CN110133088A - Lithium concentration distribution and deformation field synchronization in-situ measurement system in electrode material - Google Patents
Lithium concentration distribution and deformation field synchronization in-situ measurement system in electrode material Download PDFInfo
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- CN110133088A CN110133088A CN201910330944.8A CN201910330944A CN110133088A CN 110133088 A CN110133088 A CN 110133088A CN 201910330944 A CN201910330944 A CN 201910330944A CN 110133088 A CN110133088 A CN 110133088A
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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
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/16—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge
- G01B11/161—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge by interferometric means
- G01B11/162—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge by interferometric means by speckle- or shearing interferometry
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
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- 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
- G01N27/403—Cells and electrode assemblies
- G01N27/413—Concentration cells using liquid electrolytes measuring currents or voltages in voltaic cells
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- G—PHYSICS
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- 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
- G01N27/4161—Systems measuring the voltage and using a constant current supply, e.g. chronopotentiometry
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Abstract
The present invention relates to lithium concentration distributions in electrode material and deformation field synchronization in-situ measurement system；System includes two sets Image Acquisition optical paths, and during realization electrochromic electrode material Li insertion extraction, deformation information is synchronous with lithium ion space distribution information in same electrode zone, in situ measurement.Two sets of Image Acquisition optical paths are that gray level image acquires optical path and Color Image Acquisition optical path；Measuring system is made of image collecting device, gray level image acquisition optical path, Color Image Acquisition optical path, simulation half-cell device, cell tester and optical platform.Two sets of optical paths work alternatively, and do not interfere with each other, are respectively used in situ, the real-time acquisition of electrode gray scale image and chromatic image in lithium ion diffusion process.The color of correlation analysis and electrochromic electrode material based on electrode gray level image and the corresponding relationship of material internal lithium-inserting amount, measurement result can provide in diffusion process simultaneously, the deformation information of electrode the same area and corresponding lithium ion space distribution information.
Description
Technical field
The invention belongs to new energy field, lithium ion distribution and electrode deformation field are same in specifically a kind of electrochromic electrode
The experimental system in situ of pacing amount is diffused through applied to power-electrochemistry Multivariable Coupling inside electrode material in lithium ion battery
The synchro measure of lithium concentration field and deformation field in journey.
Background technique
Lithium ion battery is because energy density is high, power is high, self-discharge rate is low, memory-less effect and environmentally protective etc. numerous excellent
It puts and receives much attention, be current one of the most common energy transfer and storage facilities.Solid phase of the lithium ion in electrode material expands
Scattered is the basic link in battery charge and discharge process, is a power-electrochemistry Multivariable Coupling driving complex process.Electrode material
Lithium ion diffusion will cause potential change and electrode deformation in material, and the diffusion-induced stress for deforming generation can cause electrode material mechanicalness
It can degenerate and circulating battery stability decays, in addition, the stress that diffusion causes can influence the expansion of potential and lithium ion in turn again
The process of dissipating.Currently, the measuring technique of various optics, spectroscopy be used to analyze the diffusion process of lithium ion in electrode, in using
The Mass Distribution of lithium ion in sub- scatterometry electrode, the deformation of microstructure caused by being embedded in X-ray diffraction measurement lithium ion,
Electrode deformation caused by embedding lithium etc. is measured with digital image correlation technique.But at present about lithium ion transport process and electrode
The experiment measurement of deformation is often independent of one another, and single measurement method causes result that can only provide individual lithium ion distributed intelligence
Or electrode deformation information, lack for the coupling process between lithium ion distribution and its caused electrode deformation a kind of effective, more
The experimental measurement method of information.For the coupling mechanism probed between lithium ion diffusion and electrode deformation, urgent need develops a kind of comprising more
The test macro that kind of measurement method and different measurement methods can be simultaneously independent of each other each other simultaneously, with realize in electrode lithium from
The synchro measure of son diffusion and electrode deformation information.
Summary of the invention
Concentration field and deformation field information in lithium ion dissipation period electrode can not be provided simultaneously to solve existing measuring technology
The problem of.The present invention is directed to the electrode material with electrochromism attribute, and providing one kind can lithium ion inside measuring electrode simultaneously
The in-situ measurement system of distribution and electrode deformation；The system includes two sets of Image Acquisition optical paths being independent of each other, it can be achieved that electroluminescent
Deformation information is synchronous with lithium ion space distribution information during electrochromic electrode material Li insertion extraction, in same electrode zone, original position
Measurement.
