CN108286953A - The test device of battery in-situ scanning electron microscope under a kind of multi- scenarios method - Google Patents
The test device of battery in-situ scanning electron microscope under a kind of multi- scenarios method Download PDFInfo
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- CN108286953A CN108286953A CN201810088127.1A CN201810088127A CN108286953A CN 108286953 A CN108286953 A CN 108286953A CN 201810088127 A CN201810088127 A CN 201810088127A CN 108286953 A CN108286953 A CN 108286953A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
- G01B15/06—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring the deformation in a solid
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- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/225—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 measuring secondary emission from the material using electron or ion
- G01N23/2251—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 measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
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Abstract
The present invention relates to a kind of in-situ test of battery failure mechanism, more particularly to the test device of battery in-situ scanning electron microscope, belongs to battery in-situ characterization field under a kind of multi- scenarios method.For applying different temperature to battery the deformation information for monitoring battery cross sectional at different temperatures may be implemented, to analyze the failure mechanism of battery in device.Including：Load battery test system or wide temperature original position battery test system and mechanics load battery test system in situ in situ for wide temperature original position battery test system, mechanics；The present invention can also apply the effect of different external forces while can applying different temperature to battery, so as to so that the test environment of battery closer to actual running environment, so as to more acurrate analysis battery failure mechanism in different environments, to instruct battery commercially produce and subsequent research.
Description
Technical field
The present invention relates to a kind of in-situ test of battery failure mechanism, more particularly to battery is swept in situ under a kind of multi- scenarios method
The test device for retouching electron microscope belongs to battery in-situ characterization field.
Background technology
With the worsening shortages of fossil energy, novel renewable energy is developed into hot spot of people's attention.And it is secondary
Battery is as a kind of carrier of clean energy resource, because the advantages that its energy density height, good cycle, clean environment firendly is widely used in
The every field such as telecommunications, rail traffic, aerospace are the huge non-polluting energy sources of new generation of development potentiality.However,
Under some extreme environments (high/low temperature, external force, impact force), battery performance deteriorates, and body occurs in cell operation
Phenomena such as product expansion and deformation, these problems all seriously hinder the development of field of batteries.Therefore, battery structure is monitored in real time
It is highly important to change and carry out assessment to its state.
Currently, a small number of domestic and foreign scholars are seen with electron scanning Electronic Speculum (Scan electron microscope, SEM) in situ
Examine the deformation of lithium battery silicon-carbon cathode and graphite cathode under room temperature, realize under room temperature environment battery electrode surface change information and
Section deformation problem.But it is a lack of the in situ measurement battery Microstructure evolution and table of battery actual motion environment (- 40~60 DEG C)
Levy evaluation method；Also some domestic scholars are swollen with light microscope in situ and three-dimensional optical imaging test monomer test volume
Swollen problem, but it is a lack of in-situ mechanical load-on module.Existing original position Electron Microscopy can only monitor at normal temperatures and pressures
The case where battery operation, lacks the operating condition analysis under working battery actual temperature and is transported in different Mechanical loading batteries
The actual motion environment of the monitoring of row failure conditions, current monitoring technology and battery has very big difference, leads to the mistake to battery
It is inaccurate to imitate Analysis on Mechanism.
Invention content
The purpose of the present invention is to solve the prior arts there is a problem of that detection is inaccurate, provides under a kind of multi- scenarios method
The test device of battery in-situ scanning electron microscope.The device can be realized in different electrochemical fields, temperature field and difference
Battery Microstructure evolution and the in-situ test of performance deterioration under outer force effect.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：
The test device of battery in-situ scanning Electronic Speculum can for applying different temperature to battery under a kind of multi- scenarios method
To realize the deformation information for monitoring battery cross sectional at different temperatures, to analyze the failure mechanism of battery.Including：Thermal module
Pedestal, battery clamp, thermostat, temperature sensor bed course, copper heat radiation plate device and adiabatic bakelite module；
Battery clamp is for fixed tested battery；Battery clamp, thermostat and temperature sensor bed course contact successively, and
It is fixed by screw, device after being fixed；Between device after fixation is placed in two copper heat radiation plate devices, and radiated by copper
Panel assembly is fixed；Copper heat radiation plate device is fixed on thermal module pedestal；Groove is opened up at the thermal module base center, it is recessed
Adiabatic bakelite module is placed at slot；Blind hole is opened up on copper heat radiation plate device, for connecting with the flange of scanning electron microscope device
It connects, so that scanning electron microscope device can constantly detect tested battery；
The thermal module pedestal is conductive aluminium sheet；The thermostat is cooling piece；
The course of work：Tested battery is clamped with battery clamp, then battery is applied by thermostat (cooling piece)
Different temperatures, and the temperature of battery ambient is monitored by temperature sensor bed course, need copper to dissipate during thermostat
Hot plate apparatus is connected with the cavity of scanning electron microscope to cool down it to reach the constant of battery ambient temperature.By this
Device is placed into the microscopical cavity of Scanning Electron, charge-discharge test is carried out to battery, then in battery charge and discharge process
Section carry out in real time monitoring take pictures.Image (loading by means of digital image correlation method (the DIC- that the monitoring of Scanning Electron microscope is collected
Digital Image Correlation) analyzing processing is carried out, the information that battery quantitatively deforms can be obtained.
