CN115575827A - Lithium battery in-situ force electrochemical performance testing device and method - Google Patents

Lithium battery in-situ force electrochemical performance testing device and method Download PDF

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Publication number
CN115575827A
CN115575827A CN202211381778.2A CN202211381778A CN115575827A CN 115575827 A CN115575827 A CN 115575827A CN 202211381778 A CN202211381778 A CN 202211381778A CN 115575827 A CN115575827 A CN 115575827A
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electrode
electrochemical
electrochemical cell
lithium battery
working electrode
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谢科予
沈超
赵耀华
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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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]
    • G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
    • G01R31/38—Primary cells, i.e. not rechargeable
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • 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]
    • G01R31/3644—Constructional arrangements
    • 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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  • General Physics & Mathematics (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Molecular Biology (AREA)
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Abstract

The invention provides a device and a method for testing in-situ power electrochemical performance of a lithium battery, which belong to the technical field of battery performance testing and comprise the following steps: the electrochemical cell is characterized in that a cavity of the electrochemical cell is filled with electrolyte; the reference electrode is arranged on one side of the inner wall of the cavity of the electrochemical cell; the counter electrode is arranged on the other side of the inner wall of the cavity of the electrochemical cell; the electrode clamp is arranged on the bottom wall of the cavity of the electrochemical cell, and a working electrode is clamped on the electrode clamp; the external electrode is arranged on the outer wall of the electrochemical cell and is used for connecting an external electrochemical analysis device; the reference electrode, the counter electrode and the working electrode are all connected with an external electrode through leads. The invention can realize the in-situ force electrochemical performance test of the lithium battery electrode, obtain the dynamic mechanical response characteristic of the electrode in the electrochemical reaction process, and research the real-time change rule of the lithium battery electrode under different working conditions.