It is of the present invention solve the problems, such as used by technical solution are as follows:
Lithium concentration distribution and deformation field synchronization in-situ measurement system in electrode material；It is characterized in that system includes two sets
Two sets of Image Acquisition optical paths, during realizing electrochromic electrode material Li insertion extraction, in same electrode zone deformation information and lithium from
Synchronization, the in situ measurement of Subspace Distribution information.
Two sets of Image Acquisition optical paths are that gray level image acquires optical path and Color Image Acquisition optical path；Measuring system by
Image collecting device, gray level image acquisition optical path, Color Image Acquisition optical path, simulation half-cell device, cell tester and light
Learn platform composition.
The electrode gray level image acquisition optical path includes monochrome CCD camera, camera lens, filter plate, monochromatic source；Electrode
It includes color cmos video camera, camera lens, white light source that color image, which acquires optical path,；
The connecting mode of gray level image acquisition optical path is to consolidate the monochrome CCD camera equipped with camera lens and filter plate by bracket
It is scheduled on optical platform, monochrome CCD camera is apart from about 20~30 centimetres of optical platform surface；By monochrome CCD camera and figure
As acquisition device connects；Monochrome CCD camera is adjusted, makes its optical axis in vertical direction, is seen in simulation half-cell device optics
Survey the vertical surface of window；Gray level image acquire optical path light by cell apparatus, pass sequentially through filter plate, camera lens,
Monochrome CCD camera；The connecting mode of Color Image Acquisition optical path is that color cmos video camera is fixed on optics by bracket to put down
On platform, it is made to be in sustained height with monochrome CCD camera；Color cmos video camera is connect with image collecting device；Adjustment
Color cmos video camera makes its optical axis and monochrome CCD camera optical axis parallel arranged, is in same perpendicular, and make its light
The angle of axis and monochrome CCD camera optical axis is no more than 30 degree；The light of Color Image Acquisition optical path is by cell apparatus, according to
It is secondary to pass through camera lens, color cmos video camera；Monochromatic source, white light source, simulation half-cell device and cell tester are located
In on optical platform, wherein monochromatic source, white light source are placed on the surrounding of simulation half-cell device optical observation window；Mould
In quasi- half-cell device charge and discharge process, when gray level image acquires optical path work, only monochromatic source is as light source, for adopting
Collect the gray level image of electrode during embedding de- lithium；When Color Image Acquisition optical path works, only white light source is used for as light source
Acquire the color image of electrode during embedding de- lithium.Two sets of Image Acquisition optical paths are both placed on optical platform, to avoid
Influence of the extraneous vibration to Image Acquisition
It includes monochrome CCD camera 1,1, camera lens, filter plate 1, monochromatic source 2 that electrode gray level image, which acquires optical path,
It is a；It includes 1, color cmos video camera, 1, camera lens, white light source 2 that electrode color image, which acquires optical path,.
The simulation half-cell device is above electrode with glass observation window, by window can show into
The electrode material of row Li insertion extraction.
The cell tester is used to carry out charge-discharge test to simulation half-cell device, carries out embedding lithium to electrode material
With de- lithium.
The image collector is set to the computer for being mounted with image pick-up card, can acquire to two sets of Image Acquisition optical paths
The image that arrives carry out simultaneously, acquisition respectively and record.
Lithium concentration distribution and deformation field synchronization in-situ measurement system Examination on experimental operation in electrode material of the invention；
It is characterized in that steps are as follows:
1) charge-discharge test is carried out to simulation half-cell device with cell tester, during setting electric discharge, lithium ion insertion
Electrode, during charging, lithium ion deviates from electrode；
2) the electrode ash during the embedding de- lithium of electrode, under the state needed for the experiment of acquisition in real time in situ of gray level image acquisition optical path
Spend image；
3) electricity while gray level image acquisition optical path work, under the same state of Color Image Acquisition optical path synchronous recording
The color RGB image of pole surface the same area；To eliminate two optical path light sources to mutual influence, the illumination of manual switching optical path
Source, the collecting work of two sets of light path systems is interspersed to carry out, so that only opening white light source, gray level image in Color Image Acquisition
Monochromatic source is only opened when acquisition；The time interval of gray level image and Color Image Acquisition is no more than 10 seconds, since lithium ion is solid
The order of magnitude of phase diffusion coefficient is 10-8~10-10cm2/ s, so the influence that the time interval of acquisition generates experimental measurements
It is smaller, it can be ignored, it is synchronous for being approximately considered the acquisition of two kinds of images；
4) image analysis: correlation is carried out using gray level image of the digital image correlation technique DIC to certain position in electrode
Analysis, obtains the deformation information of the lithium ion dissipation period position；Corresponding relationship based on electrode color Yu its embedding lithium concentration, benefit
The lithium concentration distributed intelligence of the same space position is obtained with electrode color image.
