CN109509869B - Dry mixing process for lithium ion battery anode - Google Patents
Dry mixing process for lithium ion battery anode Download PDFInfo
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- CN109509869B CN109509869B CN201811445092.9A CN201811445092A CN109509869B CN 109509869 B CN109509869 B CN 109509869B CN 201811445092 A CN201811445092 A CN 201811445092A CN 109509869 B CN109509869 B CN 109509869B
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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
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dry mixing process for a lithium ion battery anode, which comprises the following steps: (1) adding an active substance and a powdery conductive agent into a stirring cylinder, and stirring and mixing; (2) adding the binder into the stirring cylinder, and stirring and mixing; (3) adding a solvent accounting for 50-85% of the total weight of the solvent into a stirring cylinder, and stirring and mixing; (4) adding the slurry conductive agent into a stirring cylinder, vacuumizing, stirring and mixing; (5) adding the rest solvent, continuously vacuumizing, stirring and mixing to obtain the lithium ion battery anode slurry; the invention firstly mixes the powder at high speed, then adds a proper amount of solvent to moisten the powder material, and then stirs the mixture at low speed to form high-viscosity slurry; further crushing agglomerated particles, accelerating the dissolution of the binder and uniformly dispersing materials by using shearing force formed by high-speed dispersion; through the control to the feeding sequence and the material mixing process conditions, the materials are uniformly mixed, and the stability and the material mixing efficiency of the slurry are improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dry mixing process for a lithium ion battery anode.
Background
The lithium ion battery has the advantages of high energy density, environmental friendliness, long cycle life and the like, and is widely applied to the fields of 3C digital codes, energy storage, electric tools, transportation and the like. The manufacturing process has a great influence on the quality of the lithium ion battery, and the mixing is the first step of the whole manufacturing process and has an important influence on the subsequent process and the quality of the lithium ion battery.
The traditional mixing method of the lithium ion battery anode material is wet mixing, and the specific mode is as follows: the method has the defect of poor dispersing effect of powder materials such as the conductive agent, the active substance and the like in low-viscosity glue solution, and is influenced by the dissolving characteristic of the adhesive, the whole glue preparation process needs 8-10 hours, the consumed time is long, and the mixing efficiency is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a dry mixing process for a lithium ion battery anode, and solves the problems of low efficiency and poor dispersibility of the existing mixing method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a dry mixing process for a lithium ion battery anode comprises the following steps:
(1) adding an active substance and a powdery conductive agent into a stirring cylinder, and stirring and mixing;
(2) adding the binder into the stirring cylinder, and stirring and mixing;
(3) adding a solvent accounting for 50-85% of the total weight of the solvent into a stirring cylinder, and stirring and mixing;
(4) adding a slurry conductive agent into a stirring cylinder, vacuumizing to-0.085 to-0.1 MPa, and stirring and mixing;
(5) adding the rest solvent, continuously vacuumizing to-0.085 to-0.1 MPa, and stirring and mixing to obtain the lithium ion battery anode slurry.
Preferably, in the step (1), the stirring and mixing conditions include a stirring speed of 20-25 rpm, a dispersing speed of 1500-1800 rpm, and a stirring and mixing time of 10-20 minutes.
Preferably, in the step (2), the stirring and mixing conditions include a stirring speed of 25-30 rpm, a dispersing speed of 1500-1800 rpm, and a stirring and mixing time of 10-20 minutes.
Preferably, in the step (3), the stirring and mixing conditions include a stirring speed of 25 to 30rpm, a dispersing speed of 300 to 400rpm, and a stirring and mixing time of 30 minutes.
Preferably, in the step (4), the stirring and mixing conditions include a stirring speed of 33-38 rpm, a dispersing speed of 1500-1800 rpm, and a stirring and mixing time of 120-180 minutes.
Preferably, in the step (5), the stirring and mixing conditions include a stirring speed of 20 to 25rpm, a dispersing speed of 200 to 300rpm, and a stirring and mixing time of 30 to 60 minutes.
