CN112697863B - Electrochemical optical synchronous test sample table - Google Patents
Electrochemical optical synchronous test sample table Download PDFInfo
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- CN112697863B CN112697863B CN202011433547.2A CN202011433547A CN112697863B CN 112697863 B CN112697863 B CN 112697863B CN 202011433547 A CN202011433547 A CN 202011433547A CN 112697863 B CN112697863 B CN 112697863B
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- electrode connecting
- connecting column
- sample table
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- column
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- 238000012360 testing method Methods 0.000 title claims abstract description 22
- 230000003287 optical effect Effects 0.000 title claims abstract description 15
- 230000001360 synchronised effect Effects 0.000 title claims abstract description 7
- 239000007772 electrode material Substances 0.000 claims abstract description 12
- 238000013461 design Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 71
- 238000007789 sealing Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000004519 grease Substances 0.000 claims description 3
- 239000000565 sealant Substances 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 230000005518 electrochemistry Effects 0.000 claims 7
- 238000011065 in-situ storage Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 9
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000002441 X-ray diffraction Methods 0.000 abstract description 3
- 238000001237 Raman spectrum Methods 0.000 abstract description 2
- 238000010325 electrochemical charging Methods 0.000 abstract 1
- 238000010326 electrochemical discharging Methods 0.000 abstract 1
- 238000003384 imaging method Methods 0.000 abstract 1
- 230000007774 longterm Effects 0.000 abstract 1
- 238000012827 research and development Methods 0.000 abstract 1
- 210000004027 cell Anatomy 0.000 description 12
- 238000011160 research Methods 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 210000002777 columnar cell Anatomy 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L9/00—Supporting devices; Holding devices
- B01L9/02—Laboratory benches or tables; Fittings therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Clinical Laboratory Science (AREA)
- Molecular Biology (AREA)
- Electrochemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses an electrochemical optical synchronous test sample table, which can be used as a matched instrument of an optical instrument, belongs to the field of research and development of new energy electrode materials, and can be used for carrying out optical synchronous analysis, such as X-ray diffraction analysis, raman spectrum test, microscopic imaging analysis and the like, on an ion battery in the electrochemical charging and discharging process. The sample table is provided with an internal design for adjusting the electrode assembly pressure by using the gasket and the elastic sheet, so that the electrochemical process of in-situ synchronous analysis is close to a button cell, the change of the electrode material in the charge and discharge process can be more accurately reflected, and the sample table is suitable for in-situ observation in the long-term circulation process, is convenient to mount and dismount, is easy to maintain and operate, and is suitable for beginners to use.
Description
Technical Field
The invention relates to the field of auxiliary experimental equipment required by new energy battery material research, which can be used for carrying out optical analysis on materials under electrochemical test conditions, including Raman spectrum, microscopic morphology observation, X-ray diffraction analysis and the like.
Background
Research on lithium ion batteries has gradually matured, and research on new electrode materials with high efficiency, durability and large charge-discharge voltage window has become an important component part in secondary battery development strategy, and meanwhile, research on failure reasons of lithium ion batteries has gradually developed. The failure root of the lithium ion battery is the failure process of the material in the charging and discharging process, the positive electrode material generates cracks due to volume change, the positive ions dissolve out and the electrode is attenuated due to oxygen release, and the irregular generation of SEI on the negative electrode and the electrode attenuation due to the change of a crystal structure caused by stress strain due to the volume change of the negative electrode material are the main directions of research. Meanwhile, other problems to be solved include the contribution of electrolyte and separator to the degradation of battery performance during the electrical cycle. The research on the charge and discharge process by combining various in-situ and ex-situ characterization means is an important means for continuously improving the performance of the lithium ion battery. One of the problems in-situ research is that in-situ test instruments are generally different from widely used button cells, columnar cells and soft-pack cells in structure, so that electrochemical performances of the button cells, the columnar cells and the soft-pack cells are often not matched, a certain difficulty is caused on how to combine in-situ experimental electrochemical data with real cell data, and how to improve the structure of the in-situ test instruments to enable the in-situ test instruments to have similar electrochemical data as those of the button cells, the columnar cells, the soft-pack cells and the like, so that the problems to be solved are urgent. In order to make up for the defects of the current testing method, the patent provides a sample stage which has an internal design similar to a button cell, enables an electrochemical process of in-situ synchronous analysis to be close to the button cell, and can more accurately reflect the change of electrode materials in the charge and discharge process. The design of the sample stage has universality, the appearance of the sample stage can be conveniently changed so as to meet the use requirements of different optical instruments, meanwhile, the sample stage is simple and convenient to assemble, has good repeated measurement stability, and is suitable for in-situ research of electrode materials under the condition of long circulation.
