CN109725264A - A kind of in-situ detection method and device of the distribution of electrode of liquid flow cell current density - Google Patents
A kind of in-situ detection method and device of the distribution of electrode of liquid flow cell current density Download PDFInfo
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Abstract
The present invention provides the in-situ detection method and device of a kind of electrode of liquid flow cell current density distribution, is imaged using electrode surface of the total internal reflection optical system to flow battery, according to the intensity variation of different location in image, obtains electrode current density distribution situation.The present invention is by cooperation seamless between optical total-reflection system and flow battery, realize the in situ detection of electrode surface imaging and current density in cell operation, the Two dimensional Distribution and evolution process of electrode current density under different situations are obtained, provides in situ detection tool to improve battery performance.
Description
Technical field
The present invention relates to the in situ detections that detection technique field more particularly to a kind of electrode of liquid flow cell current density are distributed
Method and device.
Background technique
Energy storage technology is the important component of new energy system.Flow battery is as a kind of extensive energy storage technology, tool
There is the features such as high capacity, service life is long, therefore, optimization flow battery performance is the target generally pursued in industry.Existing research side
Fado is to provide battery ensemble average performance by detection, can not specify local spatial distribution differences to the shadow of battery performance
It rings.
Local current density distribution be characterize electrode reaction rate and battery lasts intuitive factor, mainly by
Electrode space activity distribution and electrolyte Flow Field Distribution influence.And porosity, permeability, thickness, the specific surface area of electrode itself
It is had differences Deng may cause electrode activity spatial distribution；The performances such as composition, the concentration of electrolyte, the design of battery structure
Influence electrolyte Flow Field Distribution.Since the factor for influencing current density is complicated, it is very that in situ quantitation detection is carried out to it
It is necessary.Traditional in-situ detection method be mainly electricity in terms of Hall sensor (J.Electrochem.Soc., 2004,
151, A394-A398), by-passed resistor (J. Electrochem.Soc., 2003,150, A79-A85) and printed circuit board
(J.Appl.Electrochem., 1998,28,663-672) etc., these methods are relative complex cumbersome, and electrical detection itself
It is possible that interfering to battery operation, detection accuracy, while limited spatial resolution are influenced.And optical means, there is height
The features such as sensitivity, high-resolution is the effective ways for realizing electrode of liquid flow cell current density distribution measuring.
It is special that applicant proposes " a kind of online test method and device of electrode of liquid flow cell local reactivity " before this
Sharp (application number 201811617909.6), the patent mainly utilize Applications of surface plasmon resonance to provide a kind of flow battery
The characterizing method of electrode activity.In view of the space current Density Distribution in cell operation can embody flow battery performance,
The in situ detection to current density Two dimensional Distribution in flow battery operational process is realized in present invention proposition using total reflection technology,
And respective influence is distributed to current density by control variate method Electrode activity distribution and electrolyte Flow Field Distribution, in this way
Technical tool can be provided for factors that further discussion influences the two distributions.
Summary of the invention
In view of the above-mentioned defects in the prior art, the invention proposes a kind of original positions of electrode of liquid flow cell current density distribution
Detection method is imaged, according to the light of different location in image using electrode surface of the total internal reflection optical system to flow battery
Strength Changes obtain electrode current density distribution situation.
Specifically, the step of detection includes:
The first step, debugging total internal reflection optical system to electrode surface can be realized blur-free imaging, recording electrode image；
Second step carries out charge-discharge test, while the electrode image that acquisition changes over time to flow battery, saves as figure
As group；
The light intensity of each position in acquired image group is drawn out light intensity versus time curve by third step；
The light intensity curve of obtained each position is converted current density absolute value change curve by 4th step；
5th step extracts the current density value in the curve of each position at same time location and is drawn in current density distribution
Figure.
Further, after the 5th step, further includes: keep electrode and prism contact situation constant, change the stream of electrolyte
Field distribution, the step of obtaining current density distributing figure group of the electrode at different flow fields.
Further, further includes: guarantee that the Flow Field Distribution of electrolyte is constant, replace the electrode of different activities, obtain same
The step of current density distributing figure group in the case of the Different electrodes activity distribution of flow field.
