CN109724947A - A kind of online test method and device of electrode of liquid flow cell local reactivity - Google Patents
A kind of online test method and device of electrode of liquid flow cell local reactivity Download PDFInfo
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Abstract
The present invention relates to the online test methods and device of a kind of electrode of liquid flow cell local reactivity, real time imagery is carried out to electrode surface using surface plasma body resonant vibration SPR optical system, according to the intensity variation of different location in image, the active judgement of electrode local reaction is obtained.Electrode surface is imaged by SPR optical system, obtains the current density of electrode local, realizes and real-time detection is distributed to electrode of liquid flow cell surface different location current density, provides technical tool for characterization electrode active surface spatial distribution.
Description
Technical field
The present invention relates to imaging measurement technology field, exist more particularly to a kind of electrode of liquid flow cell local reactivity
Line detecting method and device.
Background technique
Flow battery as extensive energy storage device, be realize that the energy effectively configures it is important by way of one of.Flow battery
A kind of high-performance energy-storage battery, have the characteristics that capacity height, the long-life, easy scale and receive significant attention.Flow battery
Usually using carbon material (carbon felt, carbon paper etc.) as electrode.As the important indicator of characterization battery performance, electrode reaction activity is straight
Connect the efficiency for influencing battery.It mainly includes that potential scan method (follow by linear sweep voltammetry that electrode activity, which characterizes conventional electrical method,
Ring voltammetry (CV)), galvanostatic charge/discharge and electrochemical impedance spectroscopy etc., these methods can only provide electrode W-response activity,
Such as cyclic voltammetry can only acquisition electrode after making alive average current density variation, that is, be unable to characterize modified electrode not
With otherness active at position.In view of for different location there may be difference, seeking one kind can be after carbon felt modified active
Reflect that the active method of electrode different location is to seem extremely important in cell operation in real time.
Optical detecting method based on surface plasma body resonant vibration (SPR) technology is by its high sensitivity, high-resolution, non-
Contacting lossless advantage has application in electrochemical field.SPR is a kind of electronics collective in metal surface after by electromagnetism excitation
Oscillatory occurences.There are quantitative relationships for the frequency of oscillation of SPR and the dielectric property of interface, and changing to it can be very sensitive
Response, therefore it is widely used in sensory field.SPR has the advantage of high-throughput detection because of it, is also able to achieve imaging function
Energy.
Applicant proposes to detect all-vanadium redox flow battery electrolyte charged state by Applications of surface plasmon resonance before this
With the technology of vanadium ion concentration, referring to patent ZL201210097314.9, ZL201210097362.8,
ZL201510724523.5.In view of the activity of electrode is extremely important on the influence of flow battery performance, it is therefore desirable to directly to electricity
Pole surface is imaged and studies its active otherness.The present invention in response to this problem, is proposed based on highly sensitive, high-resolution
Realize that imaging to electrode of liquid flow cell surface and electrode different location electric current are close with high-throughput Plasmon Resonance
The real-time detection of distribution is spent, provides technical tool for characterization electrode active surface spatial distribution.
Summary of the invention
In view of the above-mentioned defects in the prior art, the present invention provides a kind of the online of electrode of liquid flow cell local reactivity
Detection method and device.
A kind of online test method of electrode of liquid flow cell local reactivity, using SPR optical system to electrode surface
Real time imagery is carried out, according to the intensity variation of different location in image, obtains the active judgement of electrode local reaction, the electricity
Extremely carbon material electrode.
Further, the SPR optical system is the light intensity type SPR system of prism-coupled total internal reflection, can be imaged
While, obtain the refractive index Two dimensional Distribution and real-time change situation of the electrode surface electrolyte.
Further, the light intensity value of any position is converted to the current density relative value of the position, draws the position
Voltage-current density relative value curve；The voltage-current density relative value curve of more several positions obtains being compared
The reactivity of position judges.
Further, it while the SPR optical system carries out real time imagery to electrode surface, is also filled using potential scan
It sets and potential scan is carried out to the flow battery, and measure the electric current of the flow battery, obtain electrode ensemble average electricity piezo-electric
Current density curve；The voltage-current density relative value curve pair of the average voltage-current density plot and any position
Than obtaining the electrode reaction activity judgment of the position, the potential scan is to carry out cyclic voltammetry using three-electrode system to sweep
It retouches.
Further, the time is imaged in different potentials or different time by calculating same position in the intensity variation
The difference of intensity and obtain.
A kind of on-line measuring device of electrode of liquid flow cell local reactivity, using SPR optical system to electrode surface
Real time imagery is carried out, the SPR optical system includes incident parallel optical module 1, SPR block 2 and imaging detection module 3；Its
In, the light intensity type SPR block 2, including prism 21 and film layer structure 22, wherein film layer structure 22 and the electrode of liquid flow cell
42 contacts.
