CN112394096A - Novel three-electrode electrochemical testing device - Google Patents
Novel three-electrode electrochemical testing device Download PDFInfo
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- CN112394096A CN112394096A CN202011416075.XA CN202011416075A CN112394096A CN 112394096 A CN112394096 A CN 112394096A CN 202011416075 A CN202011416075 A CN 202011416075A CN 112394096 A CN112394096 A CN 112394096A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- 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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
The invention discloses a novel three-electrode electrochemical testing device, and belongs to the field of testing and research of energy storage devices (such as batteries, capacitors and the like). The device has three-electrode design of a positive electrode, a negative electrode and a reference electrode, and is provided with the pressure sensing device, so that the pressure change between the positive electrode and the negative electrode in the electrode installation process and the test process can be tracked, the repeatability of the test is favorably improved, convenience is provided for optimizing the energy storage device, and the research on the electrochemical working principle and the capacity attenuation principle of a novel electrode is helped. The device is provided with a liquid/gas inlet and outlet, so that gas generated in the electrochemical test process can be conveniently led out for component test, and meanwhile, electrolyte can be added or extracted in the electrochemical test process. The testing device can be disassembled for repeated use for many times, is easy to maintain and operate, and is suitable for being used by scientific research institutions and factory workers.
Description
Technical Field
The invention relates to a novel three-electrode electrochemical testing device, and belongs to the field of testing and research of energy storage devices. The device has a positive electrode, a negative electrode and a reference electrode, is provided with a pressure sensing device, and can track the pressure change between the positive electrode and the negative electrode in the electrode installation and test process. Meanwhile, the device is provided with a liquid/gas inlet and outlet, so that gas generated in the electrochemical test process can be conveniently led out for further testing, and electrolyte can be added or extracted in the electrochemical test process.
Background
China faces serious environmental pressure, so that the development of renewable energy sources is more emphasized, and the power generation concentration time period and the power utilization time period of the renewable energy sources are inconsistent, so that battery energy storage is an effective scheme for solving the instability of power generation of the renewable energy sources. Further improving the development of battery technology, and developing a battery technology product with larger capacity and long service life is the development direction in the field of energy storage at present. Compared with a two-electrode test, the three-electrode test can provide more accurate information of electrode materials for scientific research personnel, and is helpful for overcoming the technical problem in battery development. At present, the research on a three-electrode testing device of a battery is very long, for example, a Chinese utility model patent with an authorization publication number of CN 207967200U discloses a method for a three-electrode lithium battery, a third electrode is introduced into a soft package battery test, and similarly, an invention patent with an authorization publication number of CN 108630980A discloses a lithium ion three-electrode soft package battery and a testing method thereof, and the third electrode is also introduced into a soft package battery test; in addition, patent publication CN 107959056 a discloses a "three-pole test battery" device similar to a button cell.
The function of these devices is mainly focused on introducing a third reference electrode into a conventional two-electrode test device, and it is not possible to track the pressure between the electrodes from time to time, to provide no outlet for testing the by-products generated during the electrochemical process of the cell, and to check the hermeticity of the device, etc. In summary, instruments that can perform three-electrode testing on batteries and have multifunctional testing capabilities are still missing. In order to make up the defects of the existing testing method and enable a three-electrode testing means to become a favorable tool for researching electrochemical reaction and new energy batteries, the patent provides a device capable of carrying out two-electrode and three-electrode electrochemical testing, and the device is suitable for various ion batteries, air batteries and super-electrode capacitors. The device can track pressure change and gas generation generated in the electrochemical reaction process, can test the tightness of an instrument before the electrochemical test, samples and adds electrolyte in the electrochemical test process, and can enable the electrochemical reaction to be carried out in a specific atmosphere through the gas inlet and the gas outlet. The design of this sample platform has the universality, can test the electrode slice of equidimension not, and the test space can be adjusted in order to be applicable to different test needs, and the equipment is simple and convenient simultaneously, and measurement repeatability is good, is suitable for long-circulating test.