Further, the mode of the Flow Field Distribution for changing electrolyte is to change the position of electrolysis liquid flow inlet, outflux
It sets, and/or changes flow velocity.
The present invention also proposes a kind of in situ detection device of electrode of liquid flow cell current density distribution, using total internal reflection light
Electrode surface is imaged in system, and the total internal reflection optical system includes incident optical module 1, prism 2 and imaging detection mould
Block 3；Wherein, the incident optical module 1 is for providing parallel p-type polarised light, the electricity of the prism 2 and flow battery to be detected
Pole 42a is in close contact.
It further, further include prism clip module 51 and fixed block 52, the flow battery to be detected includes battery case
43, the battery case 43 and 42 corresponding position of electrode are middle opening, are additionally provided with pad in the side electrode 42a to be detected
Circle 481；The prism clip module 51 and the fixed block 52 match, by screw by prism 2, washer 481, electricity to be detected
Pole 42a is closely connected.
Further, the side of the electrode 42 has a stage portion, the stage portion of collector 421 and the electrode 42
Contact.
Further, it is separated between the flow battery positive and negative anodes to be checked by diaphragm 41, the battery case 43 of diaphragm two sides
It is respectively provided with liquid inflow, tap hole, electrolyte is pumped into battery case 43 by conduit through peristaltic pump 46 by fluid reservoir 45.
Further, the flow battery to be detected is all-vanadium flow battery, and the electrode 42 is carbon felt.
The invention has the benefit that battery fortune is realized in cooperation seamless between optical total-reflection system and flow battery
The in situ detection of electrode surface imaging and current density, obtains the Two dimensional Distribution of electrode current density under different situations during row
And evolution process, in situ detection tool is provided to improve battery performance.
Detailed description of the invention
Fig. 1 is the total reflectance curve figure of p-type and s type polarised light.
Fig. 2 is the in-situ detection method flow chart of electrode of liquid flow cell current density distribution.
Fig. 3 is the in situ detection device block diagram of electrode of liquid flow cell current density distribution.
Fig. 4 is the in situ detection structure drawing of device of electrode of liquid flow cell current density distribution.
Fig. 5 a is prism and flow battery constitutional diagram.
Fig. 5 b is prism and flow battery expanded view.
Fig. 6 a is electrode and collector connected mode schematic diagram of the invention.
Fig. 6 b is traditional electrode and collector connected mode schematic diagram.
Fig. 7 a is the in-situ detection method schematic diagram of electrode of liquid flow cell current density distribution.
Fig. 7 b is the current density distribution schematic diagram under in situ detection difference flow field.
Fig. 7 c is the electrode activity difference schematic diagram of in situ detection Different electrodes.
Appended drawing reference meaning in figure are as follows:
1- incidence optical module, 11- light source, 12- object lens, 13- diaphragm, 14- collimation lens, 15- optical filter, 16- polarization
Piece, 2- prism, 3- imaging detection module, 31- imaging lens group, 32- area array CCD, 33- electrode imaging schematic diagram, 4- battery dress
Set module, 41- diaphragm, 42- electrode, 421- collector, 43- battery case, 44- charge and discharge instrument, 45- fluid reservoir, 46- wriggling
Pump, 47- gasket, 481- washer, the hollow backing plate of 482-, 483- full wafer backing plate, 484- nut, 485- screw, 51- prism clamping
Block, 52- fixed block.
Specific embodiment
The present invention uses total internal reflection (TIR) optical system of prism-coupled.According to total reflection formulaWherein, naFor the refractive index of interface optically thinner medium, npFor the refractive index of interface optically denser medium, lead to
It crosses theoretical modeling to calculate, the total reflectance curve of p-type and s type polarised light is as shown in Figure 1, naFor the refractive index of interface analyte, np
For the refractive index of interface couple prism.θTIRFor the angle of total reflection, θsFor the corresponding angle of sensitivity highest near the angle of total reflection.
