CN109724947B - Online detection method and device for electrode local reaction activity of flow battery - Google Patents
Online detection method and device for electrode local reaction activity of flow battery Download PDFInfo
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Abstract
The invention relates to an on-line detection method and device for electrode local reaction activity of a flow battery. The electrode surface is imaged through the SPR optical system to obtain the current density of the electrode local area, so that the current density distribution of different positions on the electrode surface of the flow cell is detected in real time, and a technical tool is provided for representing the active space distribution of the electrode surface.
Description
Technical Field
The invention relates to the technical field of imaging measurement, in particular to an on-line detection method and device for electrode local reaction activity of a flow battery.
Background
The flow battery is one of important ways for realizing effective energy configuration as large-scale energy storage equipment. The flow battery is a high-performance energy storage battery, has the characteristics of high capacity, long service life, easiness in scale production and the like, and is widely concerned. Flow batteries generally use carbon materials (carbon felt, carbon paper, etc.) as electrodes. As an important index for characterizing the performance of the battery, the electrode reaction activity directly affects the efficiency of the battery. The traditional electrical method for characterizing the electrode activity mainly comprises a potential scanning method (linear scanning voltammetry, Cyclic Voltammetry (CV)), a constant current charge-discharge method, an electrochemical impedance spectrum and the like, and the methods can only give out the whole reaction activity of the electrode, for example, the cyclic voltammetry can only collect the average current density change of the electrode after voltage is applied, namely, the activity difference of the modified electrode at different positions cannot be characterized. In consideration of the possible difference of different positions after the carbon felt is modified and activated, it is very important to find a method capable of reflecting the activity of different positions of the electrode in real time in the battery operation process.
Optical detection methods based on Surface Plasmon Resonance (SPR) technology have been applied in the electrochemical field by virtue of their high sensitivity, high resolution, non-contact and non-destructive advantages. SPR is a phenomenon of collective oscillation of metal surface electrons after electromagnetic excitation. The oscillation frequency of SPR has a quantitative relationship with dielectric properties at an interface and can respond very sensitively to changes thereof, and thus it is widely used in the sensing field. SPR also enables imaging due to its advantages for high throughput detection.
The applicant previously proposed a technology for detecting the charging state of the electrolyte and the vanadium ion concentration of the all-vanadium redox flow battery by using a surface plasmon resonance technology, which is disclosed in patent ZL201210097314.9, ZL201210097362.8, ZL 201510724523.5. Considering that the influence of the activity of the electrode on the performance of the flow battery is very important, it is necessary to directly image the surface of the electrode and study the difference of the activity of the electrode. Aiming at the problem, the invention provides a plasma resonance technology based on high sensitivity, high resolution and high flux to realize the imaging of the surface of the electrode of the flow battery and the real-time detection of the current density distribution of different positions of the electrode, and provides a technical tool for representing the active space distribution of the surface of the electrode.
Disclosure of Invention
In view of the defects of the prior art, the invention provides an online detection method and device for electrode local reaction activity of a flow battery.
An online detection method for local reaction activity of an electrode of a flow battery is characterized in that an SPR optical system is adopted to perform real-time imaging on the surface of the electrode, and the local reaction activity of the electrode is judged according to light intensity changes at different positions in an image, wherein the electrode is a carbon material electrode.
Furthermore, the SPR optical system is a prism-coupled total internal reflection light intensity type SPR system, and can obtain the two-dimensional distribution and real-time change condition of the refractive index of the electrolyte on the surface of the electrode during imaging.
Further, converting the light intensity value of any position into a current density relative value of the position, and drawing a voltage-current density relative value curve of the position; and comparing the voltage-current density relative value curves of a plurality of positions to obtain the reaction activity judgment of the compared positions.
