CN112945856A - Optical in-situ observation method for variable-temperature charging and discharging of lithium ion experimental battery - Google Patents
Optical in-situ observation method for variable-temperature charging and discharging of lithium ion experimental battery Download PDFInfo
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- CN112945856A CN112945856A CN202110207819.5A CN202110207819A CN112945856A CN 112945856 A CN112945856 A CN 112945856A CN 202110207819 A CN202110207819 A CN 202110207819A CN 112945856 A CN112945856 A CN 112945856A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
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Abstract
The invention discloses a temperature-changing charge-discharge optical in-situ observation method for a lithium ion experimental battery. The invention comprises the following steps: exposing the main body part of an experimental battery pole group at the upper end of a T-shaped observation battery clamp, taking down the cut pole group for liquid injection and negative pressure standing, packaging the experimental battery after liquid injection by using a transparent PE film, attaching a silica gel sheet with moderate cutting size to one side of the observation clamp, placing the experimental battery packaged by using the PE film in an observation device, placing the battery clamp in a middle cavity, respectively connecting the observation tool with formation charge-discharge equipment, a temperature monitor and high-magnification optical microscope objective table for observation focal length adjustment, and opening and circulating the inside of the observation tool for cooling or heating when the temperature reaches a set value. The invention solves the problem that the optical in-situ observation technology of the lithium ion experimental battery can not carry out observation at variable temperature.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a variable-temperature charging and discharging in-situ observation method for a lithium battery.
Background
In recent years, lithium ion batteries are widely used due to the characteristics of high specific energy, high environmental protection, long cycle life and the like, and particularly in the fields of new energy automobiles, energy storage systems and 3C products, with the continuous improvement of technologies in the industry, the research on the lithium ion batteries is also carried out from external electrical property tests to internal mechanism studies in the lithium embedding process in consideration of harsh environmental requirements (such as high and low temperature environments) in practical application.
The existing technologies for in-situ observation of lithium ion batteries during charging and discharging processes include: the device can realize the observation of in-situ charging and discharging of the in-situ lithium ion battery, but cannot perform optical detection in the circulating process; in addition, although the device (CN 208111618U) for in-situ Raman monitoring in the battery cycle process can carry out the test of the lithium ion battery cycle process, the visual observation in the cycle process and the lithium intercalation observation cannot be carried out; while the in-situ observation tool machine method (CN 110967343 a) relative to the battery cycle process can perform visual observation of the lithium ion battery during the cycle process, the observation for different temperature conditions cannot be performed only at normal temperature.
Disclosure of Invention
The invention aims to overcome the defects of the technology and provide a charge-discharge in-situ observation method of a lithium ion experimental battery at different temperatures.
The invention adopts the following technical scheme for realizing the purpose:
a temperature-changing charge-discharge optical in-situ observation method for a lithium ion experimental battery comprises the following steps:
(1) exposing the main body part of an experimental battery pole group at the upper end of a T-shaped observation battery clamp, and clamping and fastening the main body part through fastening bolts at two sides of the clamp, wherein the T-shaped observation battery clamp comprises a T-shaped left clamping block, a T-shaped right clamping block and a U-shaped cooling pipe, the U-shaped cooling pipe is respectively inserted into the T-shaped left clamping block and the T-shaped right clamping block, positioning pins are positioned at two sides of the top end of the left clamping block and are inserted into positioning holes in the right clamping block to realize positioning, two ends of the T-shaped left clamping block and the T-shaped right clamping block are respectively fixed through the fastening bolts, flatly cutting a battery along the upper end surface of the clamp, sticking out floating and sinking particles by using an aluminum rubber belt, ensuring that the section of the experimental battery pole group is smooth, flat;
(2) taking down the cut pole group, injecting liquid, and standing at negative pressure to ensure that the pole piece is fully soaked by electrolyte;
(3) packaging the experimental battery after liquid injection by using a transparent PE film;