Near the angle of total reflection, p-type polarization light curve (solid line in Fig. 1) is more precipitous, sensitivity with higher.In the present invention, light
Close medium is couple prism, refractive index npIt is constant, when lambda1-wavelength is certain and incidence angle θsFor sensitivity near the angle of total reflection
When highest angle, light intensity changes in θsNearby there is the very highly sensitive range of linearity.Therefore, using the p of this range of linearity
Type polarised light is for being imaged and detecting, so that the analyte refractive index n of interfaceaVariation be presented as the change of reflected light light intensity
Change, by TIR system Sensitive Detection.
Due to being primarily present faradic currents caused by redox reaction occurs in cell operation, so active
Substance variation of valence makes electrolyte refractive index change.The relationship of TIR signal and current density are as follows:Wherein n is the electron amount that redox reaction occurs, F
For Faraday constant, B is sensitivity of the TIR signal to body variations in refractive index, αRAnd αORespectively reduzate and oxide unit is dense
Refractive index variable quantity caused by degree changes, DRAnd DOThe respectively diffusion coefficient of reduzate and oxide, L-1For inverse Laplce
Transformation,For the Laplace transform of TIR signal.Therefore, it can be obtained based on above-mentioned formula electric in cell operation
The Two dimensional Distribution of electrode current density changes.
Fig. 2 is main implementation flow chart of the invention, and S1 is imaged to electrode surface first with TIR light system；Then
By charge and discharge instrument to flow battery charge and discharge, reflected at electrode under different charged states with studying in flow battery operational process
Rate variation, the continuous collecting electrode image during charge and discharge form electrode image group S2；According to the light of each position in image group
It is strong to draw each position light intensity versus time curve S3；It is close that electric current is converted by the light intensity curve of obtained each position again
Absolute value change curve S4 is spent, the current density value in the curve of each position at same time location is extracted and is drawn in current density point
Butut S5.
The in situ detection device of electrode of liquid flow cell current density distribution is overall as shown in figure 3, incident optical module 1 is used for
The quasi- monochromatic polarised light of parallel p-type is generated, light beam is using reflected light is generated after high index prism 2, due to test substance
Refractive index and the light intensity of reflected light there are quantitative relationships, therefore the refractive index that interface test substance can be measured based on light intensity is become
Change situation.Imaging detection module 3 is used for the image of acquisition electrode and prism contact interface.Battery device module 4 mainly passes through
Charge and discharge instrument carries out charge-discharge test to flow battery, studies when redox reaction occurs in cell operation at electrode
Electrolyte variations in refractive index process, and then obtain the distribution of the current density at electrode.
As shown in figure 4, in incident optical module 1, light source 11 is LED light source for the exploded view of the device, the light beam issued according to
It is secondary to become directional light after object lens 12, diaphragm 13 and collimation lens 14, then become quasi- monochromatic feux rouges by optical filter 15, in
The a length of 632.8nm of cardiac wave obtains parallel p-type polarised light using polarizing film 16, and corresponding with TIR system sensitivity highest
Angle, θsIt is incident in prism 2, in the present embodiment, the refractive index of prism 2 is 1.75.Reflected light is imaged by imaging lens group 31
In area array CCD 32, imaging schematic diagram is as shown in 33.In battery device module 4, charge and discharge instrument 44 is wired to battery
On positive and negative electrode 42, constant-current charge is carried out.It is separated between positive and negative anodes by diaphragm 41.Electrolyte in fluid reservoir 45 is by peristaltic pump 46
It is pumped into battery case 43 through conduit.
The present embodiment is using all-vanadium flow battery as in situ detection battery.The all-vanadium flow battery is with 1.5M VO2+And 2M
H2SO4As anode electrolyte, 1.5M V3+With 2M H2SO4As electrolyte liquid, using Nafion film as diaphragm.Using filling
Discharge instrument carries out constant current charge-discharge to it in the voltage window of 0.8V-1.65V.Current density is 40mA/cm3, peristaltic pump
Speed is 60mL/min.Positive and negative electrolyte is pumped into battery case from fluid reservoir by peristaltic pump and redox occurs on positive and negative electrode
Reaction, i.e. vanadium ion valence state change, and return to fluid reservoir again later, loop back and forth like this.In this way, in anode electrolyte
VO2+And VO2 +Between mutually convert, and the V in electrolyte liquid3+And V2+Between mutually convert.Under different charged states,
Electrolyte refractive index near one lateral electrode can be by real-time detection, to obtain on electrode current density distributing figure and its at any time
Change procedure.
