CN112382744A - Preparation method of negative electrode slurry for 3D printing - Google Patents
Preparation method of negative electrode slurry for 3D printing Download PDFInfo
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- CN112382744A CN112382744A CN202011254627.1A CN202011254627A CN112382744A CN 112382744 A CN112382744 A CN 112382744A CN 202011254627 A CN202011254627 A CN 202011254627A CN 112382744 A CN112382744 A CN 112382744A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
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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
- H01M4/13—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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
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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
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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 application discloses negative pole thick liquids preparation method that can be used to 3D printing in the chemical energy storage battery field, the carboxymethyl cellulose CMC is got to the title and is put into aquatic, and ultrasonic oscillation dissolves, adds silicon carbon material, conductive agent, SBR and uses the planet dispenser misce bene, gets 3D and prints the thick liquids. The cathode slurry provided by the application can be directly used for direct-writing 3D printing, a preformed pole piece is manufactured, and then drying is carried out to obtain the pole piece.
Description
Technical Field
The invention relates to the field of chemical energy storage batteries, in particular to a preparation method of negative electrode slurry for 3D printing.
Background
In recent years, with the continuous development and progress of science and technology, along with the rapid development of various portable electronic devices, electric vehicles, military weaponry, and the like, the demand for chemical power sources has been increasing, and the chemical power sources are required to have a high energy density. In weaponry, the reserved space of the power supply is generally irregular, and if a lithium ion battery (generally rectangular and cylindrical) commonly used in the current electronic field is used, the space utilization rate is not high, so that the specific energy of a battery system is low. The improvement of the space utilization rate is an important means for improving the specific energy of the battery system, so that the technology of the special-shaped battery equipment is rapidly developed. However, the research on the special-shaped power supply is delayed due to the limitation of the technical development of materials, production processes and the like.
The current commercial lithium ion battery mainly takes graphite as a negative electrode, the theoretical specific capacity is only 372mAh/g, and the improvement space of the energy density of the battery is limited. The silicon-based negative electrode material is considered to be a next generation high energy density lithium ion battery negative electrode material with great potential due to the advantages of high theoretical specific capacity, low lithium removal potential, rich reserves, environmental friendliness, low cost and the like. Therefore, the specific energy of the system can be greatly improved by adopting the silicon-carbon material to produce the special-shaped battery.
The traditional special-shaped battery adopts a die cutting method, and a cutting die meeting the space shape needs to be correspondingly designed, so that the research period is long, the die opening cost is high, and the research and development of new products are not facilitated. Therefore, the customized 3D printing is introduced to the production of the special-shaped battery, but the characteristics of the slurry required by the 3D printing are different from those of the slurry for general lithium ion production, and the use and stirring process of the solvent binder are particularly important because the viscosity of the slurry required by the 3D printing is high and the slurry is required to be uniformly mixed without agglomeration, so that at present, a negative electrode slurry specially used for the 3D printing is not available.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a cathode slurry specially used for 3D printing.
The invention discloses a preparation method of negative electrode slurry for 3D printing, which comprises the following steps:
s1, weighing sodium carboxymethylcellulose, adding the sodium carboxymethylcellulose into deionized water, and carrying out ultrasonic oscillation and dissolution to obtain a solution A;
s2, weighing the conductive agent, adding the conductive agent into the solution A, and dispersing by using a planetary dispersion machine to completely and uniformly mix the conductive agent with the solution A to obtain a solution B;
s3, weighing the silicon-carbon material, adding the silicon-carbon material into the solution B, and dispersing by using a planetary dispersion machine to completely and uniformly mix the silicon-carbon material with the solution B to obtain a solution C;
and S4, weighing styrene butadiene rubber, adding the styrene butadiene rubber into the solution C, and dispersing by using a planetary dispersion machine to completely and uniformly mix the styrene butadiene rubber and the solution C to obtain the cathode slurry suitable for 3D printing.
Preferably, in the step S1, the mass ratio of the sodium carboxymethyl cellulose to the deionized water is 3-8: 150-300.
Preferably, in step S1, the time of ultrasonic oscillation is 2 to 15 min.
