicon negative electrode.
Drawings
FIG. 1 shows the pull-out force test after pole pieces are made of the aqueous composite binder.
FIG. 2 is a drawing force test of pole pieces made of the water-based composite adhesive.
Fig. 3 shows cycle test data for 11Ah cells prepared at three ratios.
Detailed Description
Example 1:
the application of the PI-PAA-SBR composite binder in the silicon negative electrode of the lithium battery is as follows: the negative pole piece is prepared from SiOx (mixed carbon), conductive agent carbon black (Super-P) and composite binder according to the mass ratio of 7.5:1: 1.5. Preparing PI into 7.5% aqueous solution, PAA into 25% aqueous solution and SBR into 5% aqueous solution, mixing the three binders according to the mass ratio of 2:6:2), and adjusting the pH value of the mixed aqueous solution to (5-9) by using NaOH. Adding a negative electrode active material, conductive carbon and the like into a binder aqueous solution in a certain sequence, and adding water with the total mass fraction of 20-40% to mix and homogenize. And (3) after the prepared negative pole piece is rolled, putting the rolled negative pole piece into a vacuum drying oven, and heating for 6 hours in vacuum at the temperature of 140 ℃. And (5) preparing the finished negative pole piece. The peel strength test results are shown in fig. 1.
Example 2:
the application of the PI-PAA-SBR composite binder in the silicon negative electrode of the lithium battery is as follows: the negative pole piece is prepared from SiOx (mixed carbon), conductive agent carbon black (Super-P) and composite binder according to the mass ratio of 7:1.5: 1.5. PI is prepared into a 5% aqueous solution, PAA is prepared into a 30% aqueous solution, SBR is prepared into a 5% aqueous solution, three binders are mixed according to the mass ratio of 3:6:1, and NaOH is used for adjusting the pH value of the mixed aqueous solution to (5-9). Adding a negative electrode active material, conductive carbon and the like into a binder aqueous solution in a certain sequence, and adding water with the total mass fraction of 20-40% to mix and homogenize. And (3) after the prepared negative pole piece is rolled, putting the rolled negative pole piece into a vacuum drying oven, and heating for 4 hours in vacuum at 180 ℃. And (5) preparing the finished negative pole piece. The peel strength test results are shown in fig. 1.
Example 3:
the application of the PI-PAA-SBR composite binder in the silicon negative electrode of the lithium battery is as follows: the negative pole piece is prepared from SiOx (mixed carbon), conductive agent carbon black (Super-P) and composite binder according to the mass ratio of 7.5:1.5: 1. PI is prepared into 10% aqueous solution, PAA is prepared into 20% aqueous solution, SBR is prepared into 5% aqueous solution, three binders are mixed according to the mass ratio of 2.5:6:1.5, and NaOH is used for adjusting the pH value of the mixed aqueous solution to (5-9). Adding a negative electrode active material, conductive carbon and the like into a binder aqueous solution in a certain sequence, and adding water with the total mass fraction of 20-40% to mix and homogenize. And (3) after the prepared negative pole piece is rolled, putting the rolled negative pole piece into a vacuum drying oven, and heating for 2 hours in vacuum at the temperature of 200 ℃. And (5) preparing the finished negative pole piece. The peel strength test results are shown in fig. 1.
Example 4
The application of the PI-PAA-SBR composite binder in the silicon negative electrode of the lithium battery is as follows: the negative pole piece is prepared from SiOx (mixed carbon), conductive agent carbon black (Super-P) and composite binder according to the mass ratio of 6:3: 1. PI is prepared into 10% aqueous solution, PAA is prepared into 20% aqueous solution, SBR is prepared into 5% aqueous solution, three binders are mixed according to the mass ratio of 3:6:1, and NaOH is used for adjusting the pH value of the mixed aqueous solution to (5-9). Adding a negative electrode active material, conductive carbon and the like into a binder aqueous solution in a certain sequence, and adding water with the total mass fraction of 20-40% to mix and homogenize. And (3) after the prepared negative pole piece is rolled, putting the rolled negative pole piece into a vacuum drying oven, and heating for 4 hours in vacuum at 160 ℃. And (5) preparing the finished negative pole piece. And adding an electrolyte of FEC: DMC: EC =1:1:1 into the cathode and a 532 system cathode on the current market to prepare an 11Ah soft-package battery cell (64 mm 148mm 6.7 mm), and evaluating the soft-package battery cell. The capacity test results are shown in fig. 2. The cycle life test results are shown in fig. 3.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined by the appended claims and their equivalents.