Description

Lithium battery in-situ force electrochemical performance testing device and method
Technical Field
The invention belongs to the technical field of battery performance testing, particularly relates to a device and a method for testing in-situ mechanical and electrochemical performance of a lithium battery, and particularly relates to a device and a method for testing electrochemical testing and synchronous in-situ nano indentation testing of a lithium battery electrode.
Background
The lithium battery has the remarkable advantages of high energy density, good rate capability, long cycle life, strong environmental adaptability and the like, and is widely and deeply applied to various fields such as electronic products, electric tools, new energy automobiles and the like. The lithium battery is used as an energy storage and conversion integrated device and relates to the coupling influence of multiple factors such as a mechanical structure, an electrochemical reaction, temperature and the like, wherein in the charging and discharging process of the lithium battery, repeated expansion and contraction of an active material are caused by repeated de-intercalation of lithium ions, so that structural deformation of the active material and extrusion and stretching of adjacent components are caused, and further the mechanical property of a pole piece is changed in the electrochemical reaction process. And mechanical phenomena such as pole piece deformation and cracking often cause electrochemical reaction failure, so that the lithium battery operation fault is caused, and therefore, the characterization test of the mechanical properties of the lithium battery under different electrochemical conditions is facilitated, the failure mechanism of the lithium battery is further analyzed, and the lithium battery which is long-lasting and operates efficiently is constructed.
The electrochemical reaction of the lithium battery relates to the phenomena of SEI film formation, active substance denaturation and the like, and is particularly sensitive to moisture, oxygen concentration and the like in the environment, so that most in-situ lithium battery testing devices are sealing systems. However, most of the existing material mechanical property tests are open systems, and the tested material is required to have certain environmental adaptability. Therefore, most of the conventional lithium battery mechanical property test methods are characterized ex-situ, the lithium battery is disassembled after a certain degree of electrochemical reaction, and the mechanical property test is performed after substances such as active materials and the like are reprocessed, so that the obtained rule is distorted to a certain degree.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a device and a method for testing the in-situ electrochemical performance of a lithium battery. The device and the method can synchronously carry out in-situ mechanical property test on the lithium battery electrode under the condition that the lithium battery carries out different electrochemical reactions so as to obtain the force electrochemical coupling rule of the lithium battery.
In order to achieve the above purpose, the invention provides the following technical scheme:
a lithium battery in-situ force electrochemical performance testing device comprises:
the electrochemical cell is characterized in that a cavity of the electrochemical cell is filled with electrolyte;
the reference electrode is arranged on one side of the inner wall of the cavity of the electrochemical cell;
the counter electrode is arranged on the other side of the inner wall of the cavity of the electrochemical cell;
the electrode clamp is arranged on the bottom wall of the cavity of the electrochemical cell, and a working electrode is clamped on the electrode clamp;
the external electrode is arranged on the outer wall of the electrochemical cell and is used for being connected with an external electrochemical analysis device;
the reference electrode, the counter electrode and the working electrode are all connected with the external electrode through leads;
and during testing, the testing device is arranged below a pressure head of the nanoindentation tester.
Preferably, the electrode clamp comprises a conductive connecting piece arranged on the bottom wall of the cavity of the electrochemical cell and a fixing piece arranged on the conductive connecting piece, the working electrode is arranged on the conductive connecting piece and positioned inside the fixing piece, and the working electrode is connected with the external electrode through the conductive connecting piece.
Preferably, the fixing part comprises clamping plates arranged on the periphery of the conductive connecting part, and the clamping plates are connected with the conductive connecting part through return springs.
Preferably, the fixing member material is an insulating material.
Preferably, the lead is buried within the cell body of the electrochemical cell.
Preferably, the material of the electrochemical cell is polytetrafluoroethylene.
Preferably, the electrolyte is lithium hexafluorophosphate.
Based on the same inventive concept, another object of the present invention is to provide a method for testing in-situ electrochemical performance of a lithium battery, comprising the following steps:
loading a working electrode on the conductive connecting piece, and clamping the working electrode through the fixing piece;
fixing the electrochemical cell on an objective table of a nanoindentation tester,
connecting the external electrode to an external electrochemical analysis device;