Further, when the SPR optical system performs real-time imaging on the surface of the electrode, a potential scanning device is adopted to perform potential scanning on the flow battery, and the current of the flow battery is measured to obtain an electrode integral average voltage-current density curve; and comparing the average voltage-current density curve with the voltage-current density relative value curve at any position to obtain the electrode reaction activity judgment at the position, wherein the potential scanning is cyclic voltammetry scanning by adopting a three-electrode system.
Further, the light intensity variation is obtained by calculating the difference of the light intensity when the same position is imaged at different potentials or different times.
An online detection device for electrode local reaction activity of a flow battery adopts an SPR optical system to perform real-time imaging on the surface of an electrode, wherein the SPR optical system comprises an incident parallel optical module 1, an SPR module 2 and an imaging detection module 3; the light intensity type SPR module 2 comprises a prism 21 and a film structure 22, wherein the film structure 22 is in contact with the flow battery electrode 42.
Further, the device comprises a potential scanning device module 4, wherein the potential scanning device measures the current value of the flow battery by using a three- electrode system 46,47 and 48, and the three- electrode system 46,47 and 48 is placed inside an electrolyte container 41 of the flow battery through an electrolyte container cover 45.
Further, the electrolyte container includes 41 at least one side surface, and the electrode 42 is located on the side surface of the electrolyte container 41.
Further, the device also comprises a prism clamp module 51 and a fixed block 52, wherein the prism clamp module 51 is matched with the fixed block 52, and the SPR module 2, the electrode 42 and the electrolyte container 41 are hermetically connected through a screw 53.
Further, the electrodes 42 are secured in contact with the SPR block 2 by electrode support blocks 44.
The invention has the beneficial effects that: the surface of the electrode is imaged through an optical imaging system to obtain the current density of the local area of the electrode, so that the imaging of the surface of the electrode of the flow battery and the current density distribution of different positions of the electrode are detected in real time, and a technical tool is provided for representing the active space distribution of the surface of the electrode.
Drawings
FIG. 1 is a flow chart of an online detection method for local reaction activity of an electrode of a flow battery in an embodiment.
FIG. 2 is an exploded view of an on-line detection device for local reaction activity of the electrode of the flow battery in the embodiment.
FIG. 3(a) is an overall view of the SPR block and the potential scanning apparatus.
FIG. 3(b) is an expanded view of the SPR block and potential scanning apparatus.
FIG. 4 is a graph of CV curves obtained from cyclic voltammetry scans.
FIG. 5 is a graph of the change in light intensity of SPR optical system imaging the flow cell electrodes.
FIG. 6 (a) is a graph showing the variation of light intensity at different positions of the electrode during the cyclic voltammetry scanning process.
FIG. 6 (b) is a graph of the converted CV for the second cycle period (CV-2) of FIG. 6 a.
Detailed Description
The invention is further illustrated in the following description with reference to the drawings and a preferred embodiment.
The surface plasmon resonance technique can produce a sensitive response to a change in the surface and can achieve high-throughput detection. The invention adopts a Kretschmann prism structure to construct an SPR system, and the electron number density n of the plasma can be known according to the literature (Angew. chem. int. Ed.2017,56, 1629-0Angle of resonance thetaRThere is a quantitative relationship between them. Due to the resonance angle thetaRThe angle corresponding to the position of the minimum value in the reflected light intensity of different angles, and the number density n of electrons0There is a quantitative relationship with the current density J: j ═ n0ev. Where v is the electron velocity. Therefore, the SPR phenomenon can be used to relate the change in the intensity of reflected light to the current density at the corresponding position. During the electrochemical reaction, there are two currents: faraday current and non-faradaic current (electric double layer current). The above quantitative relationship applies only to non-faradaic currents. And for Faraday current, it is mainly the change in refractive index of the electrolyte after redox reaction, i.e.. epsilondA change in (c). And epsilondCan also be such that the resonance angle theta isRChanges occur, i.e. the intensity of the reflected light changes. The faraday current is considered to be the absolute dominant position in the redox reaction considered by the present invention, and therefore only the faraday current is considered. According to the literature (Science 327, 1363(2010)), the change in current density can be obtained by measuring the change in light intensity during the reaction, taking into consideration the relationship between the faraday current density of the redox reaction in electrochemistry and the concentration of active material ions and the like.
