CN112430833B - Metal lithium plating method used as reference electrode of three-electrode lithium ion battery - Google Patents

Metal lithium plating method used as reference electrode of three-electrode lithium ion battery Download PDF

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CN112430833B
CN112430833B CN201910791466.0A CN201910791466A CN112430833B CN 112430833 B CN112430833 B CN 112430833B CN 201910791466 A CN201910791466 A CN 201910791466A CN 112430833 B CN112430833 B CN 112430833B
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electrode
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CN112430833A (en
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赵星
李师
刘辉
李鹏
马留可
朱冰
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Zhengzhou Shenlan Power Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/045—Electrochemical coating; Electrochemical impregnation
    • H01M4/0452—Electrochemical coating; Electrochemical impregnation from solutions
    • 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
    • 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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Abstract

The invention relates to a metal lithium plating method used as a reference electrode of a three-electrode lithium ion battery, belonging to the field of three-electrode lithium ion batteries. The method comprises the following steps: the method comprises the following steps of taking a battery anode as a lithium-plated anode and a metal electrode as a lithium-plated cathode, firstly charging and plating lithium on the metal electrode, then discharging and dissolving lithium on the metal electrode, wherein the charging capacity of the charging and plating lithium is greater than the discharging capacity of the discharging and dissolving lithium; and sequentially and alternately carrying out lithium charging and electroplating and lithium discharging and lithium dissolving on the metal electrode until the preset total time of lithium charging and lithium discharging and lithium dissolving is reached. According to the method, the metal electrode is plated with lithium by using the alternating current pulse signal with charging and discharging as a cycle, so that a compact lithium layer is formed on the surface of the metal electrode, the electrochemical stability of the reference electrode is improved, and the accuracy of voltage monitoring is further improved.

Description

Metal lithium plating method used as reference electrode of three-electrode lithium ion battery
Technical Field
The invention belongs to the field of three-electrode lithium ion batteries, and particularly relates to a metal lithium plating method used as a reference electrode of a three-electrode lithium ion battery.
Background
Lithium ion batteries are widely applied in the fields of consumer electronics and power batteries, and three-electrode lithium ion batteries are important tools for researching working mechanisms such as anode and cathode matching, electrolyte applicability, battery failure analysis and the like. The three electrodes are not contacted with each other and are soaked in electrolyte together, and the existence of the reference electrode can monitor information such as voltage, impedance and the like between the electrodes in situ.
Chinese utility model patent with publication number CN206976495U discloses a three-electrode battery, including shell, positive pole, negative pole, diaphragm, electrolyte, reference electrode, nickel utmost point ear, the reference electrode is located between positive pole, the negative pole, and the diaphragm is located respectively between positive pole and the reference electrode, between reference electrode and the negative pole, wholly encapsulates in the shell, and the electrolyte is filled in the shell. One end of the reference electrode is a bare copper wire, and the reference electrode is completely arranged between the positive electrode and the negative electrode and is subjected to lithium plating treatment before testing. The existing lithium plating method is to plate lithium on a metal electrode under a constant current of 0.01-2mA, and the lithium plating time is 20-30 min. After the copper wire is plated with lithium by the lithium plating method, the voltage of the positive electrode and the negative electrode on the reference electrode can be accurately monitored within 1-3 times of battery cycle, but the phenomenon of inaccurate voltage monitoring can occur after more cycles, and the significance of the reference electrode is lost.
Disclosure of Invention
The invention aims to provide a metal lithium plating method used as a reference electrode of a three-electrode lithium ion battery, which aims to solve the problem that the existing method is easy to cause inaccurate voltage monitoring on the lithium plating of a metal electrode.
