CN107039694A - A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process - Google Patents
A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process Download PDFInfo
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- CN107039694A CN107039694A CN201710428608.8A CN201710428608A CN107039694A CN 107039694 A CN107039694 A CN 107039694A CN 201710428608 A CN201710428608 A CN 201710428608A CN 107039694 A CN107039694 A CN 107039694A
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000008569 process Effects 0.000 title claims abstract description 26
- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 25
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 239000011521 glass Substances 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 230000004888 barrier function Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910052594 sapphire Inorganic materials 0.000 claims description 4
- 239000010980 sapphire Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 125000006850 spacer group Chemical group 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 210000003739 neck Anatomy 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4285—Testing apparatus
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Primary Cells (AREA)
Abstract
The present invention provides a kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process, it includes being located at the housing on base, the junction of the base and housing is sealed by sealing ring, and the top end face of the housing is offered carries out sealed watch window with glass；The both sides of the housing are symmetrically threaded with positive conductive post, negative conductive post, and the positive conductive post stretches into the inside of housing, the other end with one end of negative conductive post and is connected respectively with the positive and negative electrode of power supply.The present invention coordinates SEM to observe and records the change of the interface in inferior pole piece electrochemical reaction process, and strong data and image foundation are provided for lithium ion battery type Selection Test.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of electrodes of lithium-ion batteries electrochemical reaction process
Observation device and method.
Background technology
Lithium ion battery has that energy density is big, power output is high, discharge and recharge long lifespan, cruising time length, pollution-free, work
Make many advantages, such as wide temperature range, small self discharge and environmental protection, be used as new high-energy chemistry power supply.In recent years, lithium
Ion battery is widely used in the fields such as mobile phone, computer and electric automobile.
Lithium-ion battery system is varied, to find the battery system being more suitable for, it is necessary to do substantial amounts of testing experiment, with
Detect the response situation of different battery systems.But because electrochemical reaction process belongs to microprocess, existing test mode is only
It can be judged by collecting the data such as the electric current in course of reaction, voltage, and the electrochemical reaction process between battery pole piece is nothing
What method was directly observed.
In order to solve the above problems, it is necessary to provide a kind of direct to the progress of electrodes of lithium-ion batteries electrochemical reaction process
The device and method of observation, to solve the problem of battery pole piece electrochemical reaction process can not be recorded.
The content of the invention
It is an object of the invention to solve the problems, such as the observation in lithium ion battery electrochemical reaction process and record, spy provides
A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process.
The present invention is achieved by the following technical solutions：
A kind of observation device of electrodes of lithium-ion batteries electrochemical reaction process, including the housing being located on base, the base
Sealed with the junction of housing by sealing ring, the top end face of the housing is offered carries out sealed observation window with glass
Mouthful；The both sides of the housing are symmetrically threaded with positive conductive post, negative conductive post, the positive conductive post and negative conductive
One end of post is stretched into the inside of housing, the other end and is connected respectively with the positive and negative electrode of power supply.
Further scheme, in addition to the supporting plate below base, housing top both sides are blocked respectively sets a clip,
The clip is fixedly connected by fixing bolt with supporting plate.
It is preferred that, in order that base is steady without producing displacement on the supporting plate, the center of the supporting plate is offered
The neck being engaged with the base bottom.
It is preferred that, in addition to the SEM above watch window, SEM can be by battery
Row is observed and is imaged during the electrochemical reaction process of pole piece.
Further scheme, the centre of the base opens up fluted, and horizontal direction has discharged negative pole successively in the groove
Conductive spacer, negative pole briquetting, negative plate, barrier film, positive plate, positive pole briquetting and positive conductive pad；The negative conductive post is stretched
The inside for entering housing is contacted with negative conductive pad；The positive conductive post stretches into the inside of housing and positive conductive pad connects
Touch.
It is flat that one end of further scheme, the positive conductive post and negative conductive post, which is provided with external screw thread, the other end,.