Disclosure of Invention
As mentioned above, aiming at the problem of the lack of a multifunctional easily-disassembled three-electrode battery/super-electrode capacitor testing device, the invention provides a device suitable for analyzing and testing electrode materials in a two-electrode or three-electrode electrochemical reaction, which can detect the air tightness, detect the pressure between electrode plates, control the testing atmosphere to perform experiments under different gas environment conditions, and simultaneously has an interface externally connected with a testing instrument to perform various on-line detection functions, in order to achieve the purpose, the invention adopts the technical scheme that firstly, a closed space is formed by a sample table main body base, a sample table base electrode, a sample table main body upper cover, a sample table upper cover electrode, two electrode connecting columns and a reference electrode connecting port, and all the components are sealed by pressing joints or sealing rings, the base of the sample table main body and the upper cover of the sample table main body are fixed together through the nut, and the purposes of detecting the air tightness of the device, controlling the testing atmosphere and carrying out various different on-line detections are achieved through the gas/liquid inlet and outlet. Pressure sensor is placed in the cylinder type recess on the outside bottom surface of sample platform base electrode, the sensor control line is derived through sample platform main part base wire passageway, pressure sensor can realize carrying out the purpose that detects to the pressure between the electrode piece, cylinder in the sample platform base electrode is electrode material place the platform, highly can set up the positive and negative electrode piece in order to adapt to different thickness according to the experiment requirement, sample platform upper cover electrode is equipped with double thread structure, can finely tune the distance between upper cover electrode and the sample platform base electrode, reference electrode places in the reference electrode interface, highly can adjust, in order to adapt to the requirement of different tests. The electrode connecting column is of a hidden design, the main body of the electrode connecting column is hidden inside the main body of the sample table, the situation of short circuit caused by improper operation is reduced, and the electrode connecting column is provided with a groove inside and can be directly connected with a banana plug for being connected with an external circuit.
The pressure sensor can measure the compression degree of the electrode material and the diaphragm in the assembling process and output data quantitatively, can test the electrode materials with different thicknesses under the consistent pressure condition, and can measure the pressure change generated by side reaction and volume expansion of the electrode material in the electrochemical reaction process.
The reference electrode connector can fix various reference electrodes such as Ag/AgCl, RHE, SCE, saturated calomel electrode, platinum wire, lithium metal, graphite, battery anode materials (LiFePO4, LMO and LTO) and the like, electrolyte solution can be added into the sample stage base electrode to facilitate the reference electrode to be immersed in the sample stage base electrode, and the distance between the reference electrode and the working electrode can be adjusted through the position of the reference electrode connector.
One or two gas/liquid inlets and outlets can be arranged on the upper cover of the sample table main body according to requirements, gas can be allowed to enter and exit, the gas can be in full contact with a tested material, an electrochemical reaction can be carried out in a specific atmosphere environment, the gas generated in the electrochemical reaction process can be led out of the testing device and is connected with a gas chromatograph and the like for further detection, and the functions of the gas/liquid inlets and outlets can be connected with a gas pressure meter to monitor the pressure change of the testing device caused by side reaction in the electrochemical reaction process.
The gas/liquid inlet and outlet on the upper cover of the sample stage main body has the functions of sampling and adding sample to the electrolyte in the testing device before and after the reaction process and in the reaction process, and can also test the air tightness of the testing device through the gas/liquid inlet and outlet.
The sealing ring is used for sealing the electrode on the sample table upper cover and the electrode connecting column 2, meanwhile, the sealing ring is used as a spring piece to apply pressure to the counter electrode and the diaphragm assembled in the sample table, the effects of improving contact between the electrodes and pressing the electrodes and the diaphragm are achieved, the sample table upper cover electrode is provided with a double-thread structure, the distance between the upper cover electrode and the sample table base electrode can be finely adjusted, and the stress between the electrodes and the diaphragm is controlled through adjusting the distance.