Fig. 1 is a flow chart of a main implementation of this embodiment, in which an SPR optical system is used to image the surface of an electrode in real time, and when an electrolyte at the electrode undergoes an oxidation-reduction reaction, active material ions in the electrolyte at the electrode undergo a valence change along with potential change to cause oxidation potential or reduction potential, that is, there is electron transfer, so that a refractive index changes, which can be measured by the light intensity of reflected light. Therefore, the electrode surface images obtained by the SPR optical system represent the activity distribution of different positions of the electrode.
Meanwhile, the current of the flow battery is measured by adopting a traditional electrical method, and the average current density of the whole electrode can be obtained by scanning the potential of the flow battery, so that the curve of the average voltage-current density of the whole electrode is obtained.
In the process of potential scanning, a light intensity image group of the electrode surface is obtained, light intensity signals of a plurality of positions in the image are taken to form a light intensity change curve of each position, and the light intensity change curve is converted into a current density change curve through mathematical conversion. The curve is compared with a voltage-current density curve measured by a traditional electrical method to obtain the reaction activity condition of each position of the electrode.
Fig. 2 is an exploded view of the device of this embodiment. The system comprises an incident parallel optical module 1, an SPR module 2 and an imaging detection module 3, wherein the SPR optical system is formed by the incident parallel optical module, the potential scanning device 4 is used for carrying out cyclic voltammetry scanning on electrodes through an electrochemical workstation in order to carry out quantitative measurement on the surface activity of the electrodes.
The incident parallel light module 1 mainly includes an LED light source 11, an objective lens 12, a diaphragm 13, a collimating lens 14, a filter 15, and a polarizer 16, so as to obtain quasi-monochromatic parallel p-polarized light, and the quasi-monochromatic parallel p-polarized light is incident into the SPR module 2 at an angle close to a resonance angle, that is, at an angle corresponding to the highest sensitivity of light intensity type SPR. The wavelength of the light source used in this example was 632.8 nm. The SPR block 2 is a light intensity SPR and comprises a Kretschmann prism 21 and a film layer structure 22 which are matched to realize resonance excitation so as to detect the change of the refractive index. In this case, the refractive index of the prism 21 is 1.75. The film structure 22 is at 2 x 10-4Plating a 2nm chromium adhesion layer and a 50nm gold film on the surface of the prism by magnetron sputtering under the conditions of Pa and 260 ℃. The imaging detection module 3 collects the electrode reflected light and images, wherein the interface reflected light is received by the area array CCD32 after passing through the imaging lens group 31. Because the flow battery working electrode adopts the carbon felt and is tightly contacted with the film layer structure 22, the imaging lens group can image the surface of the carbon felt, and the imaging schematic diagram is shown as 33 in the figure. Because the carbon felt is of a carbon fiber interweaving structure, a gap exists at an interface after the carbon felt is contacted with the gold film, and the gold film is directly contacted with the carbon fiber and also has a gap, so that the contrast is provided for imaging. The potential scanning device 4 mainly performs cyclic voltammetry scanning on the electrodes through the electrochemical workstation 43, on one hand, a voltage-current density change curve of the whole electrode is obtained, and on the other hand, the potential scanning prompts an electrolyte to perform an oxidation-reduction reaction to generate a refractive index change of the surface of the electrode. The potential scanning device is used for scanning the potential of the electrode, so that the refractive index of the electrolyte at the electrode is changed, namely the light intensity of SPR reflected light is changed, and the formed image is also evolved, and therefore, the difference of the activity of the electrode at different positions can be analyzed on the basis of the intensity value change of the image at different positions.