Further scheme, the both sides of the housing symmetrically offer the spiral shell for connecting positive conductive post, negative conductive post
Line through hole.
Further scheme, the top end face of the base and the bottom face of housing offer the sealing that sealing ring is put for card
Groove.
Further scheme, the negative conductive pad and positive conductive pad are elastomeric pad, and the sealing ring is resistance to
What corrosion material was made, the material of the housing is polytetrafluoroethylene (PTFE)；The glass of sealed watch window is sapphire glass.
Another goal of the invention of the present invention is to provide a kind of above-mentioned electrodes of lithium-ion batteries electrochemical reaction process
The observational technique of device is observed, it comprises the following steps：
A, by negative conductive pad of the same size, negative pole briquetting, negative plate, barrier film, positive plate, positive pole briquetting and positive conductive
Pad stacks be combined into test sample successively, is then placed in groove；
B, by electrolyte instill positive and negative plate between, unnecessary electrolyte oozes out from its bottom, stays in groove；
After c, the direction of the tapped through hole made on housing are consistent with the arragement direction of test sample, housing is fastened in test sample
On, so that test sample is located at the center of housing；And the top end face of bottom face and base is entered by sealing ring with making housing
Row crush seal；
D, negative conductive pad and positive conductive pad screwed in the tapped through hole on housing respectively, and stretch negative conductive post
The inside for entering housing is contacted with negative conductive pad, positive conductive post stretches into the inside of housing and contacted with positive conductive pad；And
Appropriateness extruding positive and negative electrode conductive pole, it is ensured that positive, negative electrode plate does not scatter；
E, clip card is placed on the housing of watch window both sides, clip is then fixed on supporting plate using fixing bolt
On；
F, the top that SEM is placed on to watch window；
G, the tail end that the positive and negative electrode clip of power supply is clamped in positive conductive post, negative conductive post respectively；Open battery after power supply
Pole piece starts electrochemical reaction, and SEM then records overall process.
Corrosion resistant sealing ring is arranged with the present invention between base and housing, when base is compressed with housing, sealing ring quilt
Extruding, full of the groove on base and housing, reaches sealing effectiveness；
Housing is made of polytetrafluoroethylene (PTFE), and its insulating properties is preferably and electrolyte resistance corrodes；One piece of blue treasured is inlayed at watch window
Stone glass, its translucency is preferably and electrolyte resistance corrodes；
Positive conductive post, negative conductive post by tapped through hole precession housing respectively with positive conductive pad, negative conductive pad
Contact, so as to reach the effect of conduction；
Positive conductive post, the tail end of negative conductive post are flat, are easy to the folder clamping of external power supply positive and negative power supply.
The present invention opens up watch window on the top of housing, and inlays one piece of preferable sapphire glass of translucency, improves
The observing effect of SEM；Battery pole piece is placed in housing by the present invention, is passed through using SEM
Watch window Real Time Observation and the electrochemical reaction process for recording battery pole piece, for test result provide detailed image according to
According to.So the present invention solves the problem of battery pole piece electrochemical reaction process is difficult record, and the assembling mode of the present apparatus
Also more convenient, safety, it is relatively low with simple in construction, manufacturing cost, the advantages of safe operation.
The present invention coordinates SEM to observe and records the change of the interface in inferior pole piece electrochemical reaction process, is
Lithium ion battery type Selection Test provides strong data and image foundation.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention；
Fig. 2 is Fig. 1 exploded perspective view.
In figure：1- bases, 2- sealing rings, 3- grooves, 4- negative conductive pads, 5- negative pole briquettings, 6- negative plates, 7- every
Film, 8- positive plates, 9- positive pole briquettings, 10- positive conductive pads, 11- negative conductive posts, 12- positive conductive posts, 13- screw threads lead to
Hole, 14- housings, 15- watch windows, 16- fixing bolts, 17- supporting plates, 18- clips, 19- necks.