Preferably, the conductive agent is one or more of superconducting carbon black, acetylene black, carbon fiber, carbon nanotube, ketjen black and graphene, and the mass ratio of the silicon-carbon material to the conductive agent is 100: 1-6.25.
Preferably, in the step S2, the operation of the planetary disperser is 400-1800 r/min for 2-15 min.
Preferably, the particle size of the silicon-carbon material is 1-50 μm.
Preferably, in the step S3, the operation of the planetary disperser is 400-1800 r/min for 2-15 min.
Preferably, the mass ratio of the styrene-butadiene rubber to the silicon-carbon material is as follows: 4-8: 100.
Preferably, in the step S4, the operation of the planetary disperser is 400-1800 r/min for 2-15 min.
Preferably, the viscosity of the negative electrode slurry for 3D printing is 50cps to 2000cps, the slurry is a pseudoplastic fluid, and the slurry is sieved by a sieve of 150 meshes to 300 meshes. The preferred negative electrode slurry has a viscosity of 800 to 1500cps or 500 to 1200cps, and a pseudoplastic fluid, i.e., a fluid whose viscosity decreases with increasing shear rate, exhibits a smaller and smaller ratio of shear stress to shear rate on the flow curve. The slurry can pass through a 150-300-mesh sieve, so that a printing plug is avoided, and the qualification rate of the 3D printing pole piece is improved.
The invention has the advantages that: 3D prints silicon carbon negative pole thick liquids, in order to reduce the thickness that 3D printed, guarantee the formability that 3D printed the pole piece, the shower nozzle that 3D printed generally is 50 mu m ~ 200 mu m, avoids having large granule group to cause the end cap in the thick liquids, can't print, and thick liquids need sieve before carrying out 3D and printing, and wherein require the material particle diameter few, and avoid agglomerating.
Adopt ultrasonic oscillation and planet dispenser to disperse in batches and get 3D and print silicon carbon negative pole thick liquids, its homogenate time is shorter, reduces traditional mode stirring time for 10min more than the shortest 12h, and adopts the planet dispenser to disperse, can optimize the double planet and can not solve the powder and hold the group phenomenon in viscous material, reduces the thick liquids and reunite the rate and improve the mixing performance of thick liquids. A screening process is added before the paste is printed, so that the qualification rate and the performance of the 3D printed pole piece are improved; and the slurry meets the rheological property of shear thinning by selecting the binder and the gelling agent and adjusting the proportion of the gelling agent and the deionized water, is more suitable for extrusion type 3D printing, meets the requirements of a special-shaped power supply and a customized battery, and has the characteristics of excellent electrical property and high specific energy of a printed negative plate.
The cathode slurry provided by the invention can be directly used for direct-writing 3D printing to prepare a preformed pole piece, and then the preformed pole piece is dried to obtain the pole piece.
Drawings
Fig. 1 is a graph of viscosity-shear rate for a 3D printed silicon carbon anode slurry prepared in example 1;
FIG. 2 is a diagram of a 3D printed profiled silicon carbon negative plate prepared in example 1;
fig. 3 is a discharge curve diagram of the first charge and discharge when the button type pole piece assembly is prepared according to two embodiments of the present invention.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
2.5g of sodium carboxymethylcellulose (CMC) is weighed and added into 100g of deionized water, and the solution A is obtained after ultrasonic oscillation and dissolution for 10 min. And (3) weighing 1.6g of superconducting carbon black and 1.6g of carbon nano tubes, adding into the solution A, and rotating for 2min at 1200r/min, 1min at 1800/min and 2min at 1200r/min by using a planetary dispersing machine to obtain a solution B. Weighing 50g of silicon-carbon material, adding into the solution B, and rotating for 2min at 1200r/min, 1min at 1800/min and 2min at 1200r/min by adopting a planetary dispersion machine to obtain a solution C; weighing 3.75g of Styrene Butadiene Rubber (SBR) and adding the SBR into the solution C, rotating for 2min at 1200r/min, 1min at 1800/min and 2min at 1200r/min by adopting a planetary dispersing machine, wherein the viscosity of the slurry is 800-1500 cps, and sieving by using a 200-mesh sieve to obtain the 3D printed cathode slurry.
