An electrolysis analysis method and system for bubble behavior visualization and impedance spectrum collaborative characterization

Abstract

The present application relates to the technical field of electrolysis analysis, and particularly relates to an electrolysis analysis method and system for visualizing bubble behavior and cooperatively representing impedance spectrum. The method comprises the following steps: during electrolysis operation, simultaneously starting electrochemical impedance spectrum test and visual observation on the surface of an electrode; obtaining data of electrochemical parameters changing with time in a first time period, and data of bubble behavior changing with time in a total time period, and obtaining data of bubble behavior changing with time in the first time period by intercepting data in a time period corresponding to the first time period from the data of bubble behavior changing with time in the total time period; and then performing correlation analysis on the bubble behavior and the electrochemical parameters. The present application simultaneously performs EIS test and visual experiment, and after time alignment, correlation analysis on the bubble behavior and the electrochemical parameters can be performed, so that the inherent mechanism of the bubble affecting electrolysis is deeply analyzed, the accurate induction factor of electrolysis performance improvement or attenuation is obtained, and operation parameter optimization guidance is provided.

Description

Technical Field

[0001] This invention relates to the field of electrolytic analysis technology, and in particular to an electrolytic analysis method and system that combines bubble behavior visualization with impedance spectroscopy characterization. Background Technology

[0002] Hydrogen energy, as a key green energy carrier for achieving carbon neutrality, has seen its large-scale production technology become a focal point of global scientific research and industrial competition. Among various water electrolysis hydrogen production technologies, anion exchange membrane water electrolysis (AEMWE) technology is widely recognized as a promising next-generation green hydrogen production solution due to its combination of the compatibility of non-precious metal catalysts in alkaline water electrolysis and the system compactness of proton exchange membrane water electrolysis.

[0003] However, this technology faces significant mass transfer challenges in practical applications: under high current density conditions, the oxygen evolution reaction at the anode continuously generates a large number of oxygen bubbles. These bubbles nucleate, grow, and accumulate on the surface and within the pores of the porous transport layer, forming a gaseous capping layer. This severely hinders the effective contact between the electrolyte and the catalytic active sites, leading to an aggravated concentration polarization effect, which in turn causes problems such as increased cell voltage, decreased operating efficiency, and long-term stability degradation.

[0004] Currently, research on bubble behavior in porous transport layers mainly relies on indirect characterization methods such as electrochemical impedance spectroscopy (ACSElectrochem. 2025, 1, 655–666; Nature Catalysis. 2024, 7, 1213–1222), inferring bubble behavior characteristics by analyzing high-frequency resistance fluctuations or equivalent circuit fitting parameters. However, these methods have inherent limitations: first, they obtain macroscopic statistical results, failing to analyze the dynamic evolution of individual bubbles; second, the measurement results are ambiguous, making it difficult to establish accurate structure-property relationships; and third, the lack of in-situ visualization verification makes the research conclusions inferential. Furthermore, offline characterization methods such as scanning electron microscopy can only provide static morphological information before and after the reaction, failing to reflect the true bubble dynamics under operating conditions. Existing technologies lack the ability to directly observe and quantitatively analyze key parameters such as bubble nucleation site distribution, size evolution, detachment kinetics, and surface coverage, severely hindering the rational design and optimization of high-performance porous transport layers.

[0005] Patent document CN119009024A discloses a flow battery testing platform, including a flow battery system, a multi-physics parameter coupling detection system, and a data acquisition system. The multi-physics parameter coupling detection system includes: an optical detection unit for real-time acquisition of internal images of the flow battery to obtain internal image data; an electrolyte detection unit for real-time acquisition of electrolyte concentration data in the storage tank via a micro-sampling circuit; a gas detection unit for real-time acquisition of gas concentration data in the storage tank; and a battery tester for charging and discharging the flow battery and acquiring electrochemical data. The data acquisition system is used to obtain key feature data based on the image data, electrolyte concentration data, and gas concentration data, and calculates corresponding deviation values ​​based on the mapping relationship between the key feature data and preset performance indicators of the flow battery, so as to adjust the operating state of the flow battery according to the deviation values.

[0006] In some implementations, this existing technology combines in-situ gas chromatography with optical visualization techniques to obtain curves showing the changes in bubble behavior parameters and byproduct concentrations over time. It correlates the visualized bubble signals with the chromatographically detected byproduct concentrations, establishing a quantitative relationship between bubble behavior and side reaction kinetics, thus forming a spatiotemporal pattern of bubble evolution. However, this correlation is between a phenomenon (bubbles) and a result (concentration), and can only provide macroscopic monitoring and evaluation of the electrolysis process and optimize bubble management, but it cannot deeply analyze the intrinsic mechanism of the bubble's influence on electrolysis. Summary of the Invention

[0007] The present invention aims to solve the above problems by providing an electrolysis analysis method and system that combines bubble behavior visualization and impedance spectroscopy to deeply analyze the intrinsic mechanism of the influence of bubbles on electrolysis.