Embodiment
Below in conjunction with the accompanying drawings the present invention is further illustrated with specific embodiment.
Embodiment one：
As shown in Figure 1, 2, a kind of observation device of electrodes of lithium-ion batteries electrochemical reaction process, including be located on base 1
Housing 14, the junction of the base 1 and housing 14 is sealed by sealing ring 2, and the top end face of the housing 14 is offered
Sealed watch window 15 is carried out with glass；The both sides of the housing 14 are symmetrically threaded with positive conductive post 12, negative pole and led
Electric post 11, one end of the positive conductive post 12 and negative conductive post 11 stretch into the inside of housing 14, the other end respectively with electricity
The positive and negative electrode connection in source.
Further scheme, in addition to the supporting plate 17 located at the lower section of base 1, the top both sides of housing 14 are blocked respectively sets one
Clip 18, the clip 18 is fixedly connected by fixing bolt 16 with supporting plate 17.
In order that base is steady without producing displacement on the supporting plate, the center of the supporting plate 17 offer with it is described
The neck 19 that the bottom of base 1 is engaged.
Also include the SEM located at the top of watch window 5（It is not drawn into figure）, SEM energy
The row during electrochemical reaction process of battery pole piece is observed and is imaged.
Further scheme, the centre of the base 1 opens up horizontal direction in fluted 3, the groove 3 and has discharged negative successively
Pole conductive spacer 4, negative pole briquetting 5, negative plate 6, barrier film 7, positive plate 8, positive pole briquetting 9 and positive conductive pad 10；It is described negative
The inside that pole conductive pole 11 stretches into housing 14 is contacted with negative conductive pad 4；The positive conductive post 12 stretches into the interior of housing 14
Portion is contacted with positive conductive pad 10.
It is flat that one end of further scheme, the positive conductive post 12 and negative conductive post 11, which is provided with external screw thread, the other end,
Flat-shaped, the tail end of its flat is easy to the folder clamping of external power supply positive and negative power supply.
Further scheme, the both sides of the housing 14 are symmetrically offered for connecting positive conductive post 12, negative conductive post
11 tapped through hole 13.
Further scheme, the top end face of the base 1 and the bottom face of housing 14 offer and put sealing ring 2 for card
Groove.
Further scheme, the negative conductive pad 4 and positive conductive pad 10 are elastomeric pad, the sealing ring 2
It is made for resistant material, the material of the housing 14 is polytetrafluoroethylene (PTFE), and its insulating properties is preferably and electrolyte resistance corrodes；It is close
The glass of the watch window 15 of envelope is sapphire glass, and its translucency is preferably and electrolyte resistance corrodes.
Corrosion resistant sealing ring is arranged with the present invention between base and housing, when base is compressed with housing, sealing ring quilt
Extruding, full of the groove on base and housing, reaches sealing effectiveness；Positive conductive post, negative conductive post pass through tapped through hole precession
Housing is contacted with positive conductive pad, negative conductive pad respectively, so as to reach the effect of conduction；When positive and negative electrode conductive pole with
When the both positive and negative polarity connection of power supply is powered, it is placed on the positive and negative plate energization in the middle of housing and is chemically reacted.