injecting electrolyte into the cavity of the electrochemical cell, wherein the working electrode, the reference electrode and the counter electrode are all positioned in the electrolyte;
marking the region to be detected of the working electrode by using an optical mirror of the nanoindentation tester;
based on the Oliver-Pharr method, pressing down the target area marked on the working electrode by using a pressure head of a nanoindentation tester and generating a scratch;
the pressure head of the nano indentation tester sends the data collected in the pressing process to a host of the nano indentation tester for analysis, and the mechanical property of the working electrode in the electrochemical reaction process is obtained;
the reference electrode and the counter electrode send the acquired data to an external electrochemical analysis device, and the data are analyzed by the external electrochemical analysis device to obtain the electrochemical performance of the working electrode in the electrochemical reaction process.
Preferably, during testing, the pressure head of the nanoindentation tester sends the acquired data to a host of the nanoindentation tester for analysis, indentation geometric parameters and a load-displacement curve of the working electrode in the electrochemical reaction process are obtained, and the mechanical property of the working electrode is obtained through the indentation geometric parameters and the load-displacement curve.
Preferably, during testing, the electrochemical cell and the matched nanoindentation tester are placed in a glove box filled with argon, and the oxygen concentration of water in the glove box is lower than 0.1mg L -1 。
The device and the method for testing the in-situ mechanical and electrochemical performance of the lithium battery have the following beneficial effects:
the device is different from the distortion characteristic of ex-situ test, the in-situ chemical performance test of the working electrode can be realized through the reference electrode and the counter electrode, the in-situ force electrochemical performance test of the working electrode can be realized through the nanoindentation tester, the dynamic mechanical response characteristic of the working electrode in the electrochemical reaction process is obtained, the real-time change rule of the working electrode under different working conditions is researched, and meanwhile, the device can be matched with more characterization means to carry out combined synchronous test.
Drawings
In order to more clearly illustrate the embodiments of the present invention and the design thereof, the drawings required for the embodiments will be briefly described below. The drawings in the following description are only some embodiments of the invention and it will be clear to a person skilled in the art that other drawings can be derived from them without inventive effort.
Fig. 1 is a front view of a lithium battery in-situ mechanical-electrochemical performance testing device in embodiment 1 of the present invention;
fig. 2 is a top view of a lithium battery in-situ mechanical-electrochemical performance testing apparatus according to embodiment 1 of the present invention;
FIG. 3 is a flow chart of a lithium battery in-situ electrochemical performance testing method provided by the invention;
description of the reference numerals: 1-an electrochemical cell, 2-a reference electrode, 3-a counter electrode, 4-a fixing piece, 5-a conductive connecting piece, 6-a lead, 7-an external electrode, 8-a working electrode, 9-a pressure head and 10-electrolyte.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention and can practice the same, the present invention will be described in detail with reference to the accompanying drawings and specific examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing technical solutions of the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the present invention, it should be noted that, unless explicitly stated or limited otherwise, the terms "connected" and "connected" are to be interpreted broadly, and may be, for example, a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art. In the description of the present invention, unless otherwise specified, "a plurality" means two or more, and will not be described in detail herein.
Example 1
The invention provides a device and a method for testing in-situ mechanical and electrochemical properties of a lithium battery, and particularly relates to a device and a method shown in figures 1 and 2, wherein the device comprises an electrochemical cell 1, a reference electrode 2, a counter electrode 3, an external electrode 7 and an electrode clamp.
Specifically, the cavity of the electrochemical cell 1 is filled with an electrolyte 10, and in this embodiment, the electrolyte 10 is lithium hexafluorophosphate. The reference electrode 2 is arranged on one side of the inner wall of the cavity of the electrochemical cell 1; the counter electrode 3 is arranged on the other side of the inner wall of the cavity of the electrochemical cell 1; the electrode clamp is arranged on the bottom wall of the cavity of the electrochemical cell 1, and a working electrode 8 is clamped on the electrode clamp; the external electrode 7 is arranged on the outer wall of the electrochemical cell 1 and is used for connecting an external electrochemical analysis device.
The voltage of the reference electrode 2, the control current of the counter electrode 3 and the working electrode 8 are all connected with an external electrode 7 through a lead 6 embedded in the cell body of the electrochemical cell 1.
During testing, the testing device is arranged below a pressure head 9 of the nanoindentation tester.