[0008] The technical solution to the problem solved by this invention is, in a first aspect, to provide an electrolytic analysis method that combines visualization of bubble behavior with synergistic characterization of impedance spectroscopy, comprising the following steps:

[0009] S1. During electrolysis operation, electrochemical impedance spectroscopy testing and visualization observation of the electrode surface are started simultaneously;

[0010] In the visualization observation, images of bubble behavior in the porous transport layer are continuously acquired to obtain data on how bubble behavior changes over time within the total time period.

[0011] In the electrochemical impedance spectroscopy test, data on the changes of electrochemical parameters over time are obtained within a first time period.

[0012] S2. From the data on the change of bubble behavior over time in the total time period, extract the data within the time period corresponding to the first time period to obtain the data on the change of bubble behavior over time in the first time period;

[0013] S3. Based on the data of bubble behavior changing over time in the first time period and the data of electrochemical parameters changing over time in the first time period, a correlation analysis of bubble behavior and electrochemical parameters is performed.

[0014] In step S1, for electrolysis, as is preferred in this invention, electrolysis is performed in a constant current mode. The current density can be set to 100–400 mA / cm² based on testing requirements. 2 For example, it could be 100 mA / cm 2 150 mA / cm 2 200mA / cm 2 250 mA / cm 2 300 mA / cm 2 350 mA / cm 2 400 mA / cm 2 .

[0015] As a preferred embodiment of the present invention, electrolysis is carried out at a constant temperature. The electrolysis temperature can be set to 25–90°C based on testing requirements; for example, it can be 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 75°C, or 90°C.

[0016] As a preferred embodiment of the present invention, the electrolyte is continuously supplied to the anode chamber via a constant-temperature circulation system at a flow rate of 30–50 mL / min, while the cathode chamber employs a passive water management method. For example, the flow rate can be 30 mL / min, 35 mL / min, 40 mL / min, 45 mL / min, or 50 mL / min.

[0017] The electrolyte concentration is not limited and is set based on the testing requirements. For example, in the AEMWE test, the test condition is 1 M KOH solution; for other test conditions, it can be set to 0–6 M (0 refers to pure water electrolysis, 6 M refers to zinc-air batteries). The method of this invention is applicable to a variety of measurement conditions, including pure water / low-alkali / seawater / high-alkali water electrolyzers, fuel cells, zinc-air batteries, and other electrocatalytic systems (some do not involve gas-producing reactions but only visualize internal changes; others include other bubble behaviors such as adsorption disappearance).

[0018] For visualization observation, the entire dynamic evolution of bubbles can be directly captured, overcoming the speculative limitations of indirect characterization. Preferably, during visualization observation, at least 10 video sequences are acquired each time, each lasting 2-5 seconds, covering no fewer than 100 bubble desorption cycles. This ensures the accuracy and representativeness of the obtained data.

[0019] As a preferred embodiment of the present invention, a high-speed camera is used for visual observation. Preferably, the high-speed camera has a frame rate of 2000–5000 fps, a resolution of not less than 1920×1080 pixels, an adjustable exposure time of 1–50 μs, and is equipped with a microscope lens with a working distance of 5–10 times and a working distance of 100–150 mm.

[0020] As a preferred embodiment of the present invention, during visualization observation, the light source is configured to illuminate from the back or side of the electrolytic cell to ensure clear imaging of bubbles on the PTL surface. Preferably, the light source is a high-brightness LED array light source with a color temperature of 5500–6500 K, equipped with an optical diffuser to achieve a light intensity uniformity of over 90%, and the illuminance is continuously adjustable within a range of 5000–20000 lux.

[0021] As a preferred embodiment of the present invention, bubble behavior images and videos are acquired, and data on the changes in bubble behavior over time within a total time period are extracted based on the videos.

[0022] As a preferred embodiment of the present invention, the bubble behavior is characterized by bubble dynamic parameters, which include at least one of equivalent diameter, diameter distribution, roundness, projected area, generation frequency, growth rate, detachment frequency, and surface coverage. Preferably, each parameter is statistically analyzed based on no fewer than 50 valid bubble samples.

[0023] As a preferred embodiment of the present invention, the bubble dynamic parameters are extracted from the bubble behavior image using an adaptive threshold segmentation algorithm and morphological operations. Preferably, the threshold range is 0.4–0.6, and morphological opening and closing operations are used to optimize contour integrity. The structuring element is a circle with a radius of 3–5 pixels. A reliable image processing algorithm enables the quantitative extraction of key bubble parameters.