Embodiment two：
A kind of observational technique of the observation device of electrodes of lithium-ion batteries electrochemical reaction process, it comprises the following steps：
A, by negative conductive pad 4 of the same size, negative pole briquetting 5, negative plate 6, barrier film 7, positive plate 8, positive pole briquetting 9 and just
Pole conductive spacer 10 is stacked successively is combined into test sample, is then placed in groove 3；
B, by electrolyte instill positive and negative plate between, unnecessary electrolyte oozes out from its bottom, stays in groove 3；
C, the tapped through hole 13 made on housing 14 direction it is consistent with the arragement direction of test sample after, housing 14 is fastened in survey
On test agent, so that test sample is located at the center of housing 14；And lead to the top end face of the ground bottom face of housing 14 and base 1
Cross sealing ring 2 and carry out crush seal；
D, negative conductive pad 4 and positive conductive pad 10 screwed in the tapped through hole 13 on housing 14 respectively, and make negative pole
The inside that conductive pole 11 stretches into housing 14 is contacted with negative conductive pad 4, positive conductive post 12 stretch into the inside of housing 14 with just
Pole conductive spacer 10 is contacted；And moderately extruding positive and negative electrode conductive pole, it is ensured that positive, negative electrode plate does not scatter；
E, by clip 18 card be placed on the housing 14 of the both sides of watch window 15, then clip 18 is consolidated using fixing bolt 16
It is scheduled in supporting plate 17；
F, the top that SEM is placed on to watch window 15；
G, the tail end that the positive and negative electrode clip of power supply is clamped in positive conductive post 12, negative conductive post 11 respectively；Open after power supply
Battery pole piece starts electrochemical reaction, and SEM then records overall process.
Lithium-ion electric is observed and recorded under the larger visual field from the foregoing, may be implemented in using apparatus and method of the present invention
The course of reaction of pond pole piece electrochemistry, and overall process is recorded, detailed image foundation is provided for test result.In addition, this dress
Put simple in construction, assembling mode is also more convenient, safety, relatively low with simple in construction, manufacturing cost, the advantages of safe operation.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
In various modifications and improvement that case is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (10)
1. a kind of observation device of electrodes of lithium-ion batteries electrochemical reaction process, it is characterised in that：Including being located at base（1）On
Housing（14）, the base（1）And housing（14）Junction pass through sealing ring（2）Sealed, the housing（14）'s
Top end face is offered carries out sealed watch window with glass（15）；The housing（14）Both sides be symmetrically threaded with positive pole
Conductive pole（12）, negative conductive post（11）, the positive conductive post（12）With negative conductive post（11）One end stretch into housing
（14）Inside, the other end is connected with the positive and negative electrode of power supply respectively.
2. observation device according to claim 1, it is characterised in that：Also include being located at base（1）The supporting plate of lower section
（17）, the housing（14）Top both sides are blocked respectively sets a clip（18）, the clip（18）Pass through fixing bolt（16）With branch
Fagging（17）It is fixedly connected.
3. observation device according to claim 2, it is characterised in that：The supporting plate（17）Center offer and institute
State base（1）The neck that bottom is engaged（19）.
4. observation device according to claim 1, it is characterised in that：Also include being located at watch window（5）The scanning of top
Electron microscope.
5. observation device according to claim 1, it is characterised in that：The base（1）Centre open up fluted（3）,
The groove（3）Middle horizontal direction has discharged negative conductive pad successively（4）, negative pole briquetting（5）, negative plate（6）, barrier film（7）、
Positive plate（8）, positive pole briquetting（9）With positive conductive pad（10）；The negative conductive post（11）Stretch into housing（14）Inside
With negative conductive pad（4）Contact；The positive conductive post（12）Stretch into housing（14）Inside and positive conductive pad（10）
Contact.
6. observation device according to claim 1, it is characterised in that：The positive conductive post（12）With negative conductive post
（11）One end provided with external screw thread, the other end be flat.
7. observation device according to claim 1, it is characterised in that：The housing（14）Both sides symmetrically offer and be used for
Connect positive conductive post（12）, negative conductive post（11）Tapped through hole（13）.
8. observation device according to claim 1, it is characterised in that：The base（1）Top end face and housing（14）'s
Bottom face offers and puts sealing ring for card（2）Seal groove.
9. observation device according to claim 1, it is characterised in that：The negative conductive pad（4）With positive conductive pad
Piece（10）It is elastomeric pad, the sealing ring（2）It is made for resistant material, the housing（14）Material be polytetrafluoro
Ethene；Sealed watch window（15）Glass be sapphire glass.