In order to achieve the purpose, the technical scheme adopted by the metal lithium plating method used as the reference electrode of the three-electrode lithium ion battery is as follows:
a lithium plating method of metal used as a reference electrode of a three-electrode lithium ion battery is characterized in that the lithium ion battery composed of a positive electrode, a negative electrode and a metal electrode is used for plating lithium on the metal electrode, the metal electrode is used as the reference electrode after being plated with lithium, and the metal electrode, the positive electrode and the negative electrode form the three-electrode lithium ion battery;
the lithium plating of the metal electrode comprises the following steps: the method comprises the following steps of taking a battery anode as a lithium-plated anode and a metal electrode as a lithium-plated cathode, firstly charging and plating lithium on the metal electrode, then discharging and dissolving lithium on the metal electrode, wherein the charging capacity of the charging and plating lithium is greater than the discharging capacity of the discharging and dissolving lithium; and sequentially and alternately carrying out lithium charging and electroplating and lithium discharging and lithium dissolving on the metal electrode until the preset total time of lithium charging and lithium discharging and lithium dissolving is reached.
The lithium layer formed by the existing direct current lithium plating method is not compact enough, and the stability of the reference electrode in the electrochemical reaction is reduced until the reference electrode fails along with the dissolution of metal lithium and the abrasion of the lithium layer on the reference electrode in the diaphragm caused by the expansion of the positive electrode and the negative electrode. According to the method for plating the lithium on the metal used as the reference electrode of the three-electrode lithium ion battery, the metal electrode is plated with the lithium by using the alternating current pulse signal with one cycle of charging and discharging, so that a compact lithium layer is formed on the surface of the metal electrode, the electrochemical stability of the reference electrode is improved, and the accuracy of voltage monitoring is further improved.
In order to further improve the accuracy of voltage monitoring, preferably, the method further comprises a negative electrode lithium plating process of using the battery negative electrode as a lithium plating positive electrode and using the metal electrode as a lithium plating negative electrode, wherein the negative electrode lithium plating process comprises the steps of firstly charging and plating lithium on the metal electrode and then discharging and dissolving lithium on the metal electrode, and the charging capacity of the charging and plating lithium is greater than the discharging capacity of the discharging and dissolving lithium; and sequentially and alternately carrying out lithium charging and electroplating and lithium discharging and lithium dissolving on the metal electrode until the preset total time of lithium charging and lithium discharging and lithium dissolving is reached. The negative electrode lithium plating process is further increased on the basis of the positive electrode lithium plating, so that a compact lithium layer can be generated on the negative electrode side of the metal electrode, the adaptability of the reference electrode under the condition of large-current discharge of the battery is improved, the concentration polarization phenomenon is reduced, and the electrochemical stability of the reference electrode is further improved.
In order to promote the formation of a compact and fine coating, preferably, the lithium plating process of taking the battery anode as a lithium plating anode and the metal electrode as a lithium plating cathode as an anode lithium plating process, wherein in the anode lithium plating process, the current for charging and lithium plating is 0.001-0.1mA, the time for charging and lithium plating is 1-30s, the current for discharging and lithium dissolving is 0.001-0.1mA, the time for discharging and lithium dissolving is 1-30s, and the charging capacity is 1-3 times of the discharging capacity; the total time of charging and plating lithium and discharging and dissolving lithium is 5-20 h. In order to further optimize the electrochemical stability of the plating layer, preferably, in the process of lithium plating of the positive electrode, constant current is adopted for both lithium charging plating and lithium discharging dissolving, the time for lithium charging plating is 10s, and the time for lithium discharging dissolving is 5 s.
In order to promote the formation of a compact and fine lithium layer on the negative electrode side of the metal electrode in the negative electrode lithium plating process, preferably, in the negative electrode lithium plating process, the current for charging lithium plating is 0.001-0.1mA, the time for charging lithium plating is 1-30s, the current for discharging lithium dissolving is 0.001-0.1mA, the time for discharging lithium dissolving is 1-30s, and the charging capacity is 1-3 times of the discharging capacity; the total time of charging and plating lithium and discharging and dissolving lithium is 5-20 h. In the process of positive electrode lithium plating and negative electrode lithium plating, the total time of charging lithium plating and discharging lithium dissolution is independently calculated, the total time and the total time can be flexibly determined within 5-20h, and the corresponding total time can be the same or different. In order to further optimize the electrochemical stability of the negative electrode lithium plating layer, preferably, in the negative electrode lithium plating process, constant current is adopted for both charging lithium plating and discharging lithium dissolution, the time for charging lithium plating is 10s, and the time for discharging lithium dissolution is 5 s.