(4) a silica gel sheet with a moderate cutting size is attached to one side of the observation clamp, so that the upper edge is flush with the edge of the top end of the clamp;
(5) placing an experimental battery packaged by a PE film in an observation device, wherein the observation device comprises an observation window, a battery clamp, a middle cavity and a lower cavity; the observation window is connected with the upper end surface of the middle cavity in a sealing and fastening way through a sealing ring and a bolt; the lower end surface of the middle cavity is hermetically and fixedly connected with the lower cavity body through a sealing ring and a bolt; connecting the anode and cathode lugs of the experimental battery with the red and black wires in the middle cavity of the observation fixture respectively, and coating and binding the anode and cathode lugs by using an insulating tape to ensure that the top end (excluding the PE film) of the battery body is flush with the top end of the observation fixture, and clamping and fastening the anode and cathode lugs;
(6) the battery clamp is placed in the middle cavity, the lower end face of the battery clamp is tightly attached to the floating plate of the lower cavity, the upper end face of the battery clamp is tightly attached to the ultra-white glass of the observation window, the top cover is covered to ensure that the ultra-white glass plate of the observation top cover is tightly contacted with the top end of the observation clamp, and the fastening bolt of the top cover is tightened;
(7) respectively connecting the observation tool with formation charging and discharging equipment (a red and black lead corresponds to a positive electrode and a negative electrode), a temperature monitor (a temperature probe plug) and temperature changing equipment (a cooling liquid conduit), and placing the observation tool on a high-magnification optical microscope objective table for observation focal length adjustment;
(8) filling the cooling liquid into a temperature-changing equipment water tank, and setting the required temperature to cool or heat the cooling liquid;
(9) when the temperature reaches a set value (the temperature of the cooling liquid of the temperature changing equipment), opening circulation to cool or heat the interior of the observation tool;
(10) air blowing is applied to the observation surface of the ultra-white glass plate of the observation tool by using an air compressor, so that the observation surface is prevented from dewing;
(11) when the temperature is kept at the required temperature (the temperature is displayed by the monitor), the phenomena of lithium intercalation and lithium deintercalation of the negative electrode in the charging and discharging process of the lithium ion battery are observed by using a high-magnification optical microscope, so that the visual observation in the charging and discharging process of the lithium ion battery is realized.
Preferably, the size of the part of the experimental battery pole group exposed in the step (1) is less than or equal to 5 mm.
Preferably, the negative pressure standing condition in the step (2) is-90 KPa and 90 min.
Preferably, after the experimental battery is packaged by the PE film in the step (3), the width is required to be less than or equal to 35 mm.
Preferably, the size of the silicone sheet in the step (4) is 15mm × 35mm × 1mm, so that the experimental battery can be completely covered.
Preferably, the cooling liquid in the step (8) is a solution prepared by mixing ethylene glycol and water according to a ratio of 3: 2.
The invention has the beneficial effects that: the problem that the optical in-situ observation technology of the lithium ion experimental battery cannot observe at variable temperature is solved; because the liquid is encapsulated again by the PE film after the liquid injection is static, the volatilization amount of the electrolyte is reduced, and the problem that the research of the optical in-situ observation technology of the lithium ion experimental battery cannot be circulated for many times is solved; meanwhile, the sample battery prepared by the method has high observation picture definition, simple and convenient process and high repeatability, and is suitable for the research of the optical in-situ observation technology of the lithium ion experimental battery.
Drawings
FIG. 1 is a schematic view of a fixture tool after sectioning an experimental battery according to the present invention;
fig. 2 is an overall schematic view of the observation tool.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in figure 1, the T-shaped observation battery clamp comprises a T-shaped left clamping block 1, a T-shaped right clamping block 2 and a U-shaped cooling pipe 4, the U-shaped cooling pipe 4 is respectively inserted into the T-shaped left clamping block 1 and the T-shaped right clamping block 2, positioning pins 5 are positioned at two sides of the top end of the left clamping block and are inserted into positioning holes in the right clamping block to realize positioning, and two ends of the T-shaped left clamping block 1 and two ends of the T-shaped right clamping block 2 are respectively fixed through fastening bolts 3.