10. a kind of observational technique of the observation device of electrodes of lithium-ion batteries electrochemical reaction process as claimed in claim 1,
It is characterized in that：Comprise the following steps：
A, by negative conductive pad of the same size（4）, negative pole briquetting（5）, negative plate（6）, barrier film（7）, positive plate（8）, just
Extreme pressure block（9）With positive conductive pad（10）Stack successively and be combined into test sample, be then placed in groove（3）In；
B, by electrolyte instill positive and negative plate between, unnecessary electrolyte oozes out from its bottom, stays in groove（3）In；
C, make housing（14）On tapped through hole（13）Direction it is consistent with the arragement direction of test sample after, by housing（14）Card
Cover on the test specimen, so that test sample is located at housing（14）Center；And make housing（14）Ground bottom face and base
（1）Top end face pass through sealing ring（2）Carry out crush seal；
D, by negative conductive pad（4）With positive conductive pad（10）Housing is screwed in respectively（14）On tapped through hole（13）In,
And make negative conductive post（11）Stretch into housing（14）Inside and negative conductive pad（4）Contact, positive conductive post（12）Stretch into
Housing（14）Inside and positive conductive pad（10）Contact；And moderately extrude positive and negative electrode conductive pole, it is ensured that positive, negative electrode plate
Do not scatter；
E, by clip（18）Card is placed on positioned at watch window（15）The housing of both sides（14）On, then using fixing bolt（16）Will
Clip（18）It is fixed on supporting plate（17）On；
F, SEM is placed on watch window（15）Top；
G, the positive and negative electrode clip of power supply is clamped in positive conductive post respectively（12）, negative conductive post（11）Tail end；Open electricity
Battery pole piece starts electrochemical reaction behind source, and SEM then records overall process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710428608.8A CN107039694A (en) | 2017-06-08 | 2017-06-08 | A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710428608.8A CN107039694A (en) | 2017-06-08 | 2017-06-08 | A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107039694A true CN107039694A (en) | 2017-08-11 |
Family
ID=59540824
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710428608.8A Pending CN107039694A (en) | 2017-06-08 | 2017-06-08 | A kind of observation device and method of electrodes of lithium-ion batteries electrochemical reaction process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107039694A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107706470A (en) * | 2017-11-20 | 2018-02-16 | 中国科学院化学研究所 | A kind of optical observation solid state battery interface detection device in situ |
| CN108286953A (en) * | 2018-01-30 | 2018-07-17 | 北京理工大学 | The test device of battery in-situ scanning electron microscope under a kind of multi- scenarios method |
| CN109860717A (en) * | 2019-01-23 | 2019-06-07 | 清华大学深圳研究生院 | A kind of in-situ Raman detection method of lithium ion battery and its dedicated lithium ion battery |
| CN111398825A (en) * | 2020-04-14 | 2020-07-10 | 中国科学院青岛生物能源与过程研究所 | Device and method for testing electrochemical performance of lithium battery and observing cross section morphology |
| CN113454443A (en) * | 2018-12-19 | 2021-09-28 | 韩国基础科学支援研究院 | In-situ optical and electrochemical analysis methods and cell profile measurement modules therefor |
| CN115078483A (en) * | 2022-06-24 | 2022-09-20 | 清华大学 | Electrochemical reactor for microscope observation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107706470A (en) * | 2017-11-20 | 2018-02-16 | 中国科学院化学研究所 | A kind of optical observation solid state battery interface detection device in situ |
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| CN113454443A (en) * | 2018-12-19 | 2021-09-28 | 韩国基础科学支援研究院 | In-situ optical and electrochemical analysis methods and cell profile measurement modules therefor |
| CN109860717A (en) * | 2019-01-23 | 2019-06-07 | 清华大学深圳研究生院 | A kind of in-situ Raman detection method of lithium ion battery and its dedicated lithium ion battery |
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| CN115078483B (en) * | 2022-06-24 | 2023-10-31 | 清华大学 | Electrochemical reactor for microscope observation |
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Application publication date: 20170811 |
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