In order to further optimize the battery state and improve the lithium plating quality of the negative electrode, preferably, at least one battery charge and discharge is performed before the negative electrode lithium plating process.
The selection of the metal substrate that can be used as a reference electrode refers to the related art, and in order to simplify the fabrication of the reference electrode, it is preferable that the reference electrode is a metal wire. The metal wire can be selected from gold wire, silver wire, copper wire, platinum wire and the like, and is preferably copper wire in view of raw material cost.
Drawings
FIG. 1 is a diagram of pulse charging current according to example 1 of the present invention;
FIG. 2 is a DC charging current diagram of comparative example 1;
FIG. 3 is a graph showing the charge monitoring at week 1 of the direct current single positive electrode lithium plating of comparative example 2;
FIG. 4 is a graph of the charge monitoring at week 3 of the direct current single positive electrode lithium plating of comparative example 2;
FIG. 5 is a graph showing the charge monitoring at week 1 in the case of AC single positive electrode lithium plating according to example 2 of the present invention;
FIG. 6 is a 17 th cycle charging monitoring chart of the AC single positive electrode lithium plating according to example 2 of the present invention;
FIG. 7 is a charge monitoring chart of comparative example 1 for week 1 of direct current positive and negative electrode lithium plating;
FIG. 8 is a 4 th week charge monitoring chart of the direct current positive and negative electrode lithium plating of comparative example 1;
FIG. 9 is a charging monitoring chart of the alternating current positive and negative electrode lithium plating of the 1 st week in accordance with embodiment 1 of the present invention;
fig. 10 is a 20 th week charging monitoring chart of ac positive and negative electrode lithium plating in example 1 of the present invention.
Detailed Description
The following examples are provided to further illustrate the practice of the invention. In the following examples, a lithium ion battery comprising a positive electrode, a negative electrode and a metal electrode can be assembled according to the prior art, for example, as disclosed in chinese utility model publication No. CN 206976495U. Specifically, the three-electrode lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm, electrolyte and a reference electrode, wherein the diaphragm is positioned between the positive electrode and the negative electrode; the reference electrode is prepared by removing a paint coat from one end of an enameled copper wire, and the end with the paint coat removed is immersed in the electrolyte and is isolated from the positive electrode and the negative electrode through a diaphragm. Taking a laminated battery as an example, after the diaphragm is stacked, placing one end of the reference electrode, from which the paint skin is removed, on the diaphragm, covering the exposed copper wire part of the reference electrode by using another diaphragm strip, and performing conventional procedures such as stacking, hot pressing and liquid injection of pole pieces to complete the assembly of the three-electrode lithium ion battery. For wound cells, reference is made to the above method for laminated cells to be prepared accordingly.
First, an embodiment of the method for plating lithium metal used as a reference electrode of a three-electrode lithium ion battery of the present invention
Example 1
The lithium plating method for the metal used as the reference electrode of the three-electrode lithium ion battery adopts the following steps: the positive electrode of the battery is used as the positive electrode, the copper wire is used as the negative electrode, the constant current of 0.005mA is used, the charging is carried out for 10s, the discharging is carried out for 5s, and the alternating current pulse signal of one cycle is used for plating lithium on the metal electrode for 18h (the positive electrode is plated with lithium); after the battery is charged and discharged for one time, the negative electrode of the battery is used as the positive electrode, the reference electrode is used as the negative electrode, the metal electrode is plated with lithium for 18h (negative electrode plating) by using an alternating current pulse signal with constant current of 0.005mA and charging for 10s and discharging for 5s as a cycle, and the manufacturing of the reference electrode is completed. In this embodiment, a pulsed charging current diagram is used as shown in fig. 1.
