CN110988708A - Preparation method of reference electrode device for detecting lithium separation of lithium ion battery - Google Patents
Preparation method of reference electrode device for detecting lithium separation of lithium ion battery Download PDFInfo
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- CN110988708A CN110988708A CN201911314781.0A CN201911314781A CN110988708A CN 110988708 A CN110988708 A CN 110988708A CN 201911314781 A CN201911314781 A CN 201911314781A CN 110988708 A CN110988708 A CN 110988708A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/382—Arrangements for monitoring battery or accumulator variables, e.g. SoC
- G01R31/3835—Arrangements for monitoring battery or accumulator variables, e.g. SoC involving only voltage measurements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R3/00—Apparatus or processes specially adapted for the manufacture or maintenance of measuring instruments, e.g. of probe tips
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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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- 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 belongs to the technical field of safety monitoring of lithium ion batteries, and particularly relates to a preparation method of a reference electrode device for detecting lithium separation of a lithium ion battery, which comprises the following steps: soaking copper metal in an electrolyte aqueous solution for surface treatment; coating the copper metal subjected to surface treatment by adopting a melting method or an ultrathin lithium sheet winding method; the copper metal coated with the metal lithium is placed in a solution containing a high molecular monomer and an initiator for soaking; and taking out the copper metal after adsorption treatment, and allowing the macromolecular monomer adsorbed on the surface of the lithium to polymerize spontaneously. The use of the reference electrode obviously inhibits the thermodynamic instability of the lithium reference electrode and the electrolyte in the practical battery system, reduces the contact between the electrolyte and the reference electrode, ensures the ion exchange of lithium ions at the electrode, obviously prolongs the service life of the reference electrode, and has good application prospect in the research of accurately monitoring lithium separation of the lithium ion battery.
Description
Technical Field
The invention belongs to the technical field of safety monitoring of lithium ion batteries, and particularly relates to a preparation method of a reference electrode device for detecting lithium separation of a lithium ion battery.
Background
The complete battery is mainly composed of a positive electrode material, a negative electrode material and electrode solution, however, the battery body is a complex system, and researchers cannot respectively obtain the electrode potentials of the positive electrode and the negative electrode from the two electrode materials because the potential of the electrode is easily influenced by factors such as current density, uniformity of an electric field on the surface of the electrode, ion concentration on the surface of the electrode and the like. Therefore, the introduction of the reference electrode is an important research topic for accurately monitoring the potentials of the positive electrode and the negative electrode. In an aqueous system, researchers usually use an ideal polarized electrode (such as a silver/silver chloride electrode, a saturated calomel electrode, etc.) as a reference electrode to calibrate the potential of a working electrode; in organic systems, a stable reference electrode has not been successfully developed, and a lithium metal wire or a lithium metal strip is used as a common reference electrode in electrode potential tests in current researches.
In the existing research reports, a metallic lithium strip is used as a reference electrode in an electrolytic cell to monitor the oxidation-reduction potential of solvent molecules or lithium salt in an electrolyte on the surface of a working electrode; in a pouch battery, a metal wire or a lithium-plated metal wire is often used as a reference electrode (patent document 1; patent document 2). However, the bare reference electrode is easy to be thermodynamically corroded in the electrolyte, so that the standard potential of the reference electrode is changed, and the existence of the reference electrode loses the meaning of the reference electrode. Therefore, it becomes very important to construct a reference electrode with stable surface chemical properties and difficult corrosion by electrolyte and micro-current, and the design of the stable reference electrode plays an important role in the fields of battery safety, accurate control and monitoring of electrode potential, research on lithium precipitation behaviors on the surface of the electrode and the like.