Compared with the prior art, the invention has the following technical effects:
according to the dry mixing process for the lithium ion battery anode, provided by the invention, active substances, a conductive agent and a binder are added step by step to carry out high-speed mixing on powder, so that aggregates of the conductive agent can be fully crushed and dispersed, and the dry powder is stirred at a high speed to realize micro mixing, thereby forming a good conductive network; adding a proper amount of solvent to wet the powdery material, and stirring at a low speed to form high-viscosity slurry; then, supplementing a slurry-shaped conductive agent, further crushing agglomerated particles through a shearing force formed by high-speed dispersion, accelerating the dissolution of the binder and uniformly dispersing the materials; and finally supplementing the residual solvent to adjust the viscosity to obtain the lithium ion battery anode slurry.
According to the invention, through controlling the feeding sequence and the mixing process conditions, the powdery materials are fully and uniformly mixed, and the stability of the slurry and the mixing efficiency are improved.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
All the starting materials in the present invention, the sources of which are not particularly limited, may be either commercially available or prepared according to conventional methods well known to those skilled in the art.
All the raw materials used in the present invention are not particularly limited in purity, and the present invention preferably employs a purity which is conventional in the field of analytical purification or composite materials.
In order to solve the technical problems of low efficiency and poor dispersibility of the existing mixing method, the invention provides a dry mixing process for a lithium ion battery anode, which comprises the following steps:
(1) adding an active substance and a powdery conductive agent into a stirring cylinder of a planetary stirrer, and stirring and mixing for 10-20 minutes under the conditions that the stirring speed is 20-25 rpm and the dispersion speed is 1500-1800 rpm;
(2) adding a binder into a stirring cylinder, and stirring and mixing for 10-20 minutes under the conditions that the stirring speed is 25-30 rpm and the dispersion speed is 1500-1800 rpm;
(3) adding a solvent accounting for 50-85% of the total weight of the solvent into a stirring cylinder, and stirring and mixing for 30 minutes under the conditions that the stirring speed is 25-30 rpm and the dispersion speed is 300-400 rpm;
(4) adding a slurry-like conductive agent into a stirring cylinder, vacuumizing to-0.085 to-0.1 MPa, and stirring and mixing for 120 to 180 minutes under the conditions that the stirring speed is 33 to 38rpm and the dispersion speed is 1500 to 1800 rpm;
(5) and adding the rest solvent, continuously vacuumizing to-0.085 to-0.1 MPa, and stirring and mixing for 30 to 60 minutes under the conditions that the stirring speed is 20 to 25rpm and the dispersion speed is 200 to 300rpm to obtain the lithium ion battery anode slurry.
According to the present invention, the types of the active material and the powdered conductive agent are not particularly limited, and may be well known to those skilled in the art, for example, the active material is one or more combinations of lithium manganate, ternary material, and lithium iron phosphate; the powdery conductive agent is one or a combination of KS-6, S-O, VGCF and Super P.
According to the invention, the slurry-like conductive agent is one or two combinations of carbon nanotubes and graphene.
The solvent is selected from common solvents for preparing the lithium ion battery anode slurry, for example, the solvent is NMP;
the binder is selected from binders commonly used for preparing the lithium ion battery anode slurry, for example, the binder is PVDF.
The lithium ion battery positive electrode dry mixing process provided by the invention is further explained by specific examples below.
Example 1
A dry mixing process for a lithium ion battery anode comprises the following steps:
(1) adding lithium manganate, Super P and KS-6 powder into a stirring cylinder of a planetary stirrer, stirring at the speed of 20rpm and the dispersion speed of 1650rpm, starting circulating water, and stirring for 10 minutes;
(2) adding PVDF into a stirring cylinder, stirring at the speed of 28rpm and the dispersion speed of 1650rpm, starting circulating water, and stirring for 20 minutes;
(3) adding NMP accounting for 68% of the total weight of the solvent into a stirring cylinder, stirring at 30rpm and a dispersion speed of 400rpm, starting circulating water, and stirring for 30 minutes;
(4) adding the carbon nano tube conductive slurry into a stirring cylinder, stirring at 35rpm and 1760rpm, starting circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 165 minutes;
(5) adding the residual NMP, stirring at 20rpm and dispersing at 220rpm, starting circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 45 minutes.