As shown in fig. 2, the device suitable for in-situ observation of high and low temperatures of a lithium ion battery comprises an observation window 6, a battery clamp (fig. 1), a middle cavity 7 and a lower cavity 8; the observation window is connected with the upper end surface of the middle cavity in a sealing and fastening way through a sealing ring and a bolt; the lower end surface of the middle cavity is hermetically and fixedly connected with the lower cavity body through a sealing ring and a bolt; the battery clamp is placed in the middle cavity, the lower end face of the battery clamp is tightly attached to the floating plate of the lower cavity, and the upper end face of the battery clamp is tightly attached to the ultra-white glass of the observation window. The U-shaped cooling pipes are respectively inserted into the T-shaped left clamping block body and the T-shaped right clamping block body and are used for heat conduction of the whole device.
A temperature-changing charge-discharge optical in-situ observation method for a lithium ion experimental battery comprises the following steps:
(1) placing an experimental battery pole group between a left clamping block 1 and a right clamping block 2 of a T-shaped observation battery clamp, exposing a battery body 4mm from the upper end of the clamp, tightening a fastening bolt 3 for fixing, flatly cutting the battery along the upper end surface of the clamp by using a hard alloy cutter, and sticking out floating and sinking particles by using an aluminum skin adhesive tape to ensure that the section of the experimental battery pole group is smooth, flat and undamaged and is used as an observation surface for variable-temperature charging and discharging of the battery;
(2) taking down the cut pole group, injecting liquid, and standing under negative pressure for (-90 KPa, 90 min) to ensure that the pole piece is fully soaked by the electrolyte;
(3) packaging the experimental battery after liquid injection by using a transparent PE film, wherein the width of the experimental battery is less than or equal to 35 mm;
(4) the method comprises the following steps that a silica gel sheet with a moderate cutting size is attached to one side of an observation clamp, the size of the silica gel sheet is 15mm multiplied by 35mm multiplied by 1mm, the experimental battery can be completely coated, and meanwhile, the upper edge is enabled to be flush with the edge of the top end of the clamp;
(5) placing an experimental battery packaged by a PE film in an observation fixture tool, respectively connecting positive and negative lugs of the experimental battery with a red and black lead in a cavity of the observation tool, and wrapping and binding the positive and negative lugs by using an insulating adhesive tape to ensure that the top end (excluding the PE film) of the battery body is flush with the top end of the observation fixture tool, and clamping and fastening the battery body;
(6) placing the fixture tool in an observation tool cavity, covering a top cover to ensure that the ultra-white glass plate of the observation top cover is in close contact with the top end of the observation fixture, and screwing a fastening bolt of the top cover;
(7) respectively connecting the observation tool with formation charging and discharging equipment (a red and black lead corresponds to a positive electrode and a negative electrode), a temperature monitor (a temperature probe plug) and temperature changing equipment (a cooling liquid conduit), and placing the observation tool on a high-magnification optical microscope objective table for observation focal length adjustment;
(8) filling cooling liquid (the cooling liquid is prepared by glycol and water according to the volume ratio of 3: 2) into a water tank of a temperature changing device, and setting the required temperature to cool (heat) the cooling liquid;
(9) when the temperature reaches a set value (the temperature of the cooling liquid of the temperature changing equipment), opening circulation to cool (heat) the interior of the observation tool;
(10) air blowing is applied to the observation surface of the ultra-white glass plate of the observation tool by using an air compressor, so that the observation surface is prevented from dewing;
(11) when the temperature is kept at the required temperature (the temperature is displayed by the monitor), the phenomena of lithium intercalation and lithium deintercalation of the negative electrode in the charging and discharging process of the lithium ion battery are observed by using a high-magnification optical microscope, so that the visual observation in the charging and discharging process of the lithium ion battery is realized.
The above description is only a preferred embodiment of the present invention, and it should be understood that those skilled in the art can make various modifications and improvements without departing from the principle of the present invention, and such modifications and improvements should be considered as the protection scope of the present invention.