It further, further include potential scan apparatus module 4, the potential scan device uses three-electrode system 46,47,
The current value of the 48 measurement flow batteries, the three-electrode system 46,47,48 are placed in the liquid by electrolyte container lid 45
Inside the electrolyte container 41 of galvanic battery.
Further, the electrolyte container includes 41 at least one side, and the electrode 42 is located at electrolyte appearance
On the side of device 41.
It further, further include prism clip module 51 and fixed block 52, the prism clip module 51 and the fixed block 52
It matches, is tightly connected SPR block 2, electrode 42, electrolyte container 41 by screw 53.
Further, the electrode 42 is by electrode supporting block 44, it is ensured that with the contact of the SPR block 2.
The invention has the benefit that electrode surface is imaged by optical imaging system, electrode local is obtained
Current density is realized and is distributed real-time detection to the imaging on electrode of liquid flow cell surface and electrode different location current density, is table
Impressing electrode surface-active spatial distribution provides technical tool.
Detailed description of the invention
Fig. 1 is the online test method flow chart of electrode of liquid flow cell local reactivity in embodiment.
Fig. 2 is the on-line measuring device exploded view of electrode of liquid flow cell local reactivity in embodiment.
Fig. 3 a is SPR block and potential scan device overall diagram.
Fig. 3 b is SPR block and potential scan device expanded view.
Fig. 4 is the CV curve graph that cyclic voltammetry scans.
Fig. 5 is the light intensity variation diagram that electrode of liquid flow cell is imaged in SPR optical system.
Fig. 6 a is electrode different location light intensity variation diagram in cyclic voltammetry scanning process.
Fig. 6 b is the CV curve graph that second cycle period (CV-2) is converted in Fig. 6 a.
Specific embodiment
The present invention is further elaborated below in conjunction with attached drawing and a kind of preferred specific embodiment.
Applications of surface plasmon resonance can generate sensitive response to the variation on surface, and be able to achieve high-throughput inspection
It surveys.The present invention using Kretschmann prism structure construct SPR system, according to document (Angew.Chem.Int.Ed.2017,
56,1629-163) the electron number densitiy n of plasma known to0With resonance angle, θRBetween there are quantitative relationships.Due to resonance angle
Spend θRCorresponding to the corresponding angle in minimum value position in the reflected light light intensity of different angle, and electron number densitiy n0With current density
There are quantitative relationships by density J: J=n0ev.Wherein v is electron velocity.It therefore, can be by the light intensity of reflected light using SPR phenomenon
Change and is connected with the current density of corresponding position.In electrochemical reaction process, there are two kinds of electric currents: faradic currents and
Nonfaradaic current (electric double layer electric current).Above-mentioned quantitative relationship is only applicable to nonfaradaic current.And for faradic currents, it is main
If the change of electrolyte refractive index after redox reaction, i.e. ε occursdVariation.And εdVariation equally enable to resonate
Angle, θRIt changes, i.e. reflected light light intensity changes.Faradic currents occupy in the redox reaction that the present invention considers
Absolute leading position, therefore only consider faradic currents.According to document (Science 327,1363 (2010)), electrochemistry is considered
The relationship of the faradic currents density of middle redox reaction and the concentration of active material ion etc. can be reacted by measurement
The variation of light intensity is in journey to obtain the variation of current density.
Fig. 1 is the main implementation flow chart of the present embodiment, using SPR optical system to electrode surface real time imagery, due to
When redox reaction occurs for electrolyte at electrode, active material ion causes to aoxidize with potential conversion in electrolyte at electrode
Variation of valence occurs when current potential or reduction potential, that is, there is the transfer of electronics, so that refractive index changes, this can lead to
The luminous intensity measurement for crossing reflected light comes out.Therefore SPR optical system electrode surface characterization image obtained electrode different location
Activity distribution situation.
Meanwhile using the electric current of conventional electrical method measurement flow battery, by carrying out potential scan to the flow battery,
The average current density that electrode entirety can be obtained obtains electrode ensemble average voltage-current density curve.
During potential scan, the intensity image group of electrode surface is obtained, the light intensity of multiple positions in image is taken to believe
The light intensity curve that number can form each position, is converted by mathematics, is converted into current density change curve.By the curve
The voltage-current density curve comparison measured with conventional electrical method obtains the reactivity situation of electrode each position.
Fig. 2 is the device exploded view of the present embodiment.Wherein incident parallel optical module 1, SPR block 2 and imaging detection module 3
SPR optical system is constituted, to carry out quantitative measurment to electrode active surface, further includes potential scan device 4, is to pass through electrification
It learns work station and carries out cyclic voltammetry scanning to electrode.