Documents of the prior art
Patent document
Patent document 1: CN 107293778A
Patent document 2: CN 204130649U
Disclosure of Invention
Technical problem to be solved by the invention
The invention aims to provide a preparation method of a reference electrode device for detecting lithium evolution of a lithium ion battery. The prepared reference electrode can be effectively used as the reference of the electrode potential, and provides a relatively stable reference potential for monitoring the potential change of the two electrodes of the full cell. The use of the reference electrode obviously inhibits the thermodynamic instability of the lithium reference electrode and the electrolyte in the practical battery system, reduces the contact between the electrolyte and the reference electrode, ensures the ion exchange of lithium ions at the electrode, obviously prolongs the service life of the reference electrode, and has good application prospect in the research of accurately monitoring lithium separation of the lithium ion battery.
Means for solving the technical problem
In order to solve the above problems, the present invention provides a method for preparing a reference electrode, wherein the method comprises: soaking copper metal in an electrolyte aqueous solution for surface treatment; coating the copper metal subjected to surface treatment by adopting a melting method or an ultrathin lithium sheet winding method; the copper metal coated with the metal lithium is placed in a solution containing a high molecular monomer and an initiator for soaking; and taking out the copper metal after adsorption treatment, and allowing the macromolecular monomer adsorbed on the surface of the lithium to polymerize spontaneously.
One embodiment is that the electrolyte is one or more of dilute hydrochloric acid, dilute sulfuric acid, dilute nitric acid, silver nitrate and chloroauric acid, the concentration of the electrolyte is 0.01-1.0 mol/L, and the solvent is water.
One embodiment is that the melting method is to immerse the treated copper metal in liquid lithium at a melting state of 170-500 ℃; the ultrathin lithium winding and coating method is to wind a lithium belt with the thickness of 2-100 mu m on the surface of the treated copper metal in a seamless manner.
In one embodiment, the polymer monomer is one or more of ethylene oxide, acrylonitrile, vinyl chloride, methyl methacrylate, ethylene glycol phenyl ether acrylate, ethylene glycol phenyl ether methacrylate and ethylene glycol phenyl ether, and the initiator is azobisisobutyronitrile.
In one embodiment, the mass fraction is 0.1 wt% of the total mass of the solution, and the soaking time is 1-60 s.
According to a second aspect of the invention, there is provided a reference electrode prepared according to the method of the invention.
According to a third aspect of the invention, an application of the reference electrode in monitoring lithium evolution of the lithium ion battery is provided, wherein the reference electrode is suitable for all-battery types which take graphite as a negative electrode and take lithium iron phosphate, lithium cobaltate, nickel-cobalt-manganese ternary, nickel-cobalt-aluminum ternary, lithium-rich manganese base, quinones and the like as a positive electrode.
The invention has the advantages of
Compared with the prior art, the preparation method has the advantages that the equipment required in the whole preparation process is simple, the experimental reproducibility is good, and the designability is strong; the thickness of the prepared lithium metal layer and the thickness of the high polymer layer are controllable; the reference electrode system has stable thermodynamic property in ester and ether electrolytes, can obviously inhibit the corrosion of the reference electrode in the use process of the battery, prolongs the service life of the battery, and accurately monitors the lithium evolution potential of the lithium ion battery.
Further features of the present invention will become apparent from the following description of exemplary embodiments.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the present invention.
FIG. 2 is a graph of electrode potentials for positive and negative polarity measurements using a reference electrode.
Detailed Description
One embodiment of the present disclosure will be specifically described below, but the present disclosure is not limited thereto.
The invention provides a preparation method of a reference electrode device for detecting lithium separation of a lithium ion battery, which is characterized in that the surface of copper metal (copper wire can be used) is soaked in an aqueous solution containing electrolyte with the concentration of 0.01-1.0 mol/L for treatment; taking out the copper wire, drying, and coating the dried copper wire by adopting a melting method or an ultrathin lithium sheet winding method; placing the copper wire coated with the metal lithium in a solution containing a high-molecular monomer and an initiator to be soaked for 1-60 s; and taking out the electrode and allowing the macromolecular monomer adsorbed on the lithium surface to spontaneously polymerize.
Examples
The present invention is described in more detail by way of examples, but the present invention is not limited to the following examples.