Disclosure of Invention
As described above, the present invention provides a device suitable for optical analysis, especially X-ray diffraction analysis experiment, in two-electrode electrochemical reaction, and has good air tightness, and can ensure the test under inert gas environment condition, the invention adopts the following technical scheme: by sample platform main part (01), sample platform main part lower cover (02), working electrode spliced pole (03), counter electrode spliced pole (04), insulating ring (05), working electrode spliced pole extension column (06), fixation nut (07) and window (08) constitute the main outer structure of sample platform, there is inclosed space in, can place the test electrode piece, the diaphragm, gasket and shell fragment, place O circle through the recess that is located in sample platform main part (01) and seal, light can be incident in the material that awaits measuring that is located the window below through window (08), have down counter bore on sample platform main part lower cover (02) and place magnet (09), play the positioning action with location magnet (11) on the fixed disc of electrode connecting wire (10) position the same, have three electrode connecting wire (12) on the fixed disc of electrode connecting wire (10) respectively with working electrode spliced pole extension column (06) and counter electrode spliced pole (04). The shape and size of the sample stage main body (01) can be changed according to actual needs.
The sample table is internally provided with the space for placing the electrode material, the diaphragm, the gasket and the elastic sheet, so that the assembly mode of the electrode plate in the sample table is the same as that of the button cell, the electrochemical performance similar to that of the button cell is obtained, and the assembly of the electrode material, the diaphragm, the gasket and the elastic sheet is carried out in the insulating ring (05), thereby being beneficial to the alignment of the electrodes and avoiding short circuit.
The working electrode connecting column extension column (06) can be composed of a pogo probe, a sealing gasket and a stainless steel column, wherein the working electrode connecting column extension column (06) is sealed by sealant, and the working electrode connecting column extension column can be composed of a pogo probe, a sealing gasket and a stainless steel column, and the working electrode connecting column extension column can be sealed by a sealing gasket ring.
The window (08) can be made of different materials, is suitable for different testing methods, is sealed with the sample stage main body (01) through vacuum grease, can be tightly combined with the insulating ring (05), and has a sealing function.
The pogo probe on the working electrode connecting column extending column (06) has certain elasticity, so that stable connection can be provided, and meanwhile, excessive extrusion damage to the viewing window (08) can not be caused.
The counter electrode connecting column (04) and the working electrode connecting column extending column (06) are all of hidden designs, and the main body of the electrode connecting column is hidden inside the sample table main body, so that the short circuit caused by improper operation is reduced.
The positions of the magnets (11) on the electrode connecting wire fixing disc (10) are the same as those of the magnets (09) on the lower cover (02) of the sample table main body, and the magnets can be attracted to each other through magnetism to play a role in positioning, the electrode connecting wire fixing disc (10) is provided with three electrode connecting wires (12) which are respectively composed of pogo probes and correspond to the working electrode connecting column extending column (06) and the counter electrode connecting column (04), and when the electrode connecting column is used, the two groups of magnets correspond to each other, so that the electrode connecting column on the sample table can be automatically connected with the three electrode connecting wires (12) on the electrode connecting wire fixing disc (10).
Drawings
The patent of the invention is further described below with reference to the accompanying drawings and examples.
FIG. 1 is a schematic overall appearance of the sample stage.
FIG. 2 is a schematic top view of the sample stage.
FIG. 3 is a schematic view of the whole appearance of the sample stage.
Fig. 4 is a schematic cross-sectional view of the sample stage 1, taken along the direction of the dashed line a in fig. 3.
Fig. 5 is a schematic cross-sectional view of the sample stage 2, taken along the direction of the dashed line b in fig. 3.
Fig. 6 is a schematic cross-sectional view of the sample stage, shown in fig. 3, in the direction of the dashed line a.
FIG. 7 is a schematic side view of the whole appearance of the sample stage.