Fig. 5 is the cooperation schematic diagram of prism and flow battery in situ detection device, and wherein Fig. 5 a is constitutional diagram, and Fig. 5 b is
Expanded view.The device ensure that prism 2 is directly contacted with one lateral electrode 42a of battery, and electrolyte does not leak out, and not influence battery fortune
Row.Wherein, positive and negative electrode 42a, 42b is in close contact with collector 421a, 421b respectively, and by gasket 47a, 47b and diaphragm 41
It separates, is then inserted in battery case 43a, 43b and forms battery module.Battery case 43 has opening, the cross-sectional area of opening
For 28mm × 20mm, matched with electrode size.It is using screw 485, nut 484 and backing plate 482,483 that battery module is closely solid
It is fixed.Wherein, the backing plate in electrode one end to be measured is hollow backing plate 482, and in-between openings of sizes is also matched with electrode size, another
Side is full wafer backing plate 483.To avoid leakage, washer 481 is additionally provided in electrode side to be measured.Finally, by prism clamp 51, fixed block
52 fix prism 2, washer 481 and battery module sealing, form the structure of Fig. 5 a.
Traditional electrode 42 and the connection type of collector 421 is as shown in Figure 6 b, and wherein collector 421 and electrode 42 be most
Large surface contact.But electrode 42 can not be imaged in which.The invention proposes a kind of new ways of contact, as shown in Figure 6 a,
The side of electrode has stage portion, contacts collector 421 with the stage portion.Using carbon felt as electrode 42 in the present embodiment,
Graphite plate is calculated as contact resistance of the collector 421 to two ways.Wherein carbon felt size is 21mm × 22mm × 5mm
7mm × 22mm × 3mm is deducted to form stage portion, graphite plate size is 22mm × 30mm × 3mm.By the way of Fig. 6 b, electricity
The contact area of pole and collector is 22mm × 21mm, and resistance is 0.046 Ω；It is contacted by the way of Fig. 6 a of the present invention, the two
Contact area be top to top part 22mm × 3mm, partial cross section 22mm × 7mm, measuring resistance is about 0.058 Ω.It is right
Than the contact resistance of two ways, it can be seen that the contact resistance of mode of the present invention is not much different with traditional approach, to cell performance
The influence of energy is within the scope of receiving.
Embodiment 1
Current density distribution of the in situ detection electrode of liquid flow cell under different flow fields.
As shown in Figure 7a, adjustment TIR system is in clear image S1 to electrode first；Then flow battery charge and discharge are acquired
The electrode image group S2 of journey, every image includes several pixels, such as A, B point in figure, takes every image in image group
Same pixel point-rendering light intensity-time-serial position, all pixels are drawn, in Fig. 7 a for pixel B draw song
Line S3.As can be seen that the light intensity curve of B point is corresponding with charge and discharge process, it is in cyclically-varying.It is close with electric current according to the angle of total reflection
The relationship of degree and the angle of total reflection and light intensity, is converted to current density absolute value-time graph for light intensity-time-serial position
S4.In experiment, almost unchanged constant value is presented in current density absolute value, but the numerical value of each pixel has a shade of difference.By institute
There is current density absolute value-time graph of pixel to take the same minimum period, draw X-Y scheme S5, the electric current of as electrode is close
Spend distribution map.
Since current density distributing figure synthesis presents caused by electrode different location activity and electrolyte Flow Field Distribution
Current density distribution is different.In order to further study influence of the flow field to current density, by control variate method, stream is individually considered
The influence of field.In the case where guaranteeing that carbon felt and prism contact situation are constant, change the inflow entrance and outflux of battery case
Position and/or flow velocity, then S1-S5 step in Fig. 7 a is carried out, the electrode current density figure in the case of different flow fields can be obtained
Group.As shown in Figure 7b, changed by flow field three times, obtain tri- width current density figure of F1, F2, F3, then it removed respectively same
Electrode activity influence current density distribution, obtain different electrolytes Flow Field Distribution influence current density distributing figure group FD1,
FD2,FD3.It is distributed as it can be seen that being able to detect electrode current density in cell operation by TIR light system, and then obtains electricity
Solve liquid stream field distribution situation.Change the difference in signal flow field in Fig. 7 b by background light and shade.