Example 1: soaking a copper wire in a 1.0mol/L dilute hydrochloric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a melting state of 170 ℃ for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene oxide monomer polymer solution with azodiisobutyronitrile as an initiator for 10s, and removing the electrode to allow the polymer to polymerize spontaneously to obtain the reference electrode.
Example 2: soaking the copper wire in 0.01mol/L dilute nitric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a melting state of 250 ℃ for surface coating; and (3) soaking the copper wire coated with the lithium layer in 0.1 wt% of acrylonitrile monomer polymer solution with azodiisobutyronitrile as an initiator for 1s, and removing the electrode to allow the polymer to spontaneously polymerize to obtain the reference electrode.
Example 3: soaking the copper wire in 0.1mol/L silver nitrate solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium in a 320-degree molten state for surface coating; and soaking the copper wire coated with the lithium layer in a vinyl chloride monomer high polymer solution with 0.1 wt% of azodiisobutyronitrile as an initiator for 60s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 4: soaking a copper wire in a 0.2mol/L chloroauric acid solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a lithium tape with the thickness of 2 mu m; and (3) soaking the copper wire coated with the lithium layer in 0.1 wt% of methyl methacrylate monomer polymer solution with azodiisobutyronitrile as an initiator for 10s, and removing the electrode to allow the polymer to polymerize spontaneously to obtain the reference electrode.
A potential test of a commercial lithium ion full cell using the reference electrode prepared in example 4 is shown in fig. 2, which shows that the potentials of the positive and negative electrodes detected by the reference electrode are still not shifted after 100 hours of continuous testing.
Example 5: soaking the copper wire in 0.3mol/L dilute hydrochloric acid solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a lithium tape with the thickness of 100 mu m; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether acrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 20s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 6: soaking the copper wire in 0.4mol/L dilute nitric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a melting state of 450 ℃ for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether methacrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 30s, and removing the electrode to allow high polymers to spontaneously polymerize to obtain the reference electrode.
Example 7: soaking the copper wire in 0.5mol/L silver nitrate solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a melting state of 500 ℃ for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether monomer high polymer solution with azodiisobutyronitrile as an initiator for 10s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 8: soaking the copper wire in 0.6mol/L dilute sulfuric acid solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a 33 mu m thick lithium tape; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene oxide monomer polymer solution with azodiisobutyronitrile as an initiator for 15s, and removing the electrode to allow the polymer to polymerize spontaneously to obtain the reference electrode.
Example 9: soaking the copper wire in 0.7mol/L silver nitrate solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a lithium tape with the thickness of 20 mu m; and (3) soaking the copper wire coated with the lithium layer in a vinyl chloride monomer high polymer solution with 0.1 wt% of azobisisobutyronitrile as an initiator for 35s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 10: soaking the copper wire in 0.8mol/L chloroauric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium in a 400-degree molten state for surface coating; and soaking the copper wire coated with the lithium layer in an acrylonitrile monomer high polymer solution with 0.1 wt% of azodiisobutyronitrile as an initiator for 50s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 11: soaking the copper wire in 0.1mol/L dilute hydrochloric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a 220-degree molten state for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether acrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 10s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 12: soaking a copper wire in 0.04mol/L dilute sulfuric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a melting state of 300 ℃ for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether methacrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 60s, and removing the electrode to allow high polymers to spontaneously polymerize to obtain the reference electrode.
Example 13: soaking the copper wire in 0.08mol/L dilute nitric acid solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a lithium tape with the thickness of 40 mu m; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether monomer high polymer solution with azodiisobutyronitrile as an initiator for 10s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 14: soaking the copper wire in 0.03mol/L silver nitrate solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a 350-degree molten state for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene oxide monomer polymer solution with azodiisobutyronitrile as an initiator for 5s, and removing the electrode to allow the polymer to polymerize spontaneously to obtain the reference electrode.