Further, in this embodiment, the electrode holder includes a conductive connecting member 5 disposed on the bottom wall of the cavity of the electrochemical cell 1 and a fixing member 4 disposed on the conductive connecting member 5, the working electrode 8 is disposed on the conductive connecting member 5 and located inside the fixing member 4, and the working electrode 8 is connected to the external electrode 7 through the conductive connecting member 5.
Specifically, in the present embodiment, the fixing member 4 includes a clamping plate disposed around the conductive connecting member 5, and the clamping plate is connected to the conductive connecting member 5 through a return spring, and the fixing member 4 in the present embodiment is similar to a clip structure in the prior art.
Further, in this embodiment, the fixing member 4 is made of an insulating material to prevent contact with the device. The material of the cell 1 is teflon to avoid reaction with the electrolyte.
Based on the same inventive concept, the embodiment also provides a method for testing the in-situ mechanical electrochemical performance of the lithium battery, in the embodiment, the working electrode 8 is a lithium cobaltate thin film electrode, and before the test, lithium cobaltate (LiCoO) is firstly carried out on an aluminum foil current collector 2 ) And performing magnetron sputtering deposition on the film to prepare a plurality of lithium cobaltate film electrodes in the same batch.
As shown in fig. 3, the test procedure includes the following steps:
step 1, loading the lithium cobaltate thin film electrode on a conductive connecting piece 5, clamping the lithium cobaltate thin film electrode through a fixing piece 4, and keeping one side of an aluminum foil current collector of the lithium cobaltate thin film electrode in close and stable contact with the conductive connecting piece 5.
Step 2, fixing the electrochemical cell 1 on an objective table of a nanoindentation tester,
step 3, connecting the external electrode 7 to an external electrochemical analysis device; the potential range was set to 2.0 to 3.7V, and charge and discharge cycles were performed at 1C, 2C and 5C rates until the cell capacity was reduced to 80% SOC.
Step 4, injecting electrolyte 10 (1M lithium hexafluorophosphate organic solvent) into the cavity of the electrochemical cell 1, wherein the lithium cobaltate film electrode, the reference electrode 2 and the counter electrode 3 are all positioned in the electrolyte 10;
step 5, marking the area to be tested of the lithium cobaltate thin film electrode through an optical mirror of the nano indentation tester, and ensuring that the intervals of all marked areas are proper and have no mutual influence;
step 6, based on the Oliver-Pharr method, pressing down the target area marked on the lithium cobaltate thin film electrode by using a pressing head 9 of a nano indentation tester and generating scratches;
and 7, sending the data acquired in the pressing process to a host of the nanoindentation tester for analysis by a Berkovich pressure head 9 of the nanoindentation tester to obtain the mechanical property of the lithium cobaltate film electrode in the electrochemical reaction process. Specifically, the mechanical properties of the lithium cobaltate thin film electrode are obtained through obtaining indentation geometric parameters and a load-displacement curve of the lithium cobaltate thin film electrode in the electrochemical reaction process and through the indentation geometric parameters and the load-displacement curve.
The reference electrode 2 and the counter electrode 3 send the acquired data to an external electrochemical analysis device, the data are analyzed by the external electrochemical analysis device to obtain the electrochemical performance of the lithium cobalt oxide film electrode in the electrochemical reaction process, and then the dynamic mechanical response rule of the lithium cobalt oxide film electrode along with the electrochemical reaction is obtained.
And carrying out statistical analysis on the data of a plurality of samples in the same batch to obtain the force-electrochemical coupling rule of the lithium cobaltate film electrode in the set electrochemical reaction process.
Furthermore, in the test of this embodiment, the electrochemical cell 1 and the nanoindentation tester were placed in a glove box filled with argon gas, and the oxygen concentration of water in the glove box was less than 0.1mg L -1 。
In summary, the present invention has the following advantages:
1. different from the distortion characteristic of ex-situ test, the invention can simultaneously realize the in-situ chemical performance test of the working electrode through the reference electrode and the counter electrode, and simultaneously can realize the in-situ force electrochemical performance test of the working electrode through the nanoindentation tester, thereby obtaining the dynamic mechanical response characteristic of the working electrode in the electrochemical reaction process and researching the real-time change rule of the working electrode under different working conditions.
2. The invention can be used for researching various lithium battery electrodes, including membranes, polished composite electrodes, metal foils and the like, and is also suitable for similar materials of other batteries.
3. The invention has simple and flexible composition, is easy to replace and maintain the components, and can be matched with more characterization means to carry out combined synchronous test by adjusting the configuration of the equipment.
The above-mentioned embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (10)

