CN112038583A - Preparation method for prelithiation of silicon monoxide negative pole piece - Google Patents
Preparation method for prelithiation of silicon monoxide negative pole piece Download PDFInfo
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- CN112038583A CN112038583A CN202010839411.5A CN202010839411A CN112038583A CN 112038583 A CN112038583 A CN 112038583A CN 202010839411 A CN202010839411 A CN 202010839411A CN 112038583 A CN112038583 A CN 112038583A
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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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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 invention discloses a preparation method for prelithiation of a silicon oxide negative electrode piece, which comprises the steps of dissolving methylnaphthalene in ethylene glycol dimethyl ether to prepare a methylnaphthalene solution, then putting a lithium piece into the solution, obtaining a methylnaphthalene lithium solution by utilizing the reaction of the methylnaphthalene and lithium, then soaking the prepared silicon oxide negative electrode piece into the methylnaphthalene lithium solution, reacting for a period of time, taking out the soaked electrode piece, and drying the electrode piece to obtain the prelithiated silicon oxide negative electrode piece. The method has the advantages of simple preparation process, low preparation cost and stable performance, can greatly improve the first efficiency of the silicon monoxide negative electrode material, and has wide application prospect.
Description
Technical Field
The invention relates to the field of lithium ion battery prelithiation, in particular to a preparation method for prelithiation of a silicon monoxide negative electrode piece.
Background
With social development and technological progress, the energy density requirements of lithium batteries in various fields are higher and higher. The theoretical specific capacity of the silicon oxide negative electrode material is 2680mAh/g, and meanwhile, the volume expansion of the silicon oxide negative electrode material is far less than that of silicon in the charging and discharging processes, and the cycle performance is better, so that the silicon oxide negative electrode material is widely concerned. However, since the silicon monoxide generates non-active substances such as lithium oxide and lithium silicate during the lithium intercalation process, the utilization rate of the electrolyte is low, and the first charge-discharge efficiency is also low. Therefore, the first time the efficiency of silica is improved is a major concern for researchers.
The prelithiation of the silicon-based material means that additional lithium element is added into the silicon oxide negative electrode material to supplement the lithium element lost in the lithium intercalation process, thereby achieving the purpose of improving the first efficiency.
The invention provides a simple prelithiation method for a silicon monoxide negative electrode material, which can greatly improve the first efficiency of the silicon monoxide negative electrode, has simple preparation process and low preparation cost, and is greatly helpful for further promoting the practical application of the silicon monoxide negative electrode.
Disclosure of Invention
The invention aims to provide a preparation method for prelithiation of a silicon oxide negative electrode material.
The purpose of the invention is realized by the following scheme: a preparation method for prelithiation of a silicon oxide negative pole piece is characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material, a conductive agent and a binder to obtain negative electrode slurry, coating the negative electrode slurry on copper foil, and drying to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and ethylene glycol dimethyl ether according to a molar ratio of (0.1-1): 1, mixing in proportion to obtain a solution A;
step three: putting the lithium sheet into the solution A for reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is (1-1.25): 1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the silicon oxide negative pole piece in the solution B for a period of time, taking out the silicon oxide negative pole piece, and drying the taken-out negative pole piece to obtain the pre-lithiated negative pole piece.
The silicon oxide negative electrode material coated by the carbon material in the first step is 0.5-90 wt% of coated carbon; the conductive agent in the first step is carbon black (SP) or acetylene black; the binder in the step one is one or more of polyacrylic acid (PAA), sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR).
The soaking time in the fourth step is 5-60 minutes.
The method has the advantages of simple preparation process, low preparation cost and stable performance, can greatly improve the first efficiency of the silicon oxide cathode material, and has wide application prospect.
Drawings
FIG. 1 is a first charge-discharge curve of the silicon oxide negative electrode material of the present invention.
Detailed Description
Example 1:
a prelithiation for a silicon monoxide negative pole piece is prepared by the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 5wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying at 80 ℃ to obtain a silicon oxide negative electrode piece;
step two: methylnaphthalene and ethylene glycol dimethyl ether are mixed according to a molar ratio of 1:1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 15 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
Fig. 1 is a graph showing the first charge and discharge curves of a half-cell (a button cell is adopted as the half-cell, a lithium sheet is used as a counter electrode, and a conventional lithium battery electrolyte) made of the pre-lithiated and non-pre-lithiated silicon oxide negative electrode material prepared in the embodiment. The first charge-discharge efficiency of the pre-lithiated silicon oxide negative electrode material prepared by the embodiment is 95%, which is much higher than the first efficiency of non-pre-lithiation by 76%.
Example 2:
a prelithiation for a silicon monoxide negative pole piece is prepared by the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 90wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode piece;
step two: methylnaphthalene and ethylene glycol dimethyl ether are mixed according to a molar ratio of 1:1, mixing in proportion to obtain a solution A;
step three: and putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1.1: 1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 10 minutes, taking out and drying to obtain a target product, namely the pre-lithiated negative pole piece.