Example 2
A dry mixing process for a lithium ion battery anode comprises the following steps:
(1) adding the lithium manganate, the ternary powder and the Super P powder into a stirring cylinder of a planetary stirrer, wherein the stirring speed is 20rpm, the dispersion speed is 1570rpm, starting circulating water, and stirring for 15 minutes;
(2) adding PVDF into a stirring cylinder, stirring at the speed of 25rpm and the dispersion speed of 1600rpm, starting circulating water, and stirring for 20 minutes;
(3) adding NMP accounting for 62% of the total weight of the solvent into a stirring cylinder, stirring at 30rpm and a dispersion speed of 400rpm, starting circulating water, and stirring for 30 minutes;
(4) adding the carbon nano tube conductive slurry into a stirring cylinder, vacuumizing to-0.085 to-0.1 MPa, stirring at 38rpm and 1750rpm at the dispersion speed, starting circulating water, and stirring for 150 minutes;
(5) adding residual NMP, stirring at 22rpm and 200rpm, starting circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 40 minutes.
Example 3
A dry mixing process for a lithium ion battery anode comprises the following steps:
(1) adding lithium iron phosphate, ternary and Super P powder into a stirring cylinder of a planetary stirrer, stirring at 22rpm and 1630rpm, starting circulating water, and stirring for 15 minutes;
(2) adding PVDF into a stirring cylinder, stirring at the speed of 30rpm and the dispersion speed of 1680rpm, starting circulating water, and stirring for 15 minutes;
(3) adding NMP accounting for 72 percent of the total weight of the solvent into a stirring cylinder, stirring at 28rpm and 380rpm, starting circulating water, and stirring for 30 minutes;
(4) adding the carbon nano tube conductive slurry into a stirring cylinder, vacuumizing to-0.085-0.1 MPa, stirring at the speed of 38rpm and the dispersion speed of 1640rpm, starting circulating water, and stirring for 150 minutes;
(5) adding residual NMP, vacuumizing to-0.085-0.1 MPa, stirring at 22rpm and 260rpm, starting circulating water, and stirring for 50 min.
Comparative example 1
A lithium ion battery anode mixing process comprises the following steps:
(1) adding lithium manganate, ternary polymer, Super P, PVDF and NMP accounting for 65% of the total weight of the solvent into a stirring cylinder of a planetary stirrer, stirring at a speed of 30rpm and a dispersion speed of 400rpm, starting circulating water, and stirring for 60 minutes;
(2) adding the carbon nano tube conductive slurry into a stirring cylinder, stirring at 38rpm and 1750rpm, vacuumizing to-0.085 to-0.1 MPa, starting circulating water, and stirring for 180 minutes;
(3) adding residual NMP, stirring at 22rpm and 200rpm, starting circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 40 minutes.
Comparative example 2
A lithium ion battery anode mixing process comprises the following steps:
(1) adding lithium manganate, ternary lithium and PVDF into a stirring cylinder of a planetary stirrer, stirring at the speed of 30rpm and the dispersion speed of 400rpm, starting circulating water, and stirring for 50 minutes;
(2) stirring Super P, carbon nano tube conductive slurry and NMP accounting for 75% of the total weight of the solvent at 28rpm and 350rpm, starting circulating water, and stirring for 60 minutes;
(3) stirring at 38rpm, dispersing at 1750rpm, vacuumizing to-0.085 to-0.1 MPa, starting circulating water, and stirring for 150 minutes;
(4) adding residual NMP, stirring at 22rpm and 250rpm, circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 40 min.