Fig. 8 is a schematic top view of the electrode connection wire fixing disk and the connection wire.
Fig. 9 is a schematic side view of the electrode connection wire fixing disk and its connection wire.
Fig. 10 is a schematic view of the electrode connection wire fixing disk and its connection wire as a whole.
In the figure, the sample platform body 01, the sample platform body lower cover 02, the working electrode connecting column 03, the counter electrode connecting column 04, the insulating ring 05, the working electrode connecting column extension column 06, the fixing nut 07, the window 08, the magnet 09, the electrode connecting wire fixing disc 10, the positioning magnet 11 and the electrode connecting wire 12.
Detailed Description
[ Example 1]
The sample stage can carry out optical test on the electrode material while charging and discharging, the assembly mode of the electrode material is the same as that of a button cell, the tightness is good, and the sample stage is suitable for carrying out long-cycle in-situ test on the electrode material.
As shown in fig. 1 to 7, the sample stage outer body according to the present invention mainly comprises a sample stage body 01, a sample stage body lower cover 02, a working electrode connecting column 03, a counter electrode connecting column 04, an insulating ring 05, a working electrode connecting column extending column 06, a fixing nut 07, a window 08, and a magnet 09. The connecting device (shown in fig. 8-10) formed by the positioning magnet 11 and the electrode connecting wire 12 is connected in a magnetic attraction mode through the fixing disc 10 for the electrode connecting wire, and meanwhile, the electrode connecting wire 12 is connected with an external electrochemical workstation for accurately controlling current and voltage.
When the sample stage is used, the sample stage main body 01 is horizontally placed on an operation table, a small amount of vacuum silicone grease is smeared at a window, the window 08 is placed, the insulating ring 05 is placed, the two working electrode connecting columns 03 are installed, then the electrode to be tested, the diaphragm and the electrolyte are sequentially assembled, the other electrode slice, the gasket and the elastic sheet are added, then the sample stage main body lower cover 02 is installed, whether the O ring is clean or not is checked, and the sample stage main body is fixed through the fixing nut 07. The counter electrode connecting column 04 and the working electrode connecting column extending column 06 are arranged on the lower cover 02 of the sample table main body. If the working electrode connecting column extending column 06 is formed by a pogo probe, the working electrode connecting column is sealed by sealant, and if the working electrode connecting column extending column 06 is formed by a pogo probe, a sealing gasket and a stainless steel column, the working electrode connecting column extending column 06 can be sealed by a sealing gasket ring. The space between the counter electrode connecting column 04 and the sample stage main body lower cover 02 is sealed by placing an O-ring. The three electrode connection lines 12 are respectively formed by soldering or physically contacting a pogo probe and a wire, the three electrode connection lines 12 are fixed on the electrode connection line fixing disk 10 through AB glue, and the magnet 11 is bonded on the electrode connection line fixing disk (10). The magnet 11 on the electrode connecting wire fixing disc 10 is the same as the magnet 09 on the sample stage main body lower cover 02 in position, and can be attracted to each other magnetically to play a role in positioning, when in use, the electrode connecting wire fixing disc 10 is close to the sample stage main body lower cover 02, and the pogo probe can stretch out and draw back through magnetic connection, and is connected with the counter electrode connecting column 04 and the working electrode connecting column extending column 06 on the sample stage while being connected magnetically. During electrochemical test, any working electrode connecting column extending column 06 is taken as a working electrode, and an electrode connecting column 04 is taken as a counter electrode and connected into an electrochemical workstation. When the air tightness detection is needed, a working electrode connecting column extending column 06 can be installed first, the air tightness detection is carried out through an uninstalled interface, and after the detection is finished, the working electrode connecting column extending column is installed.