Claims (4)
1. A temperature-changing charge-discharge optical in-situ observation method for a lithium ion experimental battery is characterized in that: the method comprises the following steps:
(1) exposing the main body part of an experimental battery pole group at the upper end of a T-shaped observation battery clamp, and clamping and fastening the main body part through fastening bolts at two sides of the clamp, wherein the T-shaped observation battery clamp comprises a T-shaped left clamping block, a T-shaped right clamping block and a U-shaped cooling pipe, the U-shaped cooling pipe is respectively inserted into the T-shaped left clamping block and the T-shaped right clamping block, positioning pins are positioned at two sides of the top end of the left clamping block and are inserted into positioning holes in the right clamping block to realize positioning, two ends of the T-shaped left clamping block and the T-shaped right clamping block are respectively fixed through the fastening bolts, flatly cutting a battery along the upper end surface of the clamp, sticking out floating and sinking particles by using an aluminum rubber belt, ensuring that the section of the experimental battery pole group is smooth, flat;
(2) taking down the cut pole group, injecting liquid, and standing at negative pressure to ensure that the pole piece is fully soaked by electrolyte;
(3) packaging the experimental battery after liquid injection by using a transparent PE film;
(4) a silica gel sheet with a moderate cutting size is attached to one side of the observation clamp, so that the upper edge is flush with the edge of the top end of the clamp;
(5) placing an experimental battery packaged by a PE film in an observation device, wherein the observation device comprises an observation window, a battery clamp, a middle cavity and a lower cavity; the observation window is connected with the upper end surface of the middle cavity in a sealing and fastening way through a sealing ring and a bolt; the lower end surface of the middle cavity is hermetically and fixedly connected with the lower cavity body through a sealing ring and a bolt; the top end of the battery body, excluding the PE film, is ensured to be flush with the top end of the observation fixture tool and clamped and fastened;
(6) the battery clamp is placed in the middle cavity, the lower end face of the battery clamp is tightly attached to the floating plate of the lower cavity, the upper end face of the battery clamp is tightly attached to the ultra-white glass of the observation window, the top cover is covered to ensure that the ultra-white glass plate of the observation top cover is tightly contacted with the top end of the observation clamp, and the fastening bolt of the top cover is tightened;
(7) respectively connecting the observation tool with cooling liquid guide pipes of formation charging and discharging equipment, a temperature monitor and temperature changing equipment, and placing the observation tool on an objective table of a high-magnification optical microscope;
(8) opening a temperature changing device to set a required temperature for cooling or heating the interior of the observation tool;
(9) air blowing is applied to the observation surface of the ultra-white glass plate of the observation tool by using an air compressor, so that the observation surface is prevented from dewing;
(10) and displaying the temperature by using a monitor, and performing visual observation on the lithium ion battery in the charging and discharging process by using a high-magnification optical microscope when the temperature is kept at the required temperature.
2. The method for observing the temperature-varying charge-discharge optical in-situ of the lithium ion experimental battery as claimed in claim 1, wherein: the size of the exposed experimental battery pole group part in the step (1) is less than or equal to 5 mm.
3. The method for observing the temperature-varying charge-discharge optical in-situ of the lithium ion experimental battery as claimed in claim 1, wherein: and (3) in the step (2), the negative pressure standing condition is-90 KPa and 90 min.
4. The method for observing the temperature-varying charge-discharge optical in-situ of the lithium ion experimental battery as claimed in claim 1, wherein: the silicone sheet size in step (4) was 15mm x 35mm x 1mm, ensuring that the experimental cells were fully encapsulated.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114235865A (en) * | 2021-11-19 | 2022-03-25 | 华南理工大学 | Temperature-controllable lithium battery in-situ X-ray diffraction spectrum testing device |
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- 2021-02-25 CN CN202110207819.5A patent/CN112945856A/en active Pending
Patent Citations (6)
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| 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 |
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| CN114235865A (en) * | 2021-11-19 | 2022-03-25 | 华南理工大学 | Temperature-controllable lithium battery in-situ X-ray diffraction spectrum testing device |
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