Claims (9)
1. A high-proportion silicon negative pole water system composite binder is characterized in that a polymer A, a polymer B and a polymer C are mixed and then mixed into a negative pole piece, and then the negative pole piece is heated in vacuum; the polymer A is water-based polyimide PI, the polymer B is polyacrylic acid PAA and/or polymethacrylic acid (PMAA), and the polymer C is water-based styrene-butadiene rubber (SBR).
2. The high-proportion silicon anode aqueous system composite binder as claimed in claim 1, wherein the polymer A, the polymer B and the polymer C are mixed in a ratio of: the polymer A accounts for 10-50% of the total mass of the composite binder; the polymer B accounts for 25-75% of the total mass of the composite binder; the polymer C accounts for 5-25% of the total mass of the composite binder.
3. The high-proportion silicon anode aqueous composite binder as claimed in claim 1, wherein the molecular weights of the polymers are as follows: the molecular weight of the polymer A and the polymer B is more than 15w, and the particle size of the polymer C is between 50nm and 300 nm.
4. The application of the high-proportion silicon negative electrode aqueous composite binder disclosed in claims 1-3 is characterized in that the application is used for preparing a negative electrode of a lithium battery, and the specific steps are as follows:
s1: the three polymers A, B, C need to be respectively prepared into aqueous solutions with certain mass ratios and then mixed, the polymer A needs to be prepared into 1-10% aqueous solution, the polymer B needs to be prepared into 10-30% aqueous solution, and the polymer C needs to be prepared into 1-10% aqueous solution;
s2: mixing the three aqueous solutions to prepare a composite binder, and adjusting the pH value of the composite binder to 5-8 by using alkali liquor;
s3, adding a negative electrode active substance and a conductive agent into the aqueous solution of the binder in a certain sequence, coating the mixed slurry on a copper foil, and then drying in vacuum to cut into electrode plates;
s4: and putting the cut electrode slice into a vacuum drying furnace again to be heated at 140-200 ℃.
5. The high-proportion silicon anode aqueous composite binder application as claimed in claim 4, wherein the anode active material is a silicon-based material.
6. The high-proportion silicon negative electrode aqueous composite binder as claimed in claim 5, wherein the silicon-based material is silicon oxide (SiOx), nano-silicon, micro-silicon, or porous silicon.
7. The application of the high-proportion silicon negative electrode aqueous composite binder as claimed in claim 4, wherein the conductive agent is one or more of graphite, acetylene black, Super P, Super S, graphene and carbon nanotubes.
8. The application of the high-proportion silicon negative pole aqueous composite binder as claimed in claim 4, wherein the usage amount of the composite binder accounts for 1-20% of the total mass of the negative pole piece.
9. The application of the high-proportion silicon cathode water system composite binder as claimed in claim 4, wherein the prepared cathode battery is heated in vacuum at 140-200 ℃ for 2-6h to enable the three polymers to generate a crosslinking reaction.
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| CN111668488A (en) * | 2020-06-17 | 2020-09-15 | 浙江中科玖源新材料有限公司 | Binder for silicon-carbon negative electrode, silicon-carbon negative electrode plate and lithium ion battery |
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| CN113258068A (en) * | 2021-04-28 | 2021-08-13 | 东莞市创明电池技术有限公司 | Binder for silicon negative electrode of lithium ion battery, negative electrode slurry and preparation method of negative electrode slurry |
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| CN112279982B (en) * | 2020-10-29 | 2023-02-03 | 珠海冠宇电池股份有限公司 | Binder for silicon-based negative electrode and lithium ion battery containing same |
| CN113258068A (en) * | 2021-04-28 | 2021-08-13 | 东莞市创明电池技术有限公司 | Binder for silicon negative electrode of lithium ion battery, negative electrode slurry and preparation method of negative electrode slurry |
| CN113258068B (en) * | 2021-04-28 | 2022-08-26 | 东莞市创明电池技术有限公司 | Binder for silicon negative electrode of lithium ion battery, negative electrode slurry and preparation method of negative electrode slurry |
| CN116093331A (en) * | 2023-04-06 | 2023-05-09 | 宁德新能源科技有限公司 | Secondary battery and electronic device |
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