1. The utility model provides a lithium cell normal position power electrochemical performance testing arrangement which characterized in that includes:
the electrochemical cell comprises an electrochemical cell (1), wherein electrolyte (10) is injected into a cavity of the electrochemical cell (1);
the reference electrode (2) is arranged on one side of the inner wall of the cavity of the electrochemical cell (1);
the counter electrode (3) is arranged on the other side of the inner wall of the cavity of the electrochemical cell (1);
the electrode clamp is arranged on the bottom wall of the cavity of the electrochemical cell (1), and a working electrode (8) is clamped on the electrode clamp;
the external electrode (7) is arranged on the outer wall of the electrochemical cell (1) and is used for being connected with an external electrochemical analysis device;
the reference electrode (2), the counter electrode (3) and the working electrode (8) are all connected with the external electrode (7) through leads (6);
during testing, the testing device is arranged below a pressure head (9) of the nanoindentation tester.
2. The lithium battery in-situ mechanical and electrochemical performance testing device according to claim 1, wherein the electrode clamp comprises a conductive connecting piece (5) arranged on the bottom wall of the cavity of the electrochemical cell (1) and a fixing piece (4) arranged on the conductive connecting piece (5), the working electrode (8) is arranged on the conductive connecting piece (5) and located inside the fixing piece (4), and the working electrode (8) is connected with the external electrode (7) through the conductive connecting piece (5).
3. The lithium battery in-situ mechanical-electrochemical performance testing device as claimed in claim 2, wherein the fixing member (4) comprises a clamping plate arranged around the conductive connecting member (5), and the clamping plate is connected with the conductive connecting member (5) through a return spring.
4. The lithium battery in-situ mechanical and electrochemical performance testing device as set forth in claim 3, characterized in that the fixing member (4) is made of an insulating material.
5. The in-situ mechatronic performance testing device of a lithium battery as claimed in claim 1, characterized in that the lead (6) is embedded in the body of the electrochemical cell (1).
6. The in-situ mechatronic performance testing device of a lithium battery as claimed in claim 1, characterized in that the material of the electrochemical cell (1) is polytetrafluoroethylene.
7. The in-situ mechanochemical performance testing device for lithium batteries according to claim 1, wherein the electrolyte (10) is lithium hexafluorophosphate.
8. A testing method of the lithium battery in-situ mechanical electrochemical performance testing device according to any one of claims 1 to 7, characterized by comprising the following steps:
loading a working electrode (8) on the conductive connecting piece (5), and clamping the working electrode (8) through the fixing piece (4);
the electrochemical cell (1) is fixed on an objective table of a nano-indentation tester,
connecting the external electrode (7) to an external electrochemical analysis device;
electrolyte (10) is injected into the cavity of the electrochemical cell (1), and the working electrode (8), the reference electrode (2) and the counter electrode (3) are all positioned in the electrolyte (10);
marking the region to be detected of the working electrode (8) through an optical mirror of the nanoindentation tester;
pressing down the marked target area on the working electrode (8) by using an indenter (9) of a nanoindentation tester based on an Oliver-Pharr method and generating a scratch;
a pressure head (9) of the nano indentation tester sends data acquired in the pressing process to a host of the nano indentation tester for analysis, and the mechanical property of a working electrode (8) in the electrochemical reaction process is obtained;
the reference electrode (2) and the counter electrode (3) send the collected data to an external electrochemical analysis device, and the external electrochemical analysis device analyzes the data to obtain the electrochemical performance of the working electrode (8) in the electrochemical reaction process.
9. The in-situ force electrochemical performance testing method of the lithium battery as claimed in claim 8, wherein during testing, the pressure head (9) of the nanoindentation tester sends the acquired data to a host of the nanoindentation tester for analysis, so as to obtain indentation geometric parameters and a load-displacement curve of the working electrode (8) in an electrochemical reaction process, and obtain the mechanical performance of the working electrode (8) through the indentation geometric parameters and the load-displacement curve.
10. The in-situ electrochemical performance testing method of the lithium battery as claimed in claim 8, wherein during testing, the electrochemical cell (1) and the matched nanoindentation tester are placed in a glove box filled with argon, and the water oxygen concentration in the glove box is lower than 0.1mg L -1 。
CN202211381778.2A 2022-11-05 2022-11-05 Lithium battery in-situ force electrochemical performance testing device and method Pending CN115575827A (en)

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CN202211381778.2A CN115575827A (en) 2022-11-05 2022-11-05 Lithium battery in-situ force electrochemical performance testing device and method

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CN202211381778.2A CN115575827A (en) 2022-11-05 2022-11-05 Lithium battery in-situ force electrochemical performance testing device and method

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