The test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method, for battery apply it is different it is outer carry power, can
The failure mechanism of battery under the action of carrying outside difference power with realization battery.Including：Mechanics module pedestal, battery clamp top
Block, guide rail, servo motor, sliding screw and mechanics sensor.
Mechanics module pedestal is U-shaped structure, guide rail is provided at bottom surface, so that battery clamp jacking block can be slided along guide rail
It is dynamic；Battery clamp jacking block is for fixed tested battery；One battery clamp jacking block is fixed by sliding screw and servo motor；Separately
One battery clamp jacking block is fixedly connected with mechanics sensor；
The course of work：Fix tested battery with battery clamp jacking block, according to servo motor drive sliding screw to
Driving battery clamp jacking block is moved by guide rail.Apply different external force to battery by different moving displacements, external force it is big
It is small to be monitored in real time by mechanics sensor.This device is placed into the microscopical cavity of Scanning Electron, battery is carried out
Then charge-discharge test carries out monitoring in real time to the section in battery charge and discharge process and takes pictures.Obtained image information (number
DIC Method (DIC-Digital Image Correlation) carries out analyzing processing, can obtain what battery quantitatively deformed
Information.
Wide temperature original position battery test system is placed into the battery clamp top in mechanics original position load battery test system
Block position can realize the effect of different temperatures and different external forces to being tested battery simultaneously.Then device is placed into surface sweeping
In the cavity of electron microscope, charge-discharge test is carried out to battery, then the section in battery charge and discharge process is carried out real-time
Monitoring is taken pictures.Obtained image information is with (loading by means of digital image correlation method (DIC-Digital Image Correlation) is divided
Analysis is handled, and can obtain quantitative deformation information of the battery under different temperature fields and external fields of force effect.
Advantageous effect
(1) a kind of device of in-situ monitoring cell deformation failure is provided, while different temperature can be applied to battery
The effect that different external forces can also be applied, so as to so that the test environment of battery closer to actual running environment, with
Just more acurrate analysis battery failure mechanism in different environments, to instruct commercially producing and subsequent grinding for battery
Study carefully.
(2) it realizes for the first time under wide temperature range, the Microstructure evolution and performance degradation phenomena of in-situ test battery,
Battery actual work temperature range is improved for research, and strong evidence is provided；
(3) this device realize outside difference carry power under the action of to battery carry out Real Time Monitoring Microstructure evolution with
And performance degradation phenomena, provide strong support for battery actual production and research；
(4) this device can be while real by applying the effects of different external forces to wide temperature original position battery test system
Now to the regulation and control in the temperature field of battery and external load field.
(5) this device can also load battery test system outside applies different temperature in situ by mechanics, while real
Now to the regulation and control in the temperature field of battery and external load field.
(6) a kind of method of SEM+DIC binding analysis cell deformation information is established.
Description of the drawings
Fig. 1 is wide temperature original position battery test system；
Fig. 2 is mechanics load battery test system in situ；
Fig. 3 is the computational methods that SEM+DIC is combined；
Fig. 4 is the schematic diagram that example 1SEM scanning patters pass through DIC processing.
In figure：1- thermal module pedestals；2- battery clamps；3- thermostats；4- temperature sensor bed courses；5- copper heat sinks
Device；6- thermal insulation bakelite modules；7- mechanics sensors；8- mechanics module pedestals；9- battery clamp jacking blocks；10- guide rails；11- is watched
Take motor；12- sliding screws.