Claims (7)
1. The electrochemistry optics synchronous test sample platform, its characterized in that: the sample table is composed of a sample table main body (01), a sample table main body lower cover (02), a working electrode connecting column (03), a counter electrode connecting column (04), an insulating ring (05), a working electrode connecting column extending column (06), a fixing nut (07) and a window (08) which form a main external structure of the sample table, a closed space is arranged in the main body, a test electrode plate, a diaphragm, a gasket and an elastic sheet are placed, an O ring is placed through a groove in the sample table main body (01) for sealing, light enters a material to be tested below the window through the window (08), a lower counter bore placing magnet (09) is arranged on the sample table main body lower cover (02), the positioning function is achieved by the same position of a positioning magnet (11) on an electrode connecting column fixing disc (10), three electrode connecting wires (12) are respectively corresponding to the working electrode connecting column extending column (06) and the counter electrode connecting column (04), the positions of the magnets (11) on the electrode connecting column fixing disc (10) are the same as the positions of the magnets (09) on the sample table main body lower cover (01), the positions of the magnets (09) are mutually connected through the magnetic connecting wires, the positioning function is achieved, the electrode connecting wires are fixedly connected to the electrode connecting column (10) by the three electrode connecting columns (12) and the electrode connecting column (06) respectively, when the electrode connecting column (12) are correspondingly connected with the electrode connecting column (06) in a mode, the electrode connecting column on the sample table is automatically connected with three electrode connecting wires (12) on the electrode connecting wire fixing disc (10).
2. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the shape and size of the sample stage main body (01) are changed according to actual needs.
3. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the sample stage is internally provided with a space for placing electrode materials, a diaphragm, a gasket and an elastic sheet, so that the assembly mode of the electrode plate in the sample stage is the same as that of the button cell, the electrochemical performance similar to that of the button cell is obtained, and the assembly of the electrode materials, the diaphragm, the gasket and the elastic sheet is carried out in an insulating ring (05), thereby being beneficial to the alignment of electrodes and avoiding short circuits.
4. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the working electrode connecting column extension column (06) is composed of a pogo probe or a pogo probe, a sealing gasket and a stainless steel column, wherein the former is sealed by sealant, and the latter is sealed by a sealing gasket ring.
5. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the window (08) is made of different materials and is suitable for different testing methods, and meanwhile, the window (08) and the sample table main body (01) are sealed through vacuum grease, and the window (08) and the insulating ring (05) are tightly combined and have a sealing function.
6. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the pogo probe on the working electrode connecting column extending column (06) has certain elasticity, and can provide stable connection without causing excessive extrusion damage to the viewing window (08).
7. The electrochemistry optical synchronization test sample stage according to claim 1, wherein: the counter electrode connecting column (04) and the working electrode connecting column extending column (06) are all of hidden designs, and the main body of the electrode connecting column is hidden inside the sample table main body, so that the short circuit caused by improper operation is reduced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011433547.2A CN112697863B (en) | 2020-12-10 | 2020-12-10 | Electrochemical optical synchronous test sample table |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011433547.2A CN112697863B (en) | 2020-12-10 | 2020-12-10 | Electrochemical optical synchronous test sample table |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112697863A CN112697863A (en) | 2021-04-23 |
| CN112697863B true CN112697863B (en) | 2024-07-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011433547.2A Active CN112697863B (en) | 2020-12-10 | 2020-12-10 | Electrochemical optical synchronous test sample table |
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| Country | Link |
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| CN (1) | CN112697863B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109813662A (en) * | 2019-01-27 | 2019-05-28 | 南杰智汇(深圳)科技有限公司 | The device of original position optic test under electrochemical conditions can be carried out to metal-air battery |
| CN110361403A (en) * | 2019-08-20 | 2019-10-22 | 南杰智汇(深圳)科技有限公司 | X-ray diffraction analysis sample stage with three-electrode electro Chemical test function |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7695601B2 (en) * | 2006-05-09 | 2010-04-13 | The United States Of America As Represented By The Secretary Of The Army | Electrochemical test apparatus and method for its use |
| JP2010217012A (en) * | 2009-03-17 | 2010-09-30 | Nec Corp | Infrared detector and device manufacturing apparatus |
| CN111830071B (en) * | 2019-04-14 | 2024-07-05 | 南杰智汇(深圳)科技有限公司 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
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2020
- 2020-12-10 CN CN202011433547.2A patent/CN112697863B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109813662A (en) * | 2019-01-27 | 2019-05-28 | 南杰智汇(深圳)科技有限公司 | The device of original position optic test under electrochemical conditions can be carried out to metal-air battery |
| CN110361403A (en) * | 2019-08-20 | 2019-10-22 | 南杰智汇(深圳)科技有限公司 | X-ray diffraction analysis sample stage with three-electrode electro Chemical test function |
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| CN112697863A (en) | 2021-04-23 |
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