Wherein, incident parallel optical module 1 mainly includes LED light source 11, object lens 12, diaphragm 13, saturating 14 mirror of collimation, optical filter
15, polarizing film 16, to obtain quasi- monochromatic parallel p-polarization light, and to approach the angle of resonance angle, i.e. light intensity type SPR sensitivity most
High corresponding angle is incident in SPR block 2.The optical source wavelength that the present embodiment uses is 632.8nm.SPR block 2 is light intensity type
SPR, including Kretschmann prism 21 and film layer structure 22, resonant excitation is realized in the two cooperation, to detect variations in refractive index.
Wherein, the refractive index of prism 21 is 1.75.Film layer structure 22 is 2 × 10-4Existed under conditions of Pa and 260 DEG C by magnetron sputtering
Prism surface is coated with what 2nm chromium adhesion layer and 50nm golden film obtained.3 acquisition electrode reflected light of imaging detection module is simultaneously imaged,
Reflected light quilt cover battle array CCD32 after imaging lens group 31 in median surface is received.Due to flow battery working electrode, the present invention is used
Carbon felt is in close contact with film layer structure 22, so Carbon felt surface can be imaged in imaging lens group, imaging schematic diagram is as schemed
In shown in 33.Since carbon felt is carbon fiber pilotaxitic texture, interface is caused after contacting with golden film, and there are gap, existing direct golden films
It is contacted between carbon fiber, also there is gap, this provides contrast for imaging.Potential scan device 4 mainly passes through electrochemistry
Work station 43 carries out cyclic voltammetry scanning to electrode, on the one hand obtains the voltage and current variable density curve of electrode totality, separately
On the one hand promote electrolyte that redox reaction occurs by potential scan to generate electrode surface variations in refractive index.Pass through potential
Scanning means carries out potential scan to electrode and electrolyte refractive index at electrode is changed, i.e., SPR reflected light light intensity changes,
It also results in institute to develop at image, therefore can be converted based on the different location intensity value of image living to analyze electrode different location
The difference of property.
Fig. 3 a is the overall diagram of SPR block and potential scan device, and Fig. 3 b is the expanded view of Fig. 3 a.Wherein the present embodiment is adopted
Potential scan is realized with three-electrode system, and three electrodes 46,47,48 are fixed by electrolyte container lid 45 and and electrolyte contacts.
Both in three-electrode system, working electrode 46 is the platinum filament of diameter 1mm, is inserted into carbon felt 42 directly through container cover 45, guarantee
There is lesser contact resistance.The graphite rod for being diameter 3mm to electrode 47, reference electrode 48 are the calomel electrode of diameter 6mm, the two
Electrolyte is immersed to lowest part and container bottom about 5mm, and distance is 10.5mm between them.They are vertical with working electrode 48
Distance is 11.5mm.In electrolyte container 41, carbon felt 42 and SPR block 2 are in close contact using supporting block 44.To guarantee each portion
It is closely connected between part, is additionally provided with prism clip module 51 and fixed block 52, pass through screw 53 for SPR block 2, carbon felt 42, electricity
The connection sealing of liquid container 41 is solved, guarantees that the electrolyte in open containers is not leaked out from gap.Carbon felt body used in the present embodiment
Product is 1 × 1 × 0.5cm3, contact area is 1 × 1cm2。
On the one hand this hatch frame enables incident light that directly carbon felt is imaged, three electricity on the other hand drawn
Pole can directly with electrochemical workstation seamless interfacing.It can guarantee electricity potential scan method in this way, the present embodiment is using circulation
Voltammetry (CV) and optical plasma resonance SPR image can simultaneously detect electrolyte variation at electrode, realize electricity
The on-line checking of pole local reactivity.
Fig. 4 is the CV curve that a three-electrode system is obtained in cyclic voltammetry scanning process by electrochemical workstation
Figure.The present embodiment is using the anode electrolyte in organic quinone flow battery as detection example (Science 327,1363
(2010)), with 2mM Fe (CN)6 4-CV and SPR test as shown in Figure 3, cyclic voltammetry are carried out as electrolyte with 1M KOH
The voltage range of scanning is 0-0.4V, and sweeping speed is 1mV/s.CV-1, CV-2 and CV-3 are respectively first, second and third scanning in figure
The CV curve in period, three's degree of agreement is preferable, shows the stability of electrode performance.
Fig. 5 is the light intensity variation diagram that electrode of liquid flow cell is imaged in SPR optical system.Carbon felt distribution shape is illustrated in Fig. 5 a
Looks, it can be seen that linear is presented in carbon felt, there is light and shade difference.Meanwhile this is the carbon felt being presented on focussing plane, so that
It is deteriorated far from the carbon felt resolving effect on focussing plane.Fig. 5 b-5g represents plot of light intensity of the carbon felt under different potentials and Fig. 5 a makees
The differential chart of difference.