Example 2
Weighing 1.7g of sodium carboxymethylcellulose (CMC) and adding into 100g of deionized water, and dissolving for 8min by ultrasonic oscillation to obtain a solution A. 0.6g of superconducting carbon black and 0.8g of carbon nano tube are weighed and added into the solution A, and a planetary dispersion machine is adopted to rotate for 1min at 1200r/min, 1min at 1800/min and 1min at 1200r/min to obtain a solution B. Weighing 50g of silicon-carbon material, adding into the solution B, and rotating for 5min at 400r/min, 20min at 800r/min, 2min at 1800r/min, 20min at 800r/min and 5min at 400r/min by adopting a planetary dispersion machine to obtain a solution C; weighing 2.5g of Styrene Butadiene Rubber (SBR) and adding the SBR into the solution C, rotating for 15min at 800r/min, 2min at 1800r/min and 15min at 800r/min by adopting a planetary dispersion machine, wherein the viscosity of the slurry is 500-1200 cps, and sieving by a 150-mesh sieve to obtain the 3D printed cathode slurry.
Comparative example 1
Weighing 1.7g of sodium carboxymethylcellulose (CMC) and adding into 100g of deionized water, and mechanically stirring for 2 hours to obtain a solution A. 0.6g of superconducting carbon black and 0.8g of carbon nano tube are weighed and added into the solution A, and the solution B is obtained by stirring for 3 hours. Weighing 50g of silicon-carbon material, adding into the solution B, and stirring for 3 hours to obtain a solution C; weighing 2.5g of Styrene Butadiene Rubber (SBR) and adding the SBR into the solution C, stirring for 3 hours by adopting a common method to obtain the solution C, wherein the viscosity of the slurry is 600-1200 cps, and sieving with a 400-mesh sieve to obtain the 3D printed negative electrode slurry.
Application example
The slurry prepared in the example 1 and the example 2 is printed on a copper foil according to a designed special-shaped pattern through 3D printing, the yield of a pole piece is 100% in the example 1 by using a 200-micron sprayer, the yield of the pole piece is 100% in the example 2 by using a 100-micron sprayer, the yield of the pole piece is 100% in the comparative example 1 by using a 200-micron sprayer, and the yield of the pole piece is 0%.
Respectively printing the slurry prepared in the embodiment 1 and the embodiment 2 on a copper foil through 3D, drying the slurry at 100 ℃ for 12h according to the pole piece forming rate, and preparing a negative pole piece with phi 16mm by using a mould; preparing a CR2032 button cell in an inert atmosphere glove box, wherein the cathode of the cell is a lithium sheet, and 1M LiPF6 and EC/DEC jointly form electrolyte (the volume ratio is 1: 1); the lithium ion battery is charged and discharged at 0-1.5V under the multiplying power of 0.1C, the first discharging gram specific capacity of the embodiment 1 is 654.77mAh/g, the first charging gram specific capacity is 552.29mAh/g, the first discharging gram specific capacity of the embodiment 2 is 661.83mAh/g, the first charging gram specific capacity is 571.97mAh/g, and the comparison of the discharging performance is shown in figure 3.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of negative electrode slurry for 3D printing; the method is characterized in that: the method comprises the following steps:
s1, weighing sodium carboxymethylcellulose, adding the sodium carboxymethylcellulose into deionized water, and carrying out ultrasonic oscillation and dissolution to obtain a solution A;
s2, weighing the conductive agent, adding the conductive agent into the solution A, and dispersing by using a planetary dispersion machine to completely and uniformly mix the conductive agent with the solution A to obtain a solution B;
s3, weighing the silicon-carbon material, adding the silicon-carbon material into the solution B, and dispersing by using a planetary dispersion machine to completely and uniformly mix the silicon-carbon material with the solution B to obtain a solution C;
and S4, weighing styrene butadiene rubber, adding the styrene butadiene rubber into the solution C, and dispersing by using a planetary dispersion machine to completely and uniformly mix the styrene butadiene rubber and the solution C to obtain the cathode slurry suitable for 3D printing.
2. The method for preparing a negative electrode paste usable for 3D printing according to claim 1, characterized in that: in the step S1, the mass ratio of the sodium carboxymethyl cellulose to the deionized water is 3-8: 150-300.