The electrode and the electrode connecting column of the sample table base are in contact connection or can be connected through threads, the electrode and the electrode connecting column 2 of the sample table upper cover are connected through threads, the sample table main body upper cover, the sample table upper cover electrode, the electrode connecting column 2 and the sealing ring can be assembled into a module, and the whole assembly of the testing device is facilitated.
Foretell testing arrangement's sample platform main part base appearance is the drop shape, and the design is unique pleasing to the eye, compares simultaneously more circularly easily fixedly, designs and appearance assorted draw-in groove, or fixes with 5 stands.
The testing device is mainly prepared from materials with chemical corrosion resistance, such as Polyetheretherketone (PEEK), polyphenylene sulfide (PPS), 316L stainless steel and the like.
The invention has the advantages that the invention provides a device which can carry out three-electrode electrochemical test on the battery/super-electrode capacitor and simultaneously measure the pressure between electrode materials, and the invention can also carry out various on-line tests while carrying out the electrochemical test.
Drawings
The invention is further described with reference to the following figures and examples.
FIG. 1 is a schematic overall appearance of a sample stage.
FIG. 2 is a cross-sectional view of a sample stage.
In the figure, 01, a sample table main body base, 001, a sample table base electrode, 02, a sample table main body upper cover, 002, a sample table upper cover electrode, 03, an electrode connecting column, 04, an electrode connecting column 2, 05, a reference electrode connecting port, 06, a gas/liquid inlet/outlet 1, 07, a gas/liquid inlet/outlet 2, 08 and a pressure sensor are arranged.
Detailed Description
[ example 1 ]
The invention relates to a novel three-electrode electrochemical testing device which can be used for carrying out three-electrode electrochemical testing on a metal ion battery. While the pressure between the electrodes is detected.
As shown in fig. 1 and 2, the external main body of the testing device according to the present invention mainly comprises a sample stage main body base 01, a sample stage base electrode 001, a sample stage main body upper cover 02, a sample stage upper cover electrode 002, an electrode connecting column 03, an electrode connecting column (2)04, a reference electrode connecting port 05, a gas/liquid inlet/outlet (1)06, a gas/liquid inlet/outlet (2)07 and a pressure sensor 08, wherein the sample stage main body base 01 and the sample stage main body upper cover 02 are fixed together by a nut, the instrument is sealed by a sealing ring, the electrode connecting column 03 is connected with the sample stage base electrode 001, and the sample stage upper cover electrode 002 is connected with the electrode connecting column 04. When the electrode connecting column is used, the electrode connecting column 03 is connected with the electrode connecting column 04, the reference electrode connecting port 05 is connected with a banana plug which is additionally arranged, and the banana plug is connected with an external electrochemical workstation and used for accurately controlling current and voltage.
When the pressure sensor is used, the pressure sensor 08 is placed in the sample stage main body 01, then the sample stage base electrode 001 is placed, the electrode connecting column 03 is installed, and the O-shaped ring is placed. The sample platform main part upper cover 02 is turned over, an O-shaped ring is placed, an electrode 002 is arranged on the sample platform upper cover, an electrode connecting column 2 is arranged, and a sample platform main part upper cover installation module is assembled. Then, an electrode plate, a diaphragm, electrolyte and the other electrode plate are sequentially arranged on the inner cylinder of the sample stage base electrode 001. And covering the sample table main body upper cover installation module, and fixing the sample table main body upper cover installation module by four nuts. And a proper reference electrode is placed at the position of the reference electrode connecting port 05 according to the requirement, and the height is adjusted. One gas/liquid inlet and outlet 06 is blocked, and the other is connected with a simple tightness testing device which is generally composed of a connector, a thin tube and a syringe for injection, so that the air tightness of the instrument is checked. If the air tightness is good, the simple tightness testing device is taken out, and the gas/liquid inlet and outlet are blocked. During testing, the electrode connecting column 03 and the electrode connecting column 04 are connected, the reference electrode connecting port 05 is connected with a banana plug which is additionally equipped, the banana plug is connected with an external electrochemical workstation, the three-electrode electrochemical test of the battery can be realized, and the pressure change between the base electrode 001 of the sample table and the upper cover electrode 002 of the sample table is recorded through a special recorder/software of the sensor. The pressure can be regulated and controlled by finely adjusting the height of the electrode 002 on the upper cover of the sample table.