Example 2
The lithium plating method for the metal used as the reference electrode of the three-electrode lithium ion battery adopts the following steps: and (3) taking the positive electrode of the battery as the positive electrode and the copper wire as the negative electrode, and plating lithium on the metal electrode for 18h by using an alternating current pulse signal which is charged for 10s and discharged for 5s as a cycle by using a constant current of 0.005mA to finish the manufacture of the reference electrode.
Examples 3 to 8
The metal lithium plating method used as a reference electrode of a three-electrode lithium ion battery of examples 3 to 8 is different from the method of example 1 only in the difference of the process parameters of the positive electrode lithium plating process and the negative electrode lithium plating process, and the difference is listed in table 1.
TABLE 1 Process parameter differences for examples 3-8
Figure BDA0002179671520000041
Second, comparative example
Comparative example 1
The lithium plating method of the three-electrode lithium ion battery of comparative example 1 employs the following steps: the positive electrode of the battery is used as the positive electrode, the copper wire is used as the negative electrode, and the battery is charged by direct current for 8 hours by using constant current of 0.005 mA; after the battery is charged and discharged for one time, the negative electrode of the battery is taken as the positive electrode, the reference electrode is taken as the negative electrode, and the battery is charged for 8 hours by direct current with the constant current of 0.005mA, so that the manufacture of the reference electrode is completed. The dc charging current profile of the comparative example is shown in fig. 2.
Comparative example 2
The lithium plating method of the three-electrode lithium ion battery of comparative example 2 employs the following steps: the positive electrode of the battery is used as the positive electrode, the copper wire is used as the negative electrode, and the battery is charged by direct current for 8 hours by using constant current of 0.005 mA; and finishing the manufacture of the reference electrode.
Third, Experimental example
And (3) testing the battery for 20 weeks in a charging and discharging cycle, analyzing the positive and negative electrode voltages, the positive and reference electrode voltages and the negative and reference electrode voltages of the three-electrode lithium ion battery in the charging and discharging process by using a data acquisition instrument in the charging and discharging process, and inspecting the monitoring effect.
The charge monitoring graphs at week 1 and week 3 of the three-electrode lithium ion battery of comparative example 2 are shown in fig. 3 and 4. In the figure, the voltage monitoring of the positive electrode and the negative electrode of the battery is normal in the first week, but when the cycle is up to the 3 rd week, the voltage of the positive electrode and the voltage of the reference electrode are smaller than the voltage of the positive electrode and the negative electrode of the battery, and the voltage of the negative electrode and the voltage of the reference electrode are smaller than 0.
The charge monitoring graphs for week 1 and week 17 of the three-electrode lithium ion battery of example 2 are shown in fig. 5 and 6. The monitoring of the voltage of the positive electrode and the negative electrode in the first week is normal, and the reference electrode has unstable monitoring when the monitoring is circulated to the 17 th week, so that the monitoring of the voltage of the positive electrode and the voltage of the negative electrode is abnormal for a period of time.
The charge monitoring graphs at week 1 and week 4 of the three-electrode lithium ion battery of comparative example 1 are shown in fig. 7 and 8. In the figure, the voltage monitoring of the positive electrode and the negative electrode of the battery is normal in the first week, but when the voltage monitoring is circulated to the 4 th week, the voltage curves of the positive electrode and the reference electrode are intersected with the voltage curves of the positive electrode and the negative electrode of the battery, and the voltage of the negative electrode and the reference electrode is less than 0, so that the normal operation working condition of the battery is not consistent, and the problem of the reference electrode is explained, and the voltage monitoring of the positive electrode and the negative electrode is abnormal at the same time.