The collecting work of two sets of light path systems is interspersed to carry out, and the switching relevant source used time is no more than 10s, so that
White light source is only opened when Color Image Acquisition, gray level image only opens monochromatic source when acquiring, due to gray level image and colour
Time interval≤10 second of Image Acquisition, therefore ignore, it is synchronous for being approximately considered the acquisition of two kinds of images.
The innovation and practicality of experiment test system of the present invention is as follows:
(1) test macro includes two sets of Image Acquisition optical paths --- and gray level image acquires optical path and Color Image Acquisition light
Road, two sets of optical paths are worked alternatively, are not interfere with each other, and are respectively used to electrode gray scale image and chromatic image in lithium ion diffusion process
In situ, acquisition in real time.The time interval for acquiring optical path alternation due to two sets is very short, it is believed that the image of two sets of optical paths
Acquisition is synchronous.
(2) color and the embedding lithium of material internal of correlation analysis and electrochromic electrode material based on electrode gray level image
The corresponding relationship of amount, measurement result can provide in diffusion process simultaneously, the deformation information of electrode the same area and corresponding lithium
Ion space distributed intelligence.
Detailed description of the invention
Fig. 1 double light path cooperates with in-situ measurement system schematic diagram；
Cell voltage potential changes with time in Fig. 2 graphite electrode process of intercalation；
Corresponding electrode strain cloud atlas (b) of color image and the lithium concentration distribution (a) of Fig. 3 graphite electrode.
Specific embodiment
Step process of the invention is further described below by way of specific embodiment, it should be noted that this implementation
Example be it is narrative, without being restrictive, do not limited the scope of protection of the present invention with this.
By taking graphite electrode as an example, in conjunction with Fig. 1, the present invention is described in further detail.In situ survey is cooperateed with using double light path
The deformation of electrode and the distribution of corresponding lithium ion, measurement process are divided into following step during measuring the embedding lithium of systematic survey graphite electrode
It is rapid:
(1) assembling of half-cell device is simulated
Assembling simulation half-cell device, battery cathode is metal lithium sheet, just extremely graphite electrode, electrolyte are being graphite electrode
Electrolyte；It carries out the embedding lithium of constant current to simulation half-cell device with Land 2001A type cell tester to test, embedding lithium current density
For 53mA/g.Variation of the cell voltage with the embedding lithium time, curve table alum ink electricity during Fig. 2 is the embedding lithium that cell tester records
Extremely embedding lithium experiment is normally carried out；This specific embodiment is set forth in detail on voltage-time curve, and star mark point corresponds to the moment 2
The lithium concentration spatial distribution of hour and the measurement process of electrode deformation.
(2) double light path cooperates in situ measurement
Double light path schematic diagram as shown in Figure 1, measuring system by be mounted with image pick-up card computer image acquisition installment,
Gray level image acquires optical path, Color Image Acquisition optical path, simulation half-cell device, Land 2001A type cell tester composition,
Measuring system is integrally placed on optical platform；Wherein, electrode gray level image acquisition optical path includes monochrome CCD camera 1, shows
Micro- enlarging lens 1, filter plate 1, monochromatic source 2；The connecting mode of gray level image acquisition optical path be will equipped with camera lens and
The monochrome CCD camera of filter plate is fixed on optical platform by bracket, and monochrome CCD camera is apart from optical platform surface about 20
Centimetre；Monochrome CCD camera is connect with image collecting device；Monochrome CCD camera is adjusted, making its optical axis is in vertical direction,
Vertical surface in simulation half-cell device optical observation window；The light of gray level image acquisition optical path is gone out by cell apparatus
Hair, passes sequentially through filter plate, camera lens, monochrome CCD camera；It includes color cmos video camera 1 that electrode color image, which acquires optical path,
A, 1, micro magnifier head, white light source 2；The connecting mode of Color Image Acquisition optical path is by color cmos video camera
It is fixed on optical platform by bracket, it is made to be in sustained height with monochrome CCD camera；By color cmos video camera and image
Acquisition device connection, adjusts color cmos video camera, makes its optical axis and monochrome CCD camera optical axis parallel arranged, in same
Perpendicular, and make its optical axis and monochrome CCD camera optical axis in 25 ° of angles；The light of Color Image Acquisition optical path is by battery
Device sets out, and passes sequentially through camera lens, color cmos video camera；Monochromatic source, white light source are placed on simulation half-cell device light
Learn the surrounding of observation window；It simulates in half-cell device charge and discharge process, when gray level image acquires optical path work, only monochromatic light
Gray level image of the source as light source, for electrode during acquiring embedding de- lithium；It is only white when Color Image Acquisition optical path works
Color image of the light source as light source, for electrode during acquiring embedding de- lithium.