[ example 2 ]
The invention relates to a novel three-electrode electrochemical testing device which can be used for carrying out two-electrode/three-electrode electrochemical testing on a metal air battery.
The installation mode refers to [ embodiment 1 ], a pressure sensor is omitted, the surface of an electrode 002 on an upper cover of a sample table is subjected to groove treatment, two gas/liquid inlets and outlets 06 and 07 are used as a gas inlet and a gas outlet, so that air/oxygen is subjected to material exchange through the surface of the electrode and the surface of the electrode, a metal air battery is common in the two-electrode test condition, and if a three-electrode test is required, a reference electrode is selected according to specific conditions.
[ example 3 ]
The invention relates to a novel three-electrode electrochemical testing device which can carry out two-electrode/three-electrode electrochemical testing on a battery/super-electrode capacitor.
The installation was referred to [ example 1 ] with the pressure sensor omitted. The reference electrode was omitted for the two electrode test. During the three-electrode test, the reference electrode, the size of the diaphragm and the amount of the electrolyte are correctly selected.
[ example 4 ]
The invention relates to a novel three-electrode electrochemical testing device which can perform online analysis on gas generated when a battery/super-electrode capacitor is subjected to two-electrode/three-electrode electrochemical testing.
Referring to embodiment 2, one of the two gas/liquid inlets and outlets is blocked, and the other is used for leading out the generated gas for online analysis, if a gas chromatograph is connected or a gas pressure sensor is connected.
Claims (10)
1. A novel three-electrode electrochemical testing device is characterized in that: the testing device comprises a sample table main body base (01), a sample table base electrode (001), a sample table main body upper cover (02), a sample table upper cover electrode (002), an electrode connecting column (03), an electrode connecting column 2(04), a reference electrode connecting port (05), a gas/liquid inlet/outlet (06), and a gas/liquid inlet/outlet 2(07), wherein the main external structure of the sample table is formed by each component through a press fit joint or a sealing ring to form a closed space, the sample table main body base (01) and the sample table main body upper cover (02) are fixed together through nuts and are sealed through the sealing rings, a cylinder in the sample table base electrode (001) is an electrode material placing platform, the height can be adjusted and controlled according to experimental requirements to adapt to positive and negative electrode plates with different thicknesses, the sample table base electrode (001) is in contact connection with the electrode connecting column (03), the reference electrode is placed in the reference electrode connecting, the height can be adjusted, sample platform upper cover electrode (002) links to each other with electrode connecting post 2(04), places pressure sensor (08) in the cylinder type recess on sample platform base electrode (001) outside bottom surface, and the sensor control line is derived through sample platform main part base (01) wire passageway, and sample platform upper cover electrode (002) is equipped with double thread structure, can finely tune the distance between upper cover electrode (002) and sample platform base electrode (001).
2. The novel three-electrode electrochemical test device of claim 1, wherein: the electrode connecting column (03) and the electrode connecting columns 2 and 04 are all of a hidden design, the main bodies of the electrode connecting columns are hidden inside the main bodies of the sample tables, the situation of short circuit caused by improper operation is reduced, and grooves are formed in the electrode connecting columns and can be directly connected with banana plugs and used for being connected with an external circuit.