Specific implementation mode,
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Mesuring battary：Lithium ion battery
Device：As shown in Figure 1, battery clamp 2 is for fixed tested battery；Battery clamp 2, thermostat 3 and temperature pass
Sensor bed course 4 contacts successively, and is fixed by screw, device after being fixed；It is 12 that device after fixation, which is placed in standoff distance,
Between two copper heat radiation plate devices 5 of ± 0.05mm, and fixed by copper heat radiation plate device；Copper heat radiation plate device is fixed on temperature mould
On block pedestal；Groove is opened up at 1 center of thermal module pedestal, groove places adiabatic bakelite module 6；Copper heat radiation plate device
On open up blind hole, for flanged joint with scanning electron microscope device, so that scanning electron microscope device can be to quilt
Battery is surveyed constantly to be detected.
The course of work：
Step 1：It is in water oxygen content<Lithium ion battery is assembled in the glove box of the argon atmosphere of 0.1ppm, battery is placed
In battery clamp 2, fixed with nut；
Step 2：Battery clamp 2 is fixedly connected with thermostat 3 and temperature sensor bed course device 4 by nut
Together；
Step 3：The above-mentioned device fixed is placed among two copper heat radiation plate devices 5, two copper heat radiation plate devices
Distance be 12 ± 0.05mm, then step up to fix, bottom has thus been assembled into wide temperature there are one adiabatic bakelite module 6
Spend battery in-situ test system
Step 4：Wide temperature battery in-situ test system is placed into Scanning Electron scope lumen body, then by blind
Copper heat radiation plate device 5 is connected by hole with the flange of cavity；
Step 5：Apply different temperature to assembled cell apparatus：- 20 degree, -10 degree, 0 degree, 10 degree, 20 degree, 30
Degree, 40 degree, 50 degree, 60 degree；
Step 6：Under a certain temperature environment of above-mentioned fixation, battery is subjected to charge-discharge test with new prestige tester, then
With scanning electron microscope to battery charge and discharge process, real-time image acquisition information is carried out to the section of battery under certain multiplying power
Step 7：The image information of acquisition is analyzed, and combines the deformation in chemical property tracing analysis image
Information；According to the method for Fig. 3, the image collected is carried out using DIC softwares to calculate the deformation failure in analysis battery operation
Mechanism, obtained result schematic diagram such as Fig. 4.
Step 8：Speckle makes, and 10ml alcohol and 2g hexagonal boron nitrides (1-2 microns of grain size) powder are mixed, and makes nothing
Machine solution, it is contemplated that powder particle can also reunite in the solution, so using ultrasonic vibration so that in alcoholic solution
Even point is let go.Mixed solution is random, it is coated on cathode section, nanometer powder is attached to electrode sections after drying, and SEM measures aobvious
Show that lower hexagonal boron nitride and graphitic carbon point are shown as white and black, forms nature black and white speckle.(D=50 μm of cathode granularity：
Si：5.4；Graphite：10.61；Boron nitride particle is in 2 microns)
Step 9：Then the sample assembly that step 8 is obtained carries out test point at battery according to step 1 to step 7
Analysis.
Embodiment 2
Mesuring battary：Lithium ion battery
Device：As shown in Fig. 2, mechanics module pedestal 8 is U-shaped structure, it is provided with guide rail 10 at bottom surface, so as to battery clamp
Jacking block 9 can be slided along guide rail 10；Battery clamp jacking block 9 is for fixed tested battery；One battery clamp jacking block passes through sliding
Screw rod 11 is fixed with servo motor 12；Another battery clamp jacking block 9 is fixedly connected with mechanics sensor 7；
The course of work：
Step 1：It is in water oxygen content<Lithium ion battery is assembled in the glove box of the argon atmosphere of 0.1ppm, battery is placed
In battery clamp jacking block 9, gum down；
Step 2：Battery is connect with new prestige tester, entire system of testing is connect with computer
Step 3：The size control servomotor that external force is arranged by computer drives sliding screw 11 to drive battery
Fixture jacking block 9 is moved by guide rail 10, to realize the load of power；
Step 4：Apply the effect of different external forces to battery：0N-5000N is tested every 100N
Step 5：Under a certain external force of above-mentioned fixation, battery is subjected to charge-discharge test with new prestige tester, is then used
Scanning electron microscope carries out real-time image acquisition information under certain multiplying power to battery charge and discharge process to the section of battery
Step 6：The image information of acquisition is analyzed, and combines the deformation in chemical property tracing analysis image
Information；According to the method for Fig. 3, the image collected is carried out using DIC softwares to calculate the deformation failure in analysis battery operation
Mechanism.