Cooperate monochromatic source, gray level image acquires the optical observation window that optical path passes through cell apparatus, collects and records embedding
The gray level image of graphite electrode during lithium；The optical axis of optical path is shown in Fig. 1 perpendicular to graphite electrode surface, sets frequency acquisition as 1
It is secondary/30 seconds；While gray level image acquires optical path work, Color Image Acquisition optical path cooperates white light source, passes through cell apparatus
Optical window, record the color image of graphite electrode surface the same area during embedding lithium, set frequency acquisition as 1 time/30 seconds；
To avoid influencing each other for two kinds of light sources, the collecting work of two sets of light path systems need to intert progress, i.e., when acquiring color image
White light source is only opened, white light source is closed after single acquisition, only opens green light source, carries out the acquisition of gray level image；
It since the time interval of gray level image and Color Image Acquisition is very of short duration (less than 10 seconds), therefore ignores, is approximately considered two
The acquisition of kind image is synchronous.
(3) analysis of experimental results
Fig. 3 (a) illustrates the graphite electrode color image at certain embedding lithium moment of this system record, and arrow is lithium ion in figure
It is embedded in the direction (parallel with x-axis) of electrode, image shows that left end electrode color is golden yellow, and right end electrode color is reddish brown
Color, along lithium ion dispersal direction, electrode color is brownish red by golden yellow gradually transition.In conjunction with electrode color and embedding lithium concentration
Corresponding relationship, electrode be golden yellow show normalized embedding lithium concentration in electrode hereinIt is 1, electrode is that brownish red shows this
Locate the normalized embedding lithium concentration of electrode in electrodeBe 0.5, the record of Color Image Acquisition optical path the result shows that, along lithium in electrode
Ion dispersal direction, lithium concentration0.5 is gradually decrease to from 1.
Using natural texture existing for graphite electrode surface as speckle, with digital image correlation technique to phase under synchronization
Electrode gray level image with region carries out correlation analysis, and Fig. 3 (b) provides attached drawing 3 (a) counter electrode strain cloud atlas.Strain cloud
Figure shows that the deformation of graphite electrode left end is larger, and the electrode strain Exx of x-axis direction is 1%.Electrode right end deforms smaller, Exx
It is 0.448%.Fig. 3 (a) and Fig. 3 (b) gives the lithium concentration distributed intelligence and electrode deformation letter of the same area in electrode
Breath, the results show that electrode color is golden yellow, corresponding lithium concentration in electrode left areaIt is 1, in corresponding region
It is 1% that electrode, which strains Exx,.Electrode color is brownish red, corresponding lithium concentration in electrode right areaIt is 0.5, it is corresponding
Electrode strain Exx in region is 0.75% or so.As a result illustrate, there are apparent dynamics with lithium concentration for electrode deformation
Causality, the more region of lithium concentration, the region that electrode deformation is larger, lithium concentration is less, electrode deformation are smaller.
Lithium concentration distribution and deformation field synchronization in-situ measurement system in the electrode material that the present invention is disclosed and proposed, this
Field technical staff can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although method of the invention and
Technology of preparing is described by preferred embodiment, and related technical personnel can obviously not depart from the content of present invention, essence
Methods and techniques described herein route is modified or is reconfigured in mind and range, to realize final technology of preparing.
In particular, it should be pointed out that all similar replacements and change are apparent to those skilled in the art, they
It is considered as being included in spirit of that invention, range and content.
Claims (10)
1. lithium concentration distribution and deformation field synchronization in-situ measurement system in electrode material；It is characterized in that system includes two sets of figures
As acquisition optical path, during realizing electrochromic electrode material Li insertion extraction, deformation information and lithium ion space in same electrode zone
Synchronization, the in situ measurement of distributed intelligence.
