CN112467086A - Preparation method of silicon-based negative electrode material based on polyamide-acid-based electrode binder - Google Patents

Preparation method of silicon-based negative electrode material based on polyamide-acid-based electrode binder Download PDF

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CN112467086A
CN112467086A CN202110065793.5A CN202110065793A CN112467086A CN 112467086 A CN112467086 A CN 112467086A CN 202110065793 A CN202110065793 A CN 202110065793A CN 112467086 A CN112467086 A CN 112467086A
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silicon
polyamic acid
binder
electrode binder
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刘耀东
张强
于毓秀
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Shanxi Institute of Coal Chemistry of CAS
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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
    • 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
    • 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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/027—Negative electrodes
    • 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 invention relates to a preparation method of a silicon-based negative electrode material based on a polyamide acid-based electrode binder, belongs to the technical field of secondary batteries, solves the technical problem that the binder is used for preparing the silicon negative electrode of the secondary battery, and adopts the following solution: firstly, polyamide acid copolymer binder modified by organic silicon, silicon-containing active material and conductive auxiliary agent are mixed according to the mass ratio of 5-20: 60-80: 5-20, adding the mixture into a solvent, and uniformly stirring the mixture for 30min-12h at room temperature to obtain paste slurry; then, the prepared slurry is applied to a current collector; and finally, drying the current collector coated with the slurry at the drying temperature of 60-80 ℃, and stamping and forming to obtain the silicon-based negative electrode after drying. The invention has low cost and easy operation, can effectively maintain the structural stability of the active material, and has higher specific cycling capacity and cycling stability.