The charge monitoring graphs at week 1 and week 20 of the three-electrode lithium ion battery of example 1 are shown in fig. 9 and 10. In the figure, when the cycle is 20 weeks, the voltage monitoring of the positive electrode and the negative electrode is still accurate, the reference effect of the reference electrode is still stable, the more excellent performance is displayed, and the electrochemical analysis in the cycle process of the lithium ion battery can be better supported.

Claims (8)

1. A metal lithium plating method used as a reference electrode of a three-electrode lithium ion battery is characterized in that the lithium ion battery composed of a positive electrode, a negative electrode and a metal electrode is used for plating lithium on the metal electrode, the metal electrode is used as the reference electrode after being plated with lithium, and the metal electrode, the positive electrode and the negative electrode form the three-electrode lithium ion battery;
the lithium plating of the metal electrode comprises the following steps: the method comprises the following steps of taking a battery anode as a lithium-plated anode and a metal electrode as a lithium-plated cathode, firstly charging and plating lithium on the metal electrode, then discharging and dissolving lithium on the metal electrode, wherein the charging capacity of the charging and plating lithium is greater than the discharging capacity of the discharging and dissolving lithium; sequentially and alternately carrying out lithium charging and electroplating and lithium discharging and lithium dissolving on the metal electrode until the preset total time of the lithium charging and electroplating and the lithium discharging and lithium dissolving is reached;
the method also comprises a negative electrode lithium plating process of taking the battery negative electrode as a lithium plating positive electrode and taking the metal electrode as a lithium plating negative electrode, wherein the negative electrode lithium plating process comprises the steps of firstly charging and plating lithium on the metal electrode, then discharging and dissolving lithium on the metal electrode, and the charging capacity of the charging and plating lithium is greater than the discharging capacity of the discharging and dissolving lithium; and sequentially and alternately carrying out lithium charging and electroplating and lithium discharging and lithium dissolving on the metal electrode until the preset total time of lithium charging and lithium discharging and lithium dissolving is reached.
2. The method of claim 1, wherein the lithium plating process using the battery anode as a lithium plating anode and the metal electrode as a lithium plating cathode is a lithium plating anode plating process, and the current for charging and lithium plating is 0.001-0.1mA, the time for charging and lithium plating is 1-30s, the current for discharging and lithium dissolving is 0.001-0.1mA, the time for discharging and lithium dissolving is 1-30s, and the charging capacity is 1-3 times of the discharging capacity; the total time of charging and plating lithium and discharging and dissolving lithium is 5-20 h.
3. The method for plating lithium on a metal used as a reference electrode of a three-electrode lithium ion battery according to claim 2, wherein during the lithium plating of the positive electrode, constant current is adopted for both lithium charging and lithium discharging, the lithium charging and plating time is 10s, and the lithium discharging and dissolving time is 5 s.
4. The method for plating lithium with metal as a reference electrode of a three-electrode lithium ion battery according to claim 1, wherein during the lithium plating of the negative electrode, the current for charging and lithium plating is 0.001-0.1mA, the time for charging and lithium plating is 1-30s, the current for discharging and lithium dissolving is 0.001-0.1mA, the time for discharging and lithium dissolving is 1-30s, and the charging capacity is 1-3 times the discharging capacity; the total time of charging and plating lithium and discharging and dissolving lithium is 5-20 h.
5. The method for plating lithium on a metal used as a reference electrode of a three-electrode lithium ion battery according to claim 4, wherein during the lithium plating on the negative electrode, constant current is adopted for both lithium charging and lithium discharging, the lithium charging and plating time is 10s, and the lithium discharging and dissolving time is 5 s.
6. The method of lithium metal plating as a reference electrode for a three-electrode lithium ion battery according to claim 1, 4 or 5, wherein at least one battery charge and discharge is performed before the negative electrode lithium plating process is performed.
7. The method of any of claims 1-5, wherein the metal electrode is a wire.
8. The method of claim 7, wherein the metal wire is a copper wire.
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