3. The method for preparing the negative electrode paste usable for 3D printing according to claim 2, characterized in that: in step S1, the ultrasonic oscillation time is 2-15 min.
4. The method for preparing the negative electrode paste usable for 3D printing according to claim 3, characterized in that: the conductive agent is one or more of superconducting carbon black, acetylene black, carbon fibers, carbon nanotubes, Ketjen black and graphene, and the mass ratio of the silicon-carbon material to the conductive agent is 100: 1-6.25.
5. The method for preparing the negative electrode paste for 3D printing according to any one of claims 1 to 4, wherein the method comprises the following steps: in the step S2, the operation of the planetary dispersion machine is 400-1800 r/min for 2-15 min.
6. The method for preparing the negative electrode paste usable for 3D printing according to claim 5, characterized in that: the particle size of the silicon-carbon material is 1-50 mu m.
7. The method for preparing the negative electrode paste usable for 3D printing according to claim 6, characterized in that: in the step S3, the operation of the planetary dispersion machine is 400-1800 r/min for 2-15 min.
8. The preparation method of the negative electrode paste for 3D printing according to claim 7, wherein the mass ratio of the styrene-butadiene rubber to the silicon-carbon material is as follows: 4-8: 100.
9. The method for preparing a negative electrode paste for 3D printing according to claim 8, wherein in the step S4, the operation of the planetary disperser is 400-1800 r/min for 2-15 min.
10. The method for preparing the negative electrode paste for 3D printing according to claim 9, wherein the viscosity of the negative electrode paste for 3D printing is 50cps to 2000cps, and the paste is a pseudoplastic fluid and passes through a 150-300 mesh sieve.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101521271A (en) * | 2008-02-26 | 2009-09-02 | 比亚迪股份有限公司 | Method for preparing cathode paste and cathode of lithium ion battery |
| CN202070307U (en) * | 2011-04-13 | 2011-12-14 | 雷立猛 | Double-planet double-power mixing dispersion machine |
| CN102593423A (en) * | 2012-02-28 | 2012-07-18 | 天津市捷威动力工业有限公司 | Method for quickly preparing anode slurry and anode of lithium ion battery |
| CN105552367A (en) * | 2015-12-21 | 2016-05-04 | 中盐安徽红四方锂电有限公司 | CNT-containing lithium ion battery waterborne positive electrode paste and preparation method therefor |
| CN108172750A (en) * | 2017-12-07 | 2018-06-15 | 银隆新能源股份有限公司 | The preparation method of graphite negative electrode of lithium ion battery highly viscous slurry |
| CN110752354A (en) * | 2019-09-24 | 2020-02-04 | 中国地质大学（武汉） | Universal 3D printing nano electrode slurry and preparation method thereof |
| CN111900391A (en) * | 2020-06-19 | 2020-11-06 | 温州大学新材料与产业技术研究院 | Lithium ion battery cathode slurry and preparation method thereof |
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2020
- 2020-11-11 CN CN202011254627.1A patent/CN112382744A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101521271A (en) * | 2008-02-26 | 2009-09-02 | 比亚迪股份有限公司 | Method for preparing cathode paste and cathode of lithium ion battery |
| CN202070307U (en) * | 2011-04-13 | 2011-12-14 | 雷立猛 | Double-planet double-power mixing dispersion machine |
| CN102593423A (en) * | 2012-02-28 | 2012-07-18 | 天津市捷威动力工业有限公司 | Method for quickly preparing anode slurry and anode of lithium ion battery |
| CN105552367A (en) * | 2015-12-21 | 2016-05-04 | 中盐安徽红四方锂电有限公司 | CNT-containing lithium ion battery waterborne positive electrode paste and preparation method therefor |
| CN108172750A (en) * | 2017-12-07 | 2018-06-15 | 银隆新能源股份有限公司 | The preparation method of graphite negative electrode of lithium ion battery highly viscous slurry |
| CN110752354A (en) * | 2019-09-24 | 2020-02-04 | 中国地质大学（武汉） | Universal 3D printing nano electrode slurry and preparation method thereof |
| CN111900391A (en) * | 2020-06-19 | 2020-11-06 | 温州大学新材料与产业技术研究院 | Lithium ion battery cathode slurry and preparation method thereof |
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