Embodiment 2
The electrode activity difference of in situ detection Different electrodes.
In the case where the Flow Field Distribution of guarantee electrolyte is constant, the electrode of different activities is replaced, is used in the present embodiment
For carbon felt as electrode, the step of replacing the carbon felt of 3 different activities, using Fig. 7 a for each carbon felt, obtains the electricity of the electrode
Current density figure, and then obtain current density distributing figure R1, R2, R3 of 3 different activities carbon felts.Then electrolyte is removed respectively
The influence of Flow Field Distribution obtains current density distributing figure RD1, RD2, the RD3 influenced by Different electrodes activity distribution.In Fig. 7 c,
The thickness variation signal carbon felt activity of lines is distinct.
The field it is to be appreciated by one skilled in the art that the above is only a specific embodiment of the present invention, and
It is not used in the limitation present invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done,
It should be included within protection scope of the present invention.
Claims (10)
1. a kind of in-situ detection method of electrode of liquid flow cell current density distribution, which is characterized in that use total internal reflection optical
The electrode surface of flow battery is imaged in system, according to the intensity variation of different location in image, obtains electrode current density
Distribution situation.
2. in-situ detection method according to claim 1, which is characterized in that the step of detection includes:
The first step, debugging total internal reflection optical system to electrode surface can be realized blur-free imaging, recording electrode image；
Second step carries out charge-discharge test, while the electrode image that acquisition changes over time to flow battery, saves as image
Group；
The light intensity of each position in acquired image group is drawn out light intensity versus time curve by third step；
The light intensity curve of obtained each position is converted current density absolute value change curve by 4th step；
5th step extracts the current density value in the curve of each position at same time location and is drawn in current density distributing figure.
3. in-situ detection method according to claim 2, which is characterized in that further comprising the steps of after the 5th step: protecting
It holds electrode and prism contact situation is constant, change the Flow Field Distribution of electrolyte, obtain electricity of the electrode at different flow fields
Current density distribution map group.
4. in-situ detection method according to claim 2 or 3, which is characterized in that further include following step after the 5th step
It is rapid: to guarantee that the Flow Field Distribution of electrolyte is constant, replace the electrode of different activities, obtain same flow field Different electrodes activity distribution feelings
Current density distributing figure group under condition.
5. according to the described in any item in-situ detection methods of claim 3, which is characterized in that the flow field for changing electrolyte point
The mode of cloth is to change the position of electrolysis liquid flow inlet, outflux, and/or change flow velocity.
6. a kind of in situ detection device of electrode of liquid flow cell current density distribution, which is characterized in that use total internal reflection optical
Electrode surface is imaged in system, and the total internal reflection optical system includes incident optical module (1), prism (2) and imaging detection
Module (3)；Wherein, the incident optical module (1) is for providing parallel p-type polarised light, the prism (2) and liquid stream to be detected
The electrode (42a) of battery is in close contact.
7. in situ detection device according to claim 6, which is characterized in that further include prism clip module (51) and fixed block
(52), the flow battery to be detected includes battery case (43), and the battery case (43) is with electrode (42) corresponding position
Middle opening is additionally provided with washer (481) in the side electrode to be detected (42a)；The prism clip module (51) and described solid
Determine block (52) to match, is closely connected prism (2), washer (481), electrode to be detected (42a) by screw.
8. in situ detection device according to claim 6 or 7, which is characterized in that the side of the electrode (42) has one
Stage portion, collector (421) are contacted with the stage portion of the electrode (42).
9. in situ detection device according to claim 7 or 8, which is characterized in that the flow battery positive and negative anodes to be checked it
Between separated by diaphragm (41), the battery case (43) of diaphragm two sides be respectively provided with liquid flow into, tap hole, electrolyte is by fluid reservoir
(45) battery case (43) are pumped by conduit through peristaltic pump (46).
10. according to the described in any item in situ detection devices of claim 6-9, which is characterized in that the liquid stream electricity to be detected
Pond is all-vanadium flow battery, and the electrode (42) is carbon felt.
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