3. The novel three-electrode electrochemical test device of claim 1, wherein: the pressure sensor (08) is used for measuring the compression degree of the electrode material and the diaphragm in the assembling process and quantitatively outputting data, can test the electrode materials with different thicknesses under consistent pressure conditions, and can measure the pressure change generated by side reaction and volume expansion of the electrode material in the electrochemical reaction process.
4. The novel three-electrode electrochemical test device of claim 1, wherein: the reference electrode connecting port (05) can be used for connecting Ag/AgCl, RHE, SCE, saturated calomel electrode, platinum wire, lithium metal, graphite and battery anode material (LiFePO)4LMO, LTO) and the like, and electrolyte solution can be added into the base electrode (001) of the sample stage so as to be convenient for the reference electrode to be immersed in the electrolyte solution, and the distance between the reference electrode and the working electrode can be adjusted through the position of the reference electrode connecting port (05).
5. A novel three-electrode electrochemical test device according to claims 1 and 4, wherein: the upper cover (02) of the sample table main body can be provided with two gas/liquid inlets and outlets as required, the gas/liquid inlet and outlet (06) and the gas/liquid inlet and outlet (2) (07) or a gas/liquid inlet and outlet which can allow gas to enter and exit so that the gas can be in full contact with a tested material, an electrochemical reaction can be carried out in a specific atmosphere environment, the gas generated in the electrochemical reaction process can be led out of the test device to carry out component detection, and the gas/liquid inlet and outlet can be connected with a gas pressure gauge to monitor the change of the internal pressure of the test device caused by side reaction in the electrochemical reaction process.
6. The novel three-electrode electrochemical test device of claim 1, wherein: the functions of the gas/liquid inlet and outlet on the upper cover (02) of the sample table main body comprise sampling and sample adding of electrolyte in the testing device before and after the electrochemical reaction process and during the reaction process, and the gas tightness of the testing device can be tested through the gas/liquid inlet and outlet.
7. The novel three-electrode electrochemical test device of claim 1, wherein: the upper cover electrode (002) of the sample table and the electrode connecting column 2(04) are sealed through the sealing ring, meanwhile, the sealing ring is used as a spring plate to apply pressure to the electrode and the diaphragm assembled in the sample table, the effects of improving contact between the electrodes and pressing the electrode and the diaphragm are achieved, the upper cover electrode (002) of the sample table is provided with a double-thread structure, the distance between the upper cover electrode (002) and the base electrode (001) of the sample table can be finely adjusted, and stress between the electrode and the diaphragm is controlled through adjustment of the distance.
8. The novel three-electrode electrochemical test device of claim 1, wherein: the electrode (001) of the sample table base is in contact connection with the electrode connecting column (03) and can also be connected through threads, the electrode (002) of the sample table upper cover is connected with the electrode connecting column 2(04) through threads, the sample table main body upper cover (02), the electrode (002) of the sample table upper cover, the electrode connecting column 2(04) and the sealing ring can be assembled into a module, and the whole assembly of the testing device is facilitated.
9. The novel three-electrode electrochemical test device of claim 1, wherein: the appearance of this testing arrangement sample platform main part base (01) is the drop shape, and the design is unique pleasing to the eye, compares easily fixedly than circular base simultaneously.
10. The novel three-electrode electrochemical test device of claim 1, wherein: the testing device is mainly prepared from polyether ether ketone (PEEK), polyphenylene sulfide (PPS) and 316L stainless steel.
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| CN202011416075.XA CN112394096A (en) | 2020-12-10 | 2020-12-10 | Novel three-electrode electrochemical testing device |
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| CN202011416075.XA CN112394096A (en) | 2020-12-10 | 2020-12-10 | Novel three-electrode electrochemical testing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112986352A (en) * | 2021-04-06 | 2021-06-18 | 新乡医学院三全学院 | Battery material electrochemical performance testing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112986352A (en) * | 2021-04-06 | 2021-06-18 | 新乡医学院三全学院 | Battery material electrochemical performance testing device |
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