Comparative example 3
A lithium ion battery anode mixing process comprises the following steps:
(1) adding PVDF and all NMP planetary mixers into a stirring cylinder, wherein the stirring speed is 30rpm, the dispersion speed is 1380rpm, starting circulating water, and stirring for 240 minutes;
(2) adding lithium manganate, ternary lithium manganate and Super P into a stirring cylinder, stirring at the speed of 35rpm and the dispersion speed of 1550rpm, starting circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 180 minutes;
(3) adding the carbon nano tube conductive slurry into a stirring cylinder, stirring at 38rpm and 1550rpm, vacuumizing to-0.085 to-0.1 MPa, starting circulating water, and stirring for 90 minutes;
(4) stirring speed 20rpm, dispersing speed 250rpm, opening circulating water, vacuumizing to-0.085 to-0.1 MPa, and stirring for 30 minutes.
The mixing time, the fineness of the slurry, the viscosity and the change in viscosity of examples 1 to 3 and comparative examples 1 to 3 were measured, and the results are shown in Table 1.
TABLE 1 mixing time and slurry Performance test results
As can be seen from Table 1, the slurries obtained in examples 1-3 of the present invention performed significantly better than those obtained in comparative examples 1-3.
According to the invention, the aggregate is sufficiently and effectively crushed by the shearing force formed by high-speed dispersion of the powdery material and high-viscosity slurry and high dispersion speed, so that micro-uniform mixing of particles is realized, and the obtained slurry has good fineness, high viscosity stability and short time consumption. Comparative examples 1-2 also used powdery materials and high-viscosity slurries for high-speed dispersion, but were inferior in terms of slurry fineness and slurry stability because of different feeding sequences. Comparative example 3 adopts the conventional wet mixing, and the glue preparation viscosity is low, the shearing force is not enough, and the dispersion effect is poor, so the stability of the slurry is poor, and simultaneously, the PVDF is slowly dissolved, and the whole batching consumes long time.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A dry mixing process for a lithium ion battery anode is characterized by comprising the following steps: the method comprises the following steps:
(1) adding an active substance and a powdery conductive agent into a stirring cylinder, stirring and mixing, wherein the stirring speed is 20-25 rpm, the dispersion speed is 1500-1800 rpm, and the stirring and mixing time is 10-20 minutes;
(2) adding the binder into a stirring cylinder, stirring and mixing at the stirring speed of 25-30 rpm and the dispersion speed of 1500-1800 rpm for 10-20 minutes;
(3) adding a solvent accounting for 50-85% of the total weight of the solvent into a stirring cylinder, stirring and mixing at a stirring speed of 25-30 rpm and a dispersion speed of 300-400 rpm for 30 minutes;
(4) adding a slurry-like conductive agent into a stirring cylinder, vacuumizing to-0.085 to-0.1 MPa, stirring and mixing at the stirring speed of 33 to 38rpm and the dispersion speed of 1500 to 1800rpm for 120 to 180 minutes;
(5) and adding the rest solvent, continuously vacuumizing to-0.085 to-0.1 MPa, stirring and mixing to obtain the lithium ion battery anode slurry, wherein the stirring speed is 20-25 rpm, the dispersion speed is 200-300 rpm, and the stirring and mixing time is 30-60 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110459410A (en) * | 2019-07-24 | 2019-11-15 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of super capacitor slurry and its supercapacitor prepared using super capacitor slurry |
| CN110416486B (en) * | 2019-07-25 | 2021-04-23 | 福建南平南孚电池有限公司 | Mixing method of positive electrode material of alkaline battery, positive electrode and alkaline battery |
| CN111933938B (en) * | 2020-06-29 | 2022-08-12 | 宁波新思创机电科技股份有限公司 | Preparation method of ternary cathode slurry |
| CN115050949B (en) * | 2022-08-11 | 2022-11-04 | 楚能新能源股份有限公司 | Positive electrode slurry, preparation method thereof and lithium ion battery |
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