[0024] For electrochemical impedance spectroscopy (EIS) testing, as a preferred embodiment of the present invention, the EIS testing is performed with an EIS scan in the frequency range of 100 kHz to 0.1 Hz.

[0025] Electrochemical parameters can be extracted using electrochemical impedance spectroscopy. Preferably, the electrochemical parameter is one of solution resistance, charge transfer resistance, or mass transfer impedance. More preferably, the electrochemical parameter is the mass transfer impedance in the low-frequency region.

[0026] As a preferred embodiment of the present invention, the time synchronization error between the electrochemical impedance spectroscopy test and the visualization observation is less than 0.5 ms, ensuring a precise correspondence between the time series of optical data and electrochemical data.

[0027] In steps S2 and S3, the time series data of bubble behavior and the time series data of electrochemical parameters are time-series aligned for the first time period, which is to associate the processes together.

[0028] In some embodiments, as a preferred embodiment of the present invention, the correlation analysis in step S3 includes at least: calculating the cross-correlation function between the data on the change of bubble behavior over time in the first time period and the data on the change of electrochemical parameters over time in the first time period, so as to determine the correlation strength and lag time between the two changes.

[0029] Based on this, we can understand how one process triggers and drives another. If a significant correlation peak is found with a time delay close to zero, it strongly suggests that the two processes are instantaneously coupled; that is, as the number of bubbles increases, the mass transfer resistance immediately increases. If a fixed time delay exists (e.g., bubble change precedes impedance change), it reveals the relaxation time of the mass transfer response, indicating that bubble change affects mass transfer impedance. Furthermore, this function can directly and quantitatively tell us how much the mass transfer impedance increases for every unit increase in bubble change. This provides direct temporal causal evidence for the mechanism by which bubble behavior leads to mass transfer deterioration.

[0030] In other embodiments, as preferred embodiments of the present invention, in step S1, at least one external operating parameter of the electrolysis process is controlled to operate at at least two different preset levels; the correlation analysis in step S3 includes at least: analyzing the dynamic response process of the bubble behavior and the electrochemical parameters based on the changes in the external operating parameter.

[0031] Based on this, we can understand how external operating parameters affect electrolysis performance by controlling the internal processes of electrolysis. For example, changing the electrolysis temperature results in a synchronous change in bubble diameter and mass transfer impedance. This not only leads to the macroscopic conclusion that increased temperature improves electrolysis performance, but also shows that bubble refinement promotes reaction kinetics. Furthermore, although bubble diameter and mass transfer impedance show the same trend, there is a time difference in their response. This indicates that as the temperature increases, the bubble diameter decreases first, then the mass transfer impedance decreases, ultimately improving electrolysis performance. This establishes the logic of "increased temperature → bubble refinement → optimized mass transfer → improved reaction kinetics".

[0032] Based on the above, it is evident that the present invention can achieve in-depth analysis of the intrinsic mechanism by which bubbles affect electrolysis, accurately identify the causes of electrolysis performance improvement or decline, and provide guidance for optimizing operating parameters.

[0033] Secondly, another objective of the present invention is to provide a system for performing the electrolytic analysis method of visualizing bubble behavior and synergistic characterization of impedance spectroscopy, comprising: an electrolytic cell with a transparent observation window, an image acquisition unit disposed in the transparent observation window, an impedance detection unit, and a synchronization trigger for controlling the image acquisition unit and the impedance detection unit to work synchronously.

[0034] As a preferred embodiment of the present invention, the image acquisition unit includes a high-speed camera.

[0035] As a preferred embodiment of the present invention, the impedance detection unit includes an electrochemical workstation.

[0036] As a preferred embodiment of the present invention, the transparent observation window of the electrolytic cell is located on the anode side of the electrolytic cell, facing the anode PTL surface. The window material is acrylic glass with a thickness of 8 to 12 mm, a light transmittance of ≥92%, and a window size of 25×25 mm to 30×30 mm.

[0037] As a preferred embodiment of the present invention, a light source disposed on the back or side of the electrolytic cell is also included.

[0038] As a preferred embodiment of the present invention, the electrolytic cell is fixed on an optical adjustment frame with three-dimensional fine-tuning function, with an adjustment accuracy of 0.01 mm, to ensure that the PTL surface is precisely located within the depth of field of the camera and the imaging clarity meets the requirements for bubble edge recognition.

[0039] The beneficial effects of this invention are:

[0040] This invention simultaneously performs EIS testing and visualization experiments. After time alignment, it can conduct correlation analysis between bubble behavior and electrochemical parameters, thereby revealing the driving relationship between bubble behavior and mass transfer, the contribution of bubble behavior and mass transfer to electrolysis behavior, and the logical relationship between external operating parameters and electrolysis performance. This enables in-depth analysis of the intrinsic mechanism by which bubbles affect electrolysis, accurate attribution of factors that improve or decrease electrolysis performance, and guidance for optimizing operating parameters.

