CN112697863A - Electrochemical optical synchronous test sample table - Google Patents
Electrochemical optical synchronous test sample table Download PDFInfo
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- CN112697863A CN112697863A CN202011433547.2A CN202011433547A CN112697863A CN 112697863 A CN112697863 A CN 112697863A CN 202011433547 A CN202011433547 A CN 202011433547A CN 112697863 A CN112697863 A CN 112697863A
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- electrode connecting
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- sample table
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- 238000012360 testing method Methods 0.000 title claims abstract description 27
- 230000003287 optical effect Effects 0.000 title claims abstract description 18
- 230000001360 synchronised effect Effects 0.000 title claims abstract description 15
- 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 75
- 238000007789 sealing Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 3
- 239000004519 grease Substances 0.000 claims description 3
- 230000005389 magnetism Effects 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000007600 charging Methods 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 4
- 238000002441 X-ray diffraction Methods 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract description 2
- 238000001237 Raman spectrum Methods 0.000 abstract 1
- 238000010325 electrochemical charging Methods 0.000 abstract 1
- 238000010326 electrochemical discharging Methods 0.000 abstract 1
- 238000003384 imaging method Methods 0.000 abstract 1
- 238000011160 research Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 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
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular 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
- 239000000565 sealant Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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
- G01N27/416—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 stage, 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, microscope imaging analysis and the like, on an ion battery in an electrochemical charging and discharging process. The sample table is provided with an internal design for adjusting the electrode assembly pressure by utilizing the gasket and the elastic sheet, so that the electrochemical process of in-situ synchronous analysis is close to that of a button cell, and the change of an electrode material in the charging and discharging process can be more accurately reflected.
Description
Technical Field
The invention relates to the field of auxiliary experimental equipment required by new energy battery material research, and can perform optical analysis on a material under an electrochemical test condition, including Raman spectroscopy, microscope morphology observation, X-ray diffraction analysis and the like.
Background
The research on lithium ion batteries has gradually matured, the research and development of new electrode materials with high efficiency, durability and large charge-discharge voltage window become an important component in the development strategy of secondary batteries, and meanwhile, the research on the failure reason of the lithium ion batteries is also gradually developed. The failure of the lithium ion battery is mainly researched by the root of the failure of the material in the charging and discharging process, the positive electrode material generates cracks due to volume change, the electrode attenuation caused by cation dissolution and oxygen release, the irregular generation of SEI on the negative electrode and the electrode attenuation caused by the change of a crystal structure caused by stress strain caused by the volume change of the negative electrode material. Meanwhile, other problems to be solved include the contribution of the electrolyte and the separator to the degradation of the battery performance during the electrical cycling process. The research on the charge and discharge process by combining various in-situ and non-in-situ characterization means is an important means for continuously improving the performance of the lithium ion battery. One of the problems in the in-situ research is that the in-situ test instrument is usually different from the button cell, the cylindrical cell and the soft package cell which are widely used in structure, so that the electrochemical performances of the in-situ test instrument and the soft package cell are often not consistent, which causes certain difficulty in combining the electrochemical data of the in-situ test with the real cell data, and how to improve the structure of the in-situ test instrument, so that the in-situ test instrument has electrochemical data similar to those of the button cell, the cylindrical cell, the soft package cell and the like, which becomes a problem to be solved urgently. In order to make up for the defects of the existing testing method, the patent provides a sample table which has an internal design similar to that of a button cell, so that the electrochemical process of in-situ synchronous analysis is close to that of the button cell, and the change of an electrode material in the charging and discharging process can be more accurately reflected. The design of the sample table has universality, the appearance of the sample table can be conveniently changed so as to meet the use requirements of different optical instruments, meanwhile, the sample table is simple and convenient to assemble, good in repeated measurement stability and suitable for in-situ research of electrode materials under a long-circulation condition.
Disclosure of Invention
As described above, the present invention provides a device suitable for performing optical analysis in two-electrode electrochemical reaction, particularly X-ray diffraction analysis experiment, and having good air tightness, and capable of ensuring the test of the experiment performed under inert gas environment conditions, aiming at the problem that the in-situ electrochemical sample stage in the current optical electrochemical synchronous analysis lacks an in-situ electrochemical sample stage capable of restoring the electrochemical test condition of a common button cell, and is also suitable for tracking and testing electrode materials under the condition of multiple cycles, the present invention adopts the technical scheme that: comprises a sample table main body (01), a sample table main body lower cover (02), a working electrode connecting column (03), the counter electrode connecting column (04), the insulating ring (05), the working electrode connecting column extending column (06), the fixing nut (07) and the window (08) form the main external structure of the sample table, a closed space is arranged in the sample table, can be used for placing a test electrode slice, a diaphragm, a gasket and a spring plate, an O ring is placed in a groove in the sample stage main body (01) for sealing, light can be transmitted through the window (08) and enters a material to be tested below the window, a lower counter bore placing magnet (09) is arranged on the sample stage main body lower cover (02), the electrode connecting wire fixing disc (10) is provided with three electrode connecting wires (12) which correspond to the working electrode connecting column extending column (06) and the counter electrode connecting column (04) respectively. The appearance and the size of the sample table main body (01) can be changed according to actual requirements.