The region variations in refractive index curve is obtained with the change curve of potential by zonule a certain in figure light intensity, and then is obtained
To the change procedure of current density.By taking different regions, two dimensional image different location can be accessed with the electric current of potential
Density Distribution.20 × 20pixel is taken to each zonule in the present embodiment2Square.
Fig. 5 b-5g is that the light intensity of one cycle period of potential in Fig. 4 such as changes, and trend dimmed after first brightening is presented, this
It is consistent with the change procedure of redox reaction in a cycle period.
Fig. 6 a is electrode different location light intensity variation diagram in cyclic voltammetry scanning process, wherein tetra- curves of A, B, C, D
Respectively correspond tetra- positions A, B, C, D in Fig. 5.It can be seen that the light intensity variation presentation mechanical periodicity of four positions is relatively stable
Property, while amplitude is difference, and then show that its current density change has differences.What abscissa characterized in Fig. 6 a is to obtain
A series of timing of plot of light intensity is taken, the temporal resolution of Image Acquisition can reach a millisecond magnitude in experiment.Fig. 6 b is to pass through electric current
Spr signal of A, B, C, D different location that relationship is converted between density and spr signal in second cycle period (CV-2)
Corresponding CV curve.Wherein, the calculating current relative value of the ordinate of Fig. 6 b is to be changed to be converted to by mathematics by light intensity
Relative data value is not specific current value.By with the average CV curve comparison that is obtained in Fig. 4 by electrochemical workstation, two
There are similitudes by person.Meanwhile the CV curve of A, B, C, D different location has fine difference, reflects the activity difference of different location,
Demonstrate the feasibility using the direct detecting electrode activity distribution of SPR optical means.
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 online test method of electrode of liquid flow cell local reactivity, which is characterized in that use surface plasma
The SPR optical system that resonates carries out real time imagery to the electrode surface of flow battery, is become according to the luminous intensity of different location in image
Change, obtain the active judgement of electrode local reaction, the electrode is carbon material electrode.
2. online test method according to claim 1, which is characterized in that the SPR optical system is that prism-coupled is complete
The light intensity type SPR system of internal reflection can obtain the refractive index Two dimensional Distribution of the electrode surface electrolyte while imaging
And real-time change situation.
3. online test method according to claim 1 or 2, which is characterized in that convert the light intensity value of any position
For the current density relative value of the position, the voltage-current density relative value curve of the position is drawn；The electricity of more several positions
Piezo-electric current density relative value curve obtains the reactivity judgement of several positions.
4. online test method according to claim 1 or 2, which is characterized in that the SPR optical system is to electrode surface
While carrying out real time imagery, potential scan is also carried out to the flow battery using potential scan device, and measure the liquid
The electric current of galvanic battery obtains electrode ensemble average voltage-current density curve；Average voltage-the current density plot and institute
The voltage-current density relative value curve comparison for stating any position, obtains the electrode reaction activity judgment of the position, the potential
Scanning is using three-electrode system progress cyclic voltammetry scanning.
5. online test method according to claim 1-3, which is characterized in that the intensity variation passes through
Same position is calculated to obtain in the difference of different potentials or different time imaging Light intensity.
6. a kind of on-line measuring device of electrode of liquid flow cell local reactivity, which is characterized in that use SPR optical system pair
Electrode surface carries out real time imagery, and the SPR optical system includes incident parallel optical module (1), SPR block (2), and imaging
Detecting module (3)；Wherein, the SPR block (2), is light intensity type SPR block, including prism (21) and film layer structure (22),
Described in film layer structure (22) contacted with the electrode of liquid flow cell (42).
7. on-line measuring device according to claim 6, which is characterized in that further include potential scan device (4), the electricity
Gesture scanning means measures the current value of the flow battery using three-electrode system (46,47,48), the three-electrode system (46,
47,48) electrolyte container (41) for being placed in the flow battery by electrolyte container lid (45) is internal.
8. on-line measuring device according to claim 7, which is characterized in that the electrolyte container (41) includes at least one
A side, the electrode (42) are located on the side of the electrolyte container (41).
9. on-line measuring device according to claim 7 or 8, which is characterized in that further include prism clip module (51) and solid
Determine block (52), the prism clip module (51) and the fixed block (52) match, by screw (53) by SPR block (2), electricity
Pole (42), electrolyte container (41) are tightly connected.
10. according to the described in any item on-line measuring devices of claim 7-9, which is characterized in that the electrode (42) is by electrode
Supporting block (44), it is ensured that with the contact of the SPR block (2).
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