Example 15: soaking a copper wire in a 0.3mol/L chloroauric acid solution, taking out the copper wire and drying; placing the dried copper wire in liquid lithium at a 270-degree molten state for surface coating; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether acrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 30s, and removing the electrode to allow the high polymer to spontaneously polymerize to obtain the reference electrode.
Example 16: soaking the copper wire in 0.5mol/L dilute hydrochloric acid solution, taking out the copper wire and drying; winding and coating the dried copper wire by using a lithium belt with the thickness of 80 mu m; and soaking the copper wire coated with the lithium layer in 0.1 wt% of ethylene glycol phenyl ether methacrylate monomer high polymer solution with azodiisobutyronitrile as an initiator for 15s, and removing the electrode to allow high polymers to spontaneously polymerize to obtain the reference electrode.
Industrial applicability
The use of the reference electrode obviously inhibits the thermodynamic instability of the lithium reference electrode and the electrolyte in the practical battery system, reduces the contact between the electrolyte and the reference electrode, ensures the ion exchange of lithium ions at the electrode, obviously prolongs the service life of the reference electrode, and is suitable for accurately monitoring the lithium precipitation of the lithium ion battery.
The present invention is not limited to the above embodiments, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A method of making a reference electrode, comprising: soaking copper metal in an electrolyte aqueous solution for surface treatment; coating the copper metal subjected to surface treatment by adopting a melting method or an ultrathin lithium sheet winding method; the copper metal coated with the metal lithium is placed in a solution containing a high molecular monomer and an initiator for soaking; and taking out the copper metal after adsorption treatment, and allowing the macromolecular monomer adsorbed on the surface of the lithium to polymerize spontaneously.
2. The method according to claim 1, wherein the electrolyte is one or more of dilute hydrochloric acid, dilute sulfuric acid, dilute nitric acid, silver nitrate and chloroauric acid, the concentration of the electrolyte is 0.01-1.0 mol/L, and the solvent is water.
3. The method according to claim 1, wherein the melting method is to immerse the treated copper metal in liquid lithium in a molten state at 170-500 ℃; the ultrathin lithium winding and coating method is to wind a lithium belt with the thickness of 2-100 mu m on the surface of the treated copper metal in a seamless manner.
4. The method according to claim 1, wherein the polymer monomer is one or more of ethylene oxide, acrylonitrile, vinyl chloride, methyl methacrylate, ethylene glycol phenyl ether acrylate, ethylene glycol phenyl ether methacrylate and ethylene glycol phenyl ether, and the initiator is azobisisobutyronitrile.
5. The method according to claim 4, wherein the mass fraction is 0.1 wt% of the total mass of the solution, and the soaking time is 1 to 60 s.
6. A reference electrode prepared according to the method of any one of claims 1 to 5.
7. The use of the reference electrode according to claim 6 for monitoring lithium evolution in lithium ion batteries, wherein the reference electrode is suitable for all-battery types with graphite as the negative electrode and lithium iron phosphate, lithium cobaltate, nickel cobalt manganese ternary, nickel cobalt aluminum ternary, lithium manganese rich base, quinones and the like as the positive electrode.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111969172A (en) * | 2020-07-30 | 2020-11-20 | 北京理工大学 | Air-stable long-acting reference electrode suitable for lithium battery |
| CN112054162A (en) * | 2020-09-16 | 2020-12-08 | 北京理工大学 | Packaging method of metal lithium reference electrode for lithium battery |
| CN112240983A (en) * | 2020-09-22 | 2021-01-19 | 清华大学 | Method and device for detecting lithium separation of battery |
| CN113793920A (en) * | 2021-08-09 | 2021-12-14 | 华中科技大学 | Construction method and application of in-situ lithium-aluminum alloy layer on surface of metal lithium |
| WO2023151335A1 (en) * | 2022-02-10 | 2023-08-17 | 中国第一汽车股份有限公司 | Lithium ion battery reference electrode and preparation method therefor and use thereof |
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