The space for placing the electrode material, the diaphragm, the gasket and the elastic sheet is arranged in the sample stage, so that the electrode plate is assembled in the sample stage in the same way as the button cell, the electrochemical performance similar to that of the button cell is obtained, and the electrode material, the diaphragm, the gasket and the elastic sheet are assembled in the insulating ring (05), thereby being beneficial to the alignment of the electrodes and avoiding short circuit.
The working electrode connecting column extending column (06) can be composed of a pogo probe, or can also be composed of a pogo probe, a sealing gasket and a stainless steel column, wherein the pogo probe is sealed by a sealing glue, and the stainless steel column is sealed by a sealing gasket ring.
The window (08) can be made of different materials and is suitable for different testing methods, meanwhile, the window (08) and the sample table main body (01) are sealed through vacuum grease, the window (08) and the insulating ring (05) can be tightly combined, and the sealing function is achieved.
The pogo probe on the working electrode connecting column extending column (06) has certain elasticity, so that stable connection can be provided, and excessive extrusion damage to the window (08) can be avoided.
The counter electrode connecting column (04) and the working electrode connecting column extending column (06) are all of a hidden design, and the main body of the electrode connecting column is hidden inside the main body of the sample table, so that the condition of short circuit caused by improper operation is reduced.
The position of the magnet (11) on the electrode connecting wire fixing disc (10) is the same as that of the magnet (09) on the sample table main body lower cover (02), the magnet can attract each other through magnetism to play a role in positioning, three electrode connecting wires (12) on the electrode connecting wire fixing disc (10) are respectively composed of pogo probes and correspond to the working electrode connecting post extending post (06) and the counter electrode connecting post (04), two groups of magnets correspond to each other during use, and the electrode connecting posts on the sample table and the three electrode connecting wires (12) on the electrode connecting wire fixing disc (10) can be automatically connected.
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 schematic view of the entire appearance of the sample stage.
FIG. 3 is a schematic view of the entire appearance of the sample stage.
FIG. 4 is a schematic sectional view of the sample stage of FIG. 1, taken along the direction of the dotted line a in FIG. 3.
FIG. 5 is a schematic cross-sectional view of the stage, taken along the direction of the dotted line b in FIG. 3, as shown in FIG. 2.
FIG. 6 is a schematic sectional view of the stage, taken along the direction of the dotted line a in FIG. 3.
FIG. 7 is a schematic side view of the entire appearance of the sample stage.
FIG. 8 is a schematic top view of the electrode connecting wire fixing disk and the connecting wire thereof.
FIG. 9 is a side view of the electrode connecting wire fixing disk and the connecting wire thereof.
FIG. 10 is an overall view of the electrode connecting wire fixing disk and the connecting wires thereof.
In the figure, 01, a sample table main body, 02, a sample table main body lower cover, 03, a working electrode connecting column, 04, a counter electrode connecting column, 05, an insulating ring, 06, a working electrode connecting column extending column, 07, a fixing nut, 08, a window, 09, a magnet, 10, an electrode connecting line fixing disc, 11, a positioning magnet and 12, an electrode connecting line.
Detailed Description
[ example 1 ]
The sample table can perform optical test on the electrode material while charging and discharging, has the same assembly mode as a button cell and good sealing property, and is suitable for performing long-cycle in-situ test on the electrode material.
As shown in fig. 1 to 7, the external main body of the sample stage according to the present invention mainly comprises a sample stage main body 01, a sample stage 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, a window 08, and a magnet 09. The connecting device (as shown in fig. 8-10) formed by the electrode connecting wire fixing disc 10, the positioning magnet 11 and the electrode connecting wire 12 is connected in a magnetic attraction mode, and meanwhile, the electrode connecting wire 12 is connected with an external electrochemical workstation and used for accurately controlling current and voltage.