Example 3:
a prelithiation for a silicon monoxide negative pole piece is prepared by the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 80wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and glycol dimethyl ether according to a molar ratio of 0.5: 1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 15 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
Example 4:
a prelithiation for a silicon monoxide negative pole piece is prepared by the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 15wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and glycol dimethyl ether according to a molar ratio of 0.5: 1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 20 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
Claims (7)
1. A preparation method for prelithiation of a silicon oxide negative pole piece is characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material, a conductive agent and a binder to obtain negative electrode slurry, coating the negative electrode slurry on copper foil, and drying to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and ethylene glycol dimethyl ether according to a molar ratio of (0.1-1): 1, mixing in proportion to obtain a solution A;
step three: putting the lithium sheet into the solution A for reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is (1-1.25): 1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the silicon oxide negative pole piece in the solution B for a period of time, taking out the silicon oxide negative pole piece, and drying the taken-out negative pole piece to obtain the pre-lithiated negative pole piece.
2. The method for preparing prelithiation of a negative pole piece of silicon oxide according to claim 1, wherein: the silicon oxide negative electrode material coated by the carbon material in the first step is 0.5-90 wt% of coated carbon; the conductive agent in the first step is carbon black (SP) or acetylene black; the binder in the step one is one or more of polyacrylic acid (PAA), sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR).
3. The method for preparing prelithiation of a negative pole piece of silicon oxide according to claim 1, wherein: and the soaking time in the fourth step is 5-60 minutes.
4. The preparation method for prelithiation of a negative electrode plate made of silicon oxide according to any of claims 1 to 3, characterized in that: the preparation method comprises the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 5wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying at 80 ℃ to obtain a silicon oxide negative electrode piece;
step two: methylnaphthalene and ethylene glycol dimethyl ether are mixed according to a molar ratio of 1:1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 15 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
5. The preparation method for prelithiation of a negative electrode plate made of silicon oxide according to any of claims 1 to 3, characterized in that: the preparation method comprises the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 90wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode piece;
step two: methylnaphthalene and ethylene glycol dimethyl ether are mixed according to a molar ratio of 1:1, mixing in proportion to obtain a solution A;
step three: and putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1.1: 1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 10 minutes, taking out and drying to obtain a target product, namely the pre-lithiated negative pole piece.
6. The preparation method for prelithiation of a negative electrode plate made of silicon oxide according to any of claims 1 to 3, characterized in that: the preparation method comprises the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 80wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and glycol dimethyl ether according to a molar ratio of 0.5: 1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 15 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
7. The preparation method for prelithiation of a negative electrode plate made of silicon oxide according to any of claims 1 to 3, characterized in that: the preparation method comprises the following steps:
the method comprises the following steps: uniformly mixing a silicon oxide negative electrode material with the carbon content of 15wt.%, a conductive agent and a binder (CMC and SBR) in a mass ratio of 8:1:1 to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, and drying in vacuum at 80 ℃ to obtain a silicon oxide negative electrode plate;
step two: mixing methylnaphthalene and glycol dimethyl ether according to a molar ratio of 0.5: 1, mixing in proportion to obtain a solution A;
step three: and (3) putting the lithium sheet into the solution A for full reaction, wherein the molar ratio of the lithium sheet to the methylnaphthalene is 1:1, obtaining methylnaphthalene lithium, and obtaining a solution B after the reaction is finished;
step four: and soaking the dried silicon monoxide negative pole piece in the solution B, standing for 20 minutes, taking out, and drying the taken-out pole piece to obtain a target product, namely the pre-lithiated negative pole piece.
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Cited By (6)
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| CN112563458A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Device for chemical prelithiation of aromatic hydrocarbons |
| CN112563454A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for pre-lithiation of negative pole piece |
| CN112886000A (en) * | 2021-01-05 | 2021-06-01 | 昆山宝创新能源科技有限公司 | Pre-lithiated silica negative electrode material and preparation method and application thereof |
| CN113594416A (en) * | 2021-07-19 | 2021-11-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for improving first coulombic efficiency of lithium ion battery silicon monoxide negative electrode pre-lithiation |
| CN113782734A (en) * | 2021-08-24 | 2021-12-10 | 南昌大学 | Preparation method of silicon monoxide negative pole piece |
| CN114242955A (en) * | 2022-01-11 | 2022-03-25 | 山东大学 | High-efficiency siloxene negative electrode material prepared by rapid chemical prelithiation and application thereof |
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Cited By (7)
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| CN112563458A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Device for chemical prelithiation of aromatic hydrocarbons |
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| CN113782734A (en) * | 2021-08-24 | 2021-12-10 | 南昌大学 | Preparation method of silicon monoxide negative pole piece |
| CN113782734B (en) * | 2021-08-24 | 2023-04-07 | 南昌大学 | Preparation method of silicon monoxide negative pole piece |
| CN114242955A (en) * | 2022-01-11 | 2022-03-25 | 山东大学 | High-efficiency siloxene negative electrode material prepared by rapid chemical prelithiation and application thereof |
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Application publication date: 20201204 |