Step 7：Speckle makes, and 10ml alcohol and 2g hexagonal boron nitrides (1-2 microns of grain size) powder are mixed, and makes nothing
Machine solution, it is contemplated that powder particle can also reunite in the solution, so using ultrasonic vibration so that in alcoholic solution
Even point is let go.Mixed solution is random, it is coated on cathode section, nanometer powder is attached to electrode sections after drying, and SEM measures aobvious
Show that lower hexagonal boron nitride and graphitic carbon point are shown as white and black, forms nature black and white speckle.(D=50 μm of cathode granularity：
Si：5.4；Graphite：10.61；Boron nitride particle is in 2 microns)
Step 8：Then the sample assembly that step 7 is obtained carries out test point at battery according to step 1 to step 6
Analysis.
Embodiment 3
Mesuring battary：Lithium ion battery
Device：Fig. 1 shown devices are placed into Fig. 2 shown devices, different temperatures then is realized to mesuring battary simultaneously
Field and the regulation and control for applying different force field.
The course of work：
Step 1：It is in water oxygen content<Lithium ion battery is assembled in the glove box of the argon atmosphere of 0.1ppm, is placed on figure
In device shown in 1；
Step 2：The device of Fig. 1 is placed into the device of Fig. 2
Step 3：Battery is connect with new prestige tester, entire system of testing is connect with computer
Step 3：The size control servomotor that external force is arranged by computer drives sliding screw to drive battery folders
Tool jacking block is moved by guide rail, to realize the load of power；
Step 4：By Fig. 1 devices, the control of different temperatures is realized to battery, -20 degree, -10 spend, 0 degree, 10 degree, and 20
Degree, 30 degree, 40 degree, 50 degree, 60 degree；
Step 5：Under a certain external force of above-mentioned fixation, temperature is adjusted, battery is subjected to charge and discharge electrical measurement with new prestige tester
Examination, then acquires the section of battery under certain multiplying power battery charge and discharge process with scanning electron microscope in real time
Image information
Step 6：At a certain temperature of above-mentioned fixation, external force is adjusted, battery is subjected to charge and discharge electrical measurement with new prestige tester
Examination, then acquires the section of battery under certain multiplying power battery charge and discharge process with scanning electron microscope in real time
Image information
Step 7：The image information of acquisition is analyzed, and combines the deformation in chemical property tracing analysis image
Information；According to the method for Fig. 3, the image collected is carried out using DIC softwares to calculate the deformation failure in analysis battery operation
Mechanism.
Above-described specific descriptions have carried out further specifically the purpose, technical solution and advantageous effect of invention
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection domain within.
Claims (7)
1. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method, it is characterised in that：Including：Thermal module pedestal,
Battery clamp, thermostat, temperature sensor bed course, copper heat radiation plate device and adiabatic bakelite module；
Battery clamp is for fixed tested battery；Battery clamp, thermostat and temperature sensor bed course contact successively, and pass through
Screw is fixed, device after being fixed；Between device after fixation is placed in two copper heat radiation plate devices, and filled by copper heat sink
Set fixation；Copper heat radiation plate device is fixed on thermal module pedestal；Groove, groove are opened up at the thermal module base center
Place adiabatic bakelite module；Blind hole is opened up on copper heat radiation plate device, is used for the flanged joint with scanning electron microscope device, with
Just scanning electron microscope device can constantly detect tested battery.
2. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method, it is characterised in that：Including：Mechanics module pedestal,
Battery clamp jacking block, guide rail, servo motor, sliding screw and mechanics sensor；Mechanics module pedestal is U-shaped structure, at bottom surface
It is provided with guide rail, so that battery clamp jacking block can be slided along guide rail；Battery clamp jacking block is for fixed tested battery；One electricity
Pond fixture jacking block is fixed by sliding screw and servo motor；Another battery clamp jacking block is fixedly connected with mechanics sensor.
3. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method, it is characterised in that：Including：Wide temperature original position battery
Test system and mechanics load battery test system in situ；Temperature-adjusting device and pressure-regulating device；The wide temperature is former
Position battery test system is placed on the mechanics and loads on battery test system in situ, and battery testing is loaded in situ by the mechanics
The battery clamp jacking block of system is clamped；
The temperature-adjusting device includes：Thermal module pedestal, battery clamp, thermostat, temperature sensor bed course, copper heat dissipation
Panel assembly and adiabatic bakelite module；
Battery clamp is for fixed tested battery；Battery clamp, thermostat and temperature sensor bed course contact successively, and pass through
Screw is fixed, device after being fixed；Between device after fixation is placed in two copper heat radiation plate devices, and filled by copper heat sink
Set fixation；Copper heat radiation plate device is fixed on thermal module pedestal；Groove, groove are opened up at the thermal module base center
Place adiabatic bakelite module；Blind hole is opened up on copper heat radiation plate device, is used for the flanged joint with scanning electron microscope device, with
Just scanning electron microscope device can constantly detect tested battery；
The pressure-regulating device includes：Mechanics module pedestal, battery clamp jacking block, guide rail, servo motor, sliding screw and power
Learn sensor；Mechanics module pedestal is U-shaped structure, guide rail is provided at bottom surface, so that battery clamp jacking block can be slided along guide rail
It is dynamic；Battery clamp jacking block is for fixed tested battery；One battery clamp jacking block is fixed by sliding screw and servo motor；Separately
One battery clamp jacking block is fixedly connected with mechanics sensor.
4. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method as described in claim 1, it is characterised in that：Institute
It is conductive aluminium sheet to state thermal module pedestal；The thermostat is cooling piece.
5. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method as described in claim 1, it is characterised in that：Institute
The test method for stating device is：Tested battery is clamped with battery clamp, not equality of temperature is then applied to battery by thermostat
Degree, and the temperature of battery ambient is monitored by temperature sensor bed course, need copper heat sink to fill during thermostat
It sets to be connected with the cavity of scanning electron microscope and cools down to reach the constant of battery ambient temperature to it；This device is put
It sets in the microscopical cavity of Scanning Electron, charge-discharge test is carried out to battery, then to the section in battery charge and discharge process
Monitoring in real time is carried out to take pictures；It is fixed can to obtain battery with analyzing processing is carried out for the image that the monitoring of Scanning Electron microscope is collected
The information of quantitative change shape.
6. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method as claimed in claim 2, it is characterised in that：Institute
The test method for stating device is：Fix tested battery with battery clamp jacking block, according to servo motor drive sliding screw from
And battery clamp jacking block is driven to be moved by guide rail；Apply different external force to battery by different moving displacements, external force
Size is monitored in real time by mechanics sensor；This device is placed into the microscopical cavity of Scanning Electron, to battery into
Then row charge-discharge test carries out monitoring in real time to the section in battery charge and discharge process and takes pictures；Obtained image information with into
Row analyzing processing can obtain the information that battery quantitatively deforms.
7. the test device of battery in-situ scanning Electronic Speculum under a kind of multi- scenarios method as claimed in claim 3, it is characterised in that：Institute
The test method for stating device is：Wide temperature original position battery test system is placed into mechanics to load in battery test system in situ
Battery clamp jacking block position, while the effect of different temperatures and different external forces is realized to being tested battery；Then device is placed
Into the microscopical cavity of Scanning Electron, to battery carry out charge-discharge test, then to the section in battery charge and discharge process into
Row in real time take pictures by monitoring；Obtained image information can obtain battery in different temperature fields and external force with analyzing processing is carried out
Quantitative deformation information under field action.
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Cited By (4)
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|---|---|---|---|---|
| CN110118793A (en) * | 2019-06-25 | 2019-08-13 | 北京工业大学 | Electrochemical in-situ experimental provision in a kind of electrochemistry sample clamp and scanning electron microscope |
| CN111337715B (en) * | 2020-04-23 | 2021-06-01 | 中国科学院化学研究所 | Device for observing surface interface of temperature-changing solid-state battery by using in-situ electrochemical atomic force microscope |
| CN112945856A (en) * | 2021-02-25 | 2021-06-11 | 天津力神电池股份有限公司 | Optical in-situ observation method for variable-temperature charging and discharging of lithium ion experimental battery |
| CN115621591A (en) * | 2022-12-16 | 2023-01-17 | 合肥视微科技有限公司 | Battery normal position image device with displacement detection function |
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