Description

Preparation method of silicon-based negative electrode material based on polyamide-acid-based electrode binder
Technical Field
The invention belongs to the technical field of secondary batteries, and particularly relates to a preparation method of a silicon-based negative electrode material based on a polyamide-acid-based electrode binder.
Background
Secondary batteries are widely used in portable electronic products due to their high energy density and rate characteristics. With the gradual expansion of the application range to high energy storage fields such as electric vehicles, aerospace and the like, higher requirements are put forward for further improving the energy density and the safety and stability of the secondary battery.
For the current commercialized secondary battery, a graphite cathode with lower specific capacity is generally adopted, certain dendritic crystal phenomenon is easy to occur, and safety risk exists. Therefore, the use of silicon-based negative electrode materials with high capacity and high safety instead of carbon-based materials such as graphite is an important way to increase the energy density potential of secondary batteries.
However, silicon as the negative electrode material of the active material may generate large volume expansion and structural change during the ion intercalation/deintercalation process, thereby destroying the structural integrity of the electrode and reducing the cycle stability. Common methods for inhibiting volume change mostly adopt structural regulation or material modification and other modes with complex preparation process and higher cost. Therefore, the binder has wide structure selectivity and performance controllability, and becomes an important research direction for maintaining the structural integrity of the electrode and improving the electrochemical stability of the silicon cathode.
Polyamide-based polymers have been attracting attention as binders in recent years. Publication No. CN110959207A describes a silicon negative electrode composite binder of a blend of polymer binder mixed polyimide binders that can form high energy density batteries with good cycling performance. However, the component composition and proportion requirements of these binders are complex, the ability of inhibiting expansion and improving cycle stability are limited, and the study of carbon cathode materials is emphasized, and the functional requirements of silicon cathode materials on the binders cannot be well solved.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the technical problem that the binder is used for preparing the silicon cathode electrode of the secondary battery, the invention provides the preparation method of the silicon-based cathode material based on the polyamide-acid-based electrode binder, which has the advantages of low cost, easy operation, capability of effectively maintaining the structural stability of an active material and higher specific cycling capacity and cycling stability.
The invention is realized by the following technical scheme.
A preparation method of a silicon-based negative electrode material based on a polyamide-acid-based electrode binder comprises the following steps: firstly, polyamide acid copolymer binder modified by organic silicon, silicon-containing active material and conductive auxiliary agent are mixed according to the mass ratio of 5-20: 60-80: 5-20, adding the mixture into a solvent, and uniformly stirring the mixture for 30min-12h at room temperature to obtain paste slurry; then, the prepared slurry is applied to a current collector; and finally, drying the current collector coated with the slurry at the drying temperature of 60-80 ℃, and stamping and forming to obtain the silicon-based negative electrode after drying.
The polyamide acid copolymer modified by organic silicon is used as a binder of a silicon-based negative electrode of a secondary battery, and the secondary battery is preferably a lithium ion battery. Wherein the organosilicon can be one or more of silane coupling agent, ethyl orthosilicate and 3-aminopropyltriethoxysilane. The monomer of the polyamic acid copolymer can be one or more of polyamic acid, polyimide and polyamide-imide, and preferably polyamic acid. The active material in the silicon-based negative electrode comprises one or more of silicon, silicon oxide and a silicon-carbon composite material, and the size condition of the material can be set, wherein the size condition of the material comprises one or two of nanoscale silicon or micron-sized silicon, and the nanoscale silicon is preferred. The conductive auxiliary agent comprises one or more of Super P, Ketjen black and acetylene black.
Further, the solvent is N-methyl-2-pyrrolidone, water, dimethylformamide, dimethylacetamide, methylformamide or dimethylsulfoxide, preferably N-methyl-2-pyrrolidone.
Further, the current collector is a foil or a mesh of a conductive metal material, and the thickness of the current collector is 5 to 30 μm.
Further, the current collector is a foil or mesh of copper, aluminum, nickel, stainless steel, preferably a copper foil.
Further, the coating method is a doctor blade method, a coater method, a spray coating method or a combined method, and preferably a doctor blade method.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses the polyamic acid copolymer modified by organic silicon as a binder to prepare the slurry and the electrode of the silicon-based negative electrode of the secondary battery in a simple and easy operation mode. On one hand, the polyamic acid copolymer has excellent mechanical properties, and the high tensile strength of the polyamic acid copolymer can effectively limit the volume expansion of the silicon-based negative electrode in the charge and discharge processes. On the other hand, the polyamic acid modified by the organic silicon introduces a silicon-containing group or a siloxane chain segment, and hydroxyl and a silicon-oxygen bond widely exist to generate intermolecular interaction with the silicon-containing active material, so that the structural integrity and the volume stability of the active material in the embedding/removing process are enhanced, and the cycle stability is improved. Meanwhile, carbonyl, nitrogen hydrogen bond, aromatic carbon hydrogen bond and the like in the polyamic acid copolymer can form a physically cross-linked three-dimensional network structure, which is beneficial to ion transmission between the electrolyte and the active material, thereby improving the conductivity and the specific capacity of the electrode. Compared with widely used artificial binders such as polyvinylidene fluoride (PVDF), polyacrylic acid (PAA), Styrene Butadiene Rubber (SBR) and the like, the silicon-based negative electrode can more effectively inhibit the volume expansion of the silicon-based negative electrode and enhance the ion transmission, so that the silicon-based negative electrode with high specific capacity and high cycling stability is obtained. The materials selected by the invention are common chemical substances, the operation is simple, the cost is low, and the method is suitable for industrial production.
Drawings
FIG. 1 is a graph of the normal temperature cycling ratio capacity of the button cell prepared in example 3 and the button cell prepared in the comparative example.
Detailed Description
In order to further illustrate the present invention, the following examples are given in detail, without limiting the scope of the invention. Unless otherwise specified, the examples follow conventional experimental conditions. In addition, it will be apparent to those skilled in the art that various modifications or improvements can be made to the material components and amounts in these embodiments without departing from the spirit and scope of the invention as defined in the appended claims.
Example 1
In this embodiment 1, a preparation method of a silicon-based negative electrode material based on a polyamic acid-based electrode binder, which uses a polyamic acid copolymer modified by a silane coupling agent as a binder, specifically includes the following steps: weighing nano silicon powder, the silane coupling agent modified polyamic acid copolymer and Super P according to the weight ratio of 90:5:5, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Example 2
In this embodiment 2, a preparation method of a silicon-based negative electrode material based on a polyamic acid-based electrode binder, which uses a polyamic acid copolymer modified by a silane coupling agent as a binder, specifically includes the following steps: weighing nano silicon powder, the silane coupling agent modified polyamic acid copolymer and Super P according to the weight ratio of 80:10:10, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Example 3
In example 3, a silicon-based negative electrode material based on a polyamic acid-based electrode binder is prepared by using a polyamic acid copolymer modified by a silane coupling agent as a binderThe preparation method specifically comprises the following steps: weighing nano silicon powder, the silane coupling agent modified polyamic acid copolymer and Super P according to the weight ratio of 70:15:15, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Example 4
In this embodiment 4, a preparation method of a silicon-based negative electrode material based on a polyamic acid-based electrode binder, which uses a polyamic acid copolymer modified by a silane coupling agent as a binder, specifically includes the following steps: weighing nano silicon powder, the silane coupling agent modified polyamic acid copolymer and Super P according to the weight ratio of 70:15:15, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Example 5
In this embodiment 5, a method for preparing a silicon-based negative electrode material based on a polyamic acid-based electrode binder by using a polyamic acid copolymer modified with tetraethoxysilane as a binder includes the following steps: weighing nano silicon powder, tetraethoxysilane modified polyamic acid copolymer and Super P according to the weight ratio of 70:15:15, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Example 6
In example 6, 3-aminopropyltriethoxysilane modified polyamic acid copolymer is used as a binder, a silicon-based negative electrode binder based on polyamic acidThe preparation method of the pole material specifically comprises the following steps: weighing nano silicon powder, 3-aminopropyltriethoxysilane modified polyamide acid copolymer and Super P according to the weight ratio of 70:15:15, adding N-methyl-2-pyrrolidone, and stirring at room temperature for 30min to form uniform slurry. The slurry was coated onto a copper foil having a thickness of 5 μm using a doctor blade method, transferred to a vacuum drying oven, and dried at 70 ℃ for 12 hours. The obtained current collector was punched into a sheet to obtain an active material having a density of 1mg/cm3The electrode for a lithium battery of (1).
Comparative example 1
A general polyamic acid binder was used instead of the silicone-modified polyamic acid copolymer binder, and a paste and an electrode were prepared in the same manner as in example 3. Button cell type cell assembly was performed using the electrodes prepared in examples 1 to 6 and comparative example 1, respectively, comprising the steps of:
the button cell, which includes a negative electrode sheet, a separator, a lithium foil electrode, a current collector, and a support sheet, was assembled in a glove box filled with argon gas, and 1M LiPF was used6Ethylene Carbonate (EC)/diethyl carbonate (DEC) (volume ratio 1: 1)/fluoroethylene carbonate (FEC) (weight ratio 10%) as an electrolyte, and was encapsulated with a positive and negative electrode case to obtain a button cell.
The assembled button cell is used for constant current charge and discharge test, and the test conditions are as follows:
and connecting the battery with a charge and discharge tester at room temperature, wherein the potential window is 1.5V-0.01V, and performing cyclic charge and discharge test at a constant current of 0.5C. Capacity retention (%) = discharge capacity after N cycles ÷ discharge capacity at first time × 100.
The test performance results are as follows:
Figure 718853DEST_PATH_IMAGE002
the normal-temperature cycling specific capacity curve of the button cells prepared in the example 3 and the comparative example 1 is shown in figure 1.
As can be seen from the electrochemical performance test results of the button cells of examples 1-6 and comparative example 1, examples 1-6 exhibited excellent cycling stability and had higher specific capacities. The invention uses organic silicon modified polyamide acid copolymer as the adhesive of the silicon-based negative electrode of the secondary battery, compared with the common unmodified polyamide acid adhesive, the invention has better stability, better inhibits the volume expansion of the silicon-based active material in the charge-discharge cycle process, keeps the structure complete and further shows excellent electrochemical characteristics.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (10)