When the test platform is used, the sample platform main body 01 is flatly placed on an operation table, a little 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 tested electrodes, the diaphragm, the electrolyte, the other electrode slice, the gasket and the elastic sheet are sequentially assembled, then the sample platform main body lower cover 02 is installed, whether the O ring is clean or not is checked, and foreign matters are not detected, and the sample platform main body is fixed through the fixing nut 07. The sample table main body lower cover 02 is provided with a counter electrode connecting column 04 and a working electrode connecting column extending column 06. If the working electrode connecting column extending column 06 is composed of pogo probes, sealing is performed through sealant, and if the working electrode connecting column extending column 06 is composed of pogo probes, sealing gaskets and stainless steel columns, sealing can be performed through sealing gasket rings. And an O-ring is arranged between the counter electrode connecting column 04 and the lower cover 02 of the sample table main body for sealing. The three electrode connecting wires 12 are respectively formed by pogo probes and wire welding or physical contact, the three electrode connecting wires 12 are fixed on the electrode connecting wire fixing disc 10 through AB glue, and meanwhile, the magnet 11 is bonded on the electrode connecting wire fixing disc (10). The position of the magnet 11 on the electrode connecting wire fixing disc 10 is the same as the magnet 09 on the sample table main body lower cover 02, and the magnet mutually attracts through magnetism, so that the positioning effect is achieved, when the electrode connecting wire fixing disc 10 is used, the electrode connecting wire fixing disc 10 is close to the sample table main body lower cover 02, the pogo probe can stretch and retract through magnetic connection, and the magnetic connection is simultaneously connected with the counter electrode connecting column 04 on the sample table and the working electrode connecting column extending column 06. During electrochemical test, any working electrode connecting column extending column 06 is taken as a working electrode, and the electrode connecting column 04 is taken as a counter electrode and is connected into an electrochemical workstation. When the air tightness detection is needed, a working electrode connecting column extending column 06 can be installed firstly, 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 (8)
1. Electrochemical optical synchronous test sample platform which characterized in that: the sample table comprises a sample table main body (01), a sample table main body lower cover (02), a working electrode connecting column (03), the counter electrode connecting column (04), the insulating ring (05), the working electrode connecting column extending column (06), the fixing nut (07) and the window (08) form the main external structure of the sample table, a closed space is arranged in the sample table, can be used for placing a test electrode slice, a diaphragm, a gasket and a spring plate, an O ring is placed in a groove in the sample stage main body (01) for sealing, light can be transmitted through the window (08) and enters a material to be tested below the window, a lower counter bore placing magnet (09) is arranged on the sample stage main body lower cover (02), the electrode connecting wire fixing disc (10) is provided with three electrode connecting wires (12) which correspond to the working electrode connecting column extending column (06) and the counter electrode connecting column (04) respectively.
2. The electrochemical optical synchronous test sample stage of claim 1, wherein: the appearance and the size of the sample table main body (01) can be changed according to actual requirements.
3. The electrochemical optical synchronous test sample stage of claim 1, wherein: the sample stage is internally provided with a space for placing an electrode material, a diaphragm, a gasket and an elastic sheet, so that the electrode sheet is assembled in the sample stage in the same way as the button cell to obtain the electrochemical performance similar to that of the button cell, and the electrode material, the diaphragm, the gasket and the elastic sheet are assembled in an insulating ring (05), thereby being beneficial to the alignment of electrodes and avoiding short circuit.
4. The electrochemical optical synchronous test sample stage of claim 1, wherein: the working electrode connecting column extending column (06) can be composed of a pogo probe, or can also be composed of a pogo probe, a sealing gasket and a stainless steel column, wherein the pogo probe is sealed by a sealing glue, and the stainless steel column is sealed by a sealing gasket ring.
5. The electrochemical optical synchronous test sample stage of claims 1 and 4, wherein: the window (08) can be made of different materials and is suitable for different testing methods, meanwhile, the window (08) and the sample table main body (01) are sealed through vacuum grease, the window (08) and the insulating ring (05) can be tightly combined, and the sealing function is achieved.
6. The electrochemical optical synchronous test sample stage of claim 1, wherein: the pogo probe on the working electrode connecting column extending column (06) has certain elasticity, so that stable connection can be provided, and excessive extrusion damage to the window (08) can be avoided.
7. The electrochemical optical synchronous test sample stage of claim 1, wherein: the counter electrode connecting column (04) and the working electrode connecting column extending column (06) are all of a hidden design, and the main body of the electrode connecting column is hidden inside the main body of the sample table, so that the condition of short circuit caused by improper operation is reduced.
8. The electrochemical optical synchronous test sample stage of claim 1, wherein: the position of magnet (11) on the fixed disc of electrode connecting wire (10) is the same with the position of magnet (09) on sample platform main part lower cover (02), can pass through magnetism inter attraction, play the positioning action, it comprises pogo probe and electrode connecting wire respectively to have three electrode connecting wire (12) on the fixed disc of electrode connecting wire (10), it is corresponding with working electrode spliced pole extension post (06) and counter electrode spliced pole (04), it is corresponding with two sets of magnets during the use, just can be connected three electrode connecting wire (12) on the fixed disc of electrode connecting wire (10) with the electrode connecting post on the sample platform automatically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011433547.2A CN112697863B (en) | 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 | Electrochemical optical synchronous test sample table |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112697863A true CN112697863A (en) | 2021-04-23 |
| CN112697863B CN112697863B (en) | 2024-07-23 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070261958A1 (en) * | 2006-05-09 | 2007-11-15 | U.S.A. 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 |
| 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 |
| CN111830071A (en) * | 2019-04-14 | 2020-10-27 | 南杰智汇(深圳)科技有限公司 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070261958A1 (en) * | 2006-05-09 | 2007-11-15 | U.S.A. 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 |
| 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 |
| CN111830071A (en) * | 2019-04-14 | 2020-10-27 | 南杰智汇(深圳)科技有限公司 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
| 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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