[0041] If visualization experiments and EIS tests are conducted separately, even with deliberate control of conditions, it is difficult to guarantee that the operating conditions (such as solution concentration, electrode surface state, and airflow disturbance) of the two experiments are completely consistent. Simultaneous testing allows for the observation of bubble behavior and electrochemical response at the same time and location, eliminating errors caused by fluctuations in conditions and making the data more comparable. Attached Figure Description

[0042] Figure 1 This is a schematic diagram of the structure of an electrolytic analysis system that combines bubble behavior visualization with impedance spectroscopy characterization.

[0043] In the diagram: 1. Electrolytic cell; 2. Image acquisition unit; 3. Light source; 4. Impedance detection unit; 5. Synchronous trigger; 6. Computer system; 7. Vibration isolation optical platform.

[0044] Figure 2 These are in-situ observation photographs of the bubble behavior on the PTL surface at different temperatures obtained in Example 2;

[0045] Figure 3 This is a comparative histogram of bubble diameter distribution at different temperatures obtained in Example 2;

[0046] Figure 4 These are the EIS curves obtained at different temperatures in Example 2. Detailed Implementation

[0047] The following are specific embodiments of the present invention, and the technical solution of the present invention will be further described in conjunction with the accompanying drawings. However, the present invention is not limited to these embodiments.

[0048] Example 1

[0049] An electrolysis analysis system that combines bubble behavior visualization with impedance spectroscopy characterization, such as Figure 1 As shown, the system includes: an electrolytic cell 1, an image acquisition unit 2, an impedance detection unit 4, and a synchronization trigger 5 for controlling the start-up error of the image acquisition unit 2 and the impedance detection unit 4 to not exceed 0.5 ms. It also includes a computer system 6 for data processing. A transparent acrylic glass observation window with a thickness of 10 mm and a size of 25 × 25 mm is configured on the anode side of the electrolytic cell 1. The electrolytic cell contains a PTL, membrane electrode assembly, and electrolyte inlet and outlet. The image acquisition unit 2, consisting of a high-speed camera, a microscope lens, and a three-dimensional fine-tuning frame, is positioned at the transparent observation window, facing the window. A light source 3, including an LED backlight and a diffuser plate, is located on the side of the electrolytic cell 1, providing uniform backlighting. The impedance detection unit 4 is an electrochemical workstation with impedance spectroscopy measurement capabilities. All units are mounted on a vibration-isolated optical platform 7.

[0050] During operation, the electrolyte circulates through electrolytic cell 1, the electrochemical workstation provides electrolytic current and performs EIS scanning, and the synchronous trigger 5 simultaneously starts the high-speed camera and the electrochemical workstation to acquire data, thereby realizing in-situ observation of bubble behavior on the PTL surface, synchronous measurement of impedance spectrum, and correlation recording of the two data, providing a data basis for collaborative analysis.

[0051] Example 2

[0052] An electrolytic analysis method combining bubble behavior visualization and impedance spectroscopy characterization, using the system of Example 1, includes the following steps:

[0053] Using commercial 400-mesh double-layer nickel mesh as the PTL substrate, after ultrasonic cleaning with acetone, acid washing and activation, and cleaning with deionized water, it is assembled into an electrolytic cell with an anion exchange membrane and catalyst layer.

[0054] S1. Electrolysis experiment used 1.0 M KOH solution, circulated at a flow rate of 35 mL / min. It was conducted in constant current mode (current density 100 mA cm⁻¹). -2 Electrolysis was performed under [condition missing] conditions, and a high-speed camera system (2000 fps, 1920×1080 pixels, 20 μs exposure time) and an electrochemical workstation were simultaneously activated via a synchronous trigger (time synchronization error less than 0.5 ms). Tests were conducted at 50℃, 60℃, 70℃, and 80℃.

[0055] Video sequences acquired by high-speed camera systems, such as Figure 2 As shown, adaptive threshold segmentation (threshold 0.5) and morphological operations (circular structuring element, radius 3 pixels) are used for processing and analysis to extract bubble dynamic parameters and obtain data on the change of bubble diameter over time in the total time period.

[0056] After electrolysis stabilizes, the electrochemical workstation automatically performs an electrochemical impedance spectroscopy (EIS) scan from 100 kHz to 0.1 Hz to extract electrochemical parameters and obtain data on the change of mass transfer impedance in the low-frequency region over time during the first time period.

[0057] S2. Based on the first time period in the electrochemical impedance spectroscopy, extract the data