1. A preparation method of a silicon-based negative electrode material based on a polyamide-acid-based electrode binder is characterized by comprising the following steps: firstly, polyamide acid copolymer binder modified by organic silicon, silicon-containing active material and conductive auxiliary agent are mixed according to the mass ratio of 5-20: 60-80: 5-20, adding the mixture into a solvent, and uniformly stirring the mixture for 30min-12h at room temperature to obtain paste slurry; then, the prepared slurry is applied to a current collector; and finally, drying the current collector coated with the slurry at the drying temperature of 60-80 ℃, and stamping and forming to obtain the silicon-based negative electrode after drying.
2. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the organic silicon is one or more of silane coupling agent, ethyl orthosilicate or 3-aminopropyltriethoxysilane.
3. The method according to claim 1 for the preparation of a silicon-based anode material based on a polyamide acid based electrode binder, characterized in that: the monomer of the polyamic acid copolymer is one or more of polyamic acid, polyimide or polyamide-imide.
4. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the silicon-containing active material is one or more of silicon, silicon oxide or a silicon-carbon composite material.
5. The method for preparing a silicon-based anode material based on a polyamic acid-based electrode binder according to claim 4, wherein: the silicon-containing active material is one or two of nano-scale silicon or micron-scale silicon.
6. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the conductive additive is one or more of Super P, Ketjen black or acetylene black.
7. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the solvent is N-methyl-2-pyrrolidone, water, dimethylformamide, dimethylacetamide, methylformamide or dimethyl sulfoxide.
8. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the current collector is a foil or a mesh of a conductive metal material, and the thickness of the current collector is 5 to 30 μm.
9. The method of claim 8 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the current collector is a foil or mesh of copper, aluminum, nickel, stainless steel.
10. The method of claim 1 for preparing a silicon-based anode material based on a polyamic acid-based electrode binder, wherein: the coating mode is a doctor blade method, a coating machine, a spraying method or a combination method.
CN202110065793.5A 2020-09-07 2021-01-19 Preparation method of silicon-based negative electrode material based on polyamide-acid-based electrode binder Pending CN112467086A (en)

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Cited By (2)

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WO2022225381A1 (en) * 2021-04-22 2022-10-27 피아이첨단소재 주식회사 Polyamic acid composition

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CN113594429A (en) * 2021-06-02 2021-11-02 浙江中科玖源新材料有限公司 Polyamide acid modified nano-silicon negative electrode active material and preparation method thereof

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Application publication date: 20210309