FIG. 3(a) is an overall view of the SPR block and the potential scanning apparatus, and FIG. 3(b) is an expanded view of FIG. 3(a)Figure (a). In this embodiment, a three-electrode system is used to achieve potential scanning, and the three electrodes 46,47,48 are held in contact with the electrolyte by an electrolyte reservoir cover 45. In the three-electrode system, the working electrode 46 is a platinum wire with the diameter of 1mm, and is directly inserted into the carbon felt 42 through the container cover 45, so that the working electrode and the carbon felt have smaller contact resistance. Counter electrode 47 is a 3mm diameter graphite rod and reference electrode 48 is a 6mm diameter calomel electrode immersed in the electrolyte to the lowest point approximately 5mm from the bottom of the vessel and spaced 10.5mm apart. They are at a vertical distance of 11.5mm from the working electrode 48. In the electrolyte tank 41, the carbon felt 42 is brought into close contact with the SPR module 2 by means of the support block 44. In order to ensure the tight connection among the components, a prism clamp module 51 and a fixed block 52 are further arranged, the SPR module 2, the carbon felt 42 and the electrolyte container 41 are connected and sealed through screws 53, and the electrolyte in the open container is ensured not to leak out of gaps. The volume of the carbon felt used in this example was 1X 0.5cm3Contact area of 1X 1cm2。
The opening structure enables incident light to directly image the carbon felt on one hand, and enables the three led-out electrodes to be in seamless butt joint with an electrochemical workstation directly on the other hand. In this way, an electrical potential scanning method can be ensured, and the Cyclic Voltammetry (CV) and optical plasma resonance SPR images can be used to simultaneously detect the electrolyte change at the electrode, so as to realize the on-line detection of the local reaction activity of the electrode.
FIG. 4 is a CV plot of a three electrode system obtained from an electrochemical workstation during cyclic voltammetry scans. In this example, the positive electrode electrolyte in an organoquinone flow battery was used as an example of detection (Science 327, 1363(2010)) and 2mM Fe (CN)6 4-And 1M KOH as the electrolyte, the voltage range of the cyclic voltammetry sweep was 0-0.4V, and the sweep rate was 1mV/s, as shown in FIG. 3 for CV and SPR tests. CV-1, CV-2 and CV-3 in the figure are CV curves of a first scanning period, a second scanning period and a third scanning period respectively, the coincidence degree of the three is good, and the stability of the electrode performance is shown.
FIG. 5 is a graph of the change in light intensity of SPR optical system imaging the flow cell electrodes. Fig. 5 (a) shows the distribution morphology of the carbon felt, and it can be seen that the carbon felt is linear and has bright and dark differences. At the same time, this is simply the presence of the carbon felt at the focal plane, making the carbon felt less effective at resolving away from the focal plane. FIGS. 5 (b) -5 (g) represent difference graphs of the light intensity plots of the carbon felt at different potentials from FIG. 5 (a).
And obtaining a change curve of the refractive index of a certain small region according to the change curve of the light intensity of the region along with the potential in the graph, and further obtaining the change process of the current density. By taking different areas, the current density distribution of different positions of the two-dimensional image along with the electric potential can be obtained. In the present embodiment, 20 × 20 pixels are taken for each small area2Square of (2).
Fig. 5 (b) -5 (g) show the light intensity change of the potential in fig. 4 for one cycle period, showing the tendency of first becoming brighter and then becoming darker, which is consistent with the change process of the redox reaction in one cycle period.