2. measuring system as described in claim 1；It is characterized in that two sets of Image Acquisition optical paths be gray level image acquire optical path and
Color Image Acquisition optical path；Measuring system acquires optical path, Color Image Acquisition optical path, mould by image collecting device, gray level image
Quasi- half-cell device, cell tester and optical platform composition.
3. measuring system as claimed in claim 2；It is imaged it is characterized in that electrode gray level image acquires optical path including monochrome CCD
Machine, camera lens, filter plate, monochromatic source；It includes color cmos video camera, camera lens, white light source that electrode color image, which acquires optical path,；
The connecting mode of gray level image acquisition optical path is that the monochrome CCD camera equipped with camera lens and filter plate is fixed on optics by bracket
On platform, monochrome CCD camera is apart from 20~30 centimetres of optical platform surface；By monochrome CCD camera and image collecting device
Connection；Monochrome CCD camera is adjusted, makes its optical axis in vertical direction, in the perpendicular of simulation half-cell device optical observation window
Right above straight；The light of gray level image acquisition optical path is by cell apparatus, filter plate, camera lens, monochrome CCD camera shooting are passed sequentially through
Machine；The connecting mode of Color Image Acquisition optical path is to be fixed on color cmos video camera on optical platform by bracket, make its with
Monochrome CCD camera is in sustained height；Color cmos video camera is connect with image collecting device；Adjust color cmos camera shooting
Machine makes its optical axis and monochrome CCD camera optical axis parallel arranged, is in same perpendicular, and take the photograph its optical axis with monochrome CCD
The angle of camera optical axis is no more than 30 degree；The light of Color Image Acquisition optical path is by cell apparatus, camera lens, coloured silk are passed sequentially through
Color cmos camera；Monochromatic source, white light source, simulation half-cell device and cell tester are on optical platform,
Wherein, monochromatic source, white light source are placed on the surrounding of simulation half-cell device optical observation window；Simulation half-cell device fills
In discharge process, gray level image acquisition optical path is used cooperatively with monochromatic source, the grayscale image for electrode during acquiring embedding de- lithium
Picture；Color Image Acquisition optical path is used cooperatively with white light source, the color image for electrode during acquiring embedding de- lithium.
4. measuring system as claimed in claim 2；It is characterized in that measuring system is integrally placed on optical platform, to avoid outer
Boundary vibrates the influence to Image Acquisition.
5. measuring system as claimed in claim 2；It is characterized in that electrode gray level image acquisition optical path includes monochrome CCD camera
1,1, camera lens, filter plate 1, monochromatic source 2；Electrode color image acquisition optical path include 1, color cmos video camera,
1, camera lens, white light source 2.
6. measuring system as claimed in claim 2；It is characterized in that simulation half-cell device is to observe above electrode with glass
Window observes the electrode material for carrying out Li insertion extraction by window.
7. measuring system as claimed in claim 2；It is characterized in that cell tester is used to fill simulation half-cell device
Discharge test realizes the embedding and removing process of electrode material.
8. measuring system as claimed in claim 2；It is characterized in that image collecting device is by the computer equipped with image pick-up card
It constitutes, for acquisition and recording gray level image acquisition optical path and color image to acquire the image that optical path obtains simultaneously, respectively.
9. lithium concentration distribution and deformation field synchronization in-situ measurement system experimental implementation side in the electrode material of claim 1
Method；It is characterized in that steps are as follows:
1) charge-discharge test being carried out to simulation half-cell device with cell tester, during setting electric discharge, lithium ion is embedded in electrode,
During charging, lithium ion deviates from electrode；
2) during the embedding de- lithium of electrode, the electrode grayscale image of the state needed for the experiment of acquisition in real time in situ of gray level image acquisition optical path
Picture；
3) while gray level image acquisition optical path work, the electrode surface of the same state of Color Image Acquisition optical path synchronous recording
The color RGB image of the same area；To eliminate two optical path light sources to mutual influence, switching-over light path light source, so that two
The interspersed progress of collecting work for covering light path system, i.e., only open white light source, when gray level image acquires in Color Image Acquisition
Only open monochromatic source；Meanwhile the time interval of gray level image and Color Image Acquisition is no more than 10s；
4) image analysis: carrying out correlation analysis using gray level image of the digital image correlation technique DIC to certain position in electrode,
Obtain the deformation information of the lithium ion dissipation period position；Corresponding relationship based on electrode color Yu its embedding lithium concentration, utilizes electricity
Pole color image obtains the lithium concentration distributed intelligence of the same space position.
10. method as claimed in claim 9, it is characterized in that time interval≤10 second of gray level image and Color Image Acquisition.
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