FIG. 6 (a) is a graph of light intensity variation of different positions of an electrode during cyclic voltammetry scanning, wherein A, B, C, D four curves correspond to A, B, C, D four positions in FIG. 5, respectively. It can be seen that the light intensity changes at the four positions show relative stability of periodic change, and the amplitudes are different, so that the current density changes are different. The abscissa in fig. 6 (a) represents the time sequence for acquiring a series of light intensity maps, and the time resolution of image acquisition in the experiment can reach millisecond order. FIG. 6 (b) is a CV curve corresponding to the SPR signal at the second cycle period (CV-2) for various positions A, B, C, D as transformed by the relationship between current density and SPR signal. Here, the calculated current relative value of the ordinate of fig. 6 (b) is a relative data value obtained by mathematical conversion from the light intensity change, and is not a specific current value. There is similarity between the two by comparison with the average CV curve obtained from the electrochemical workstation in fig. 4. Meanwhile, the CV curves of A, B, C, D at different positions have slight difference, so that the activity difference of different positions is reflected, and the feasibility of directly detecting the electrode activity distribution by using an SPR optical method is verified.
It will be appreciated by those skilled in the art that the foregoing is merely exemplary of the present invention, and is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. An online detection method for local reaction activity of an electrode of a flow battery is characterized in that a Surface Plasmon Resonance (SPR) optical system is adopted to perform real-time imaging on the surface of the electrode of the flow battery, and the local reaction activity of the electrode is judged according to light intensity changes at different positions in an image, wherein the electrode is a carbon material electrode; the SPR optical system is a prism-coupled total internal reflection light intensity type SPR system, and can obtain the two-dimensional distribution and real-time change of the refractive index of the electrolyte on the surface of the electrode while imaging;
the judgment of the local reaction activity of the electrode is obtained according to the light intensity change of different positions in the image, which specifically comprises the following steps: converting the light intensity value of any position into a current density relative value of the position, and drawing a voltage-current density relative value curve of the position; comparing voltage-current density relative value curves of a plurality of positions to obtain the reaction activity judgment of the plurality of positions; potential scanning is carried out on the flow battery by adopting a potential scanning device, and the current of the flow battery is measured to obtain an electrode integral average voltage-current density curve; and comparing the average voltage-current density curve with a voltage-current density relative value curve at any position to obtain the electrode reaction activity judgment at the position.
2. The on-line detection method according to claim 1, wherein the potential scanning is cyclic voltammetry scanning using a three-electrode system.
3. The on-line detection method according to claim 2, wherein the light intensity variation is obtained by calculating the difference of light intensity when the same position is imaged at different potentials or different times.
4. The on-line detection device for the electrode local reaction activity of the flow battery is characterized in that an SPR optical system is adopted to carry out real-time imaging on the surface of an electrode, and the SPR optical system comprises an incident parallel optical module (1), an SPR module (2) and an imaging detection module (3); the SPR module (2) is a light intensity type SPR module and comprises a prism (21) and a film structure (22), wherein the film structure (22) is in contact with the flow battery electrode (42).
5. The on-line detection device of claim 4, further comprising a potential scanning device (4), wherein the potential scanning device measures the current value of the flow battery by using a three-electrode system (46,47,48), and the three-electrode system (46,47,48) is placed inside an electrolyte container (41) of the flow battery through an electrolyte container cover (45).
6. The on-line testing device of claim 5, wherein said electrolyte reservoir (41) comprises at least one side surface, said electrode (42) being located on said side surface of said electrolyte reservoir (41).
7. The on-line detection device of claim 6, further comprising a prism clamp module (51) and a fixed block (52), wherein the prism clamp module (51) and the fixed block (52) are matched, and the SPR module (2), the electrode (42) and the electrolyte container (41) are hermetically connected through screws (53).
8. The on-line detection device of claim 7, wherein the electrodes (42) are secured in contact with the SPR module (2) by electrode support blocks (44).
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| CN109725264B (en) * | 2019-01-22 | 2021-01-01 | 清华大学深圳研究生院 | In-situ detection method and device for current density distribution of flow battery electrode |
| CN109856142B (en) * | 2019-02-22 | 2020-07-31 | 北京化工大学 | Device and method for observing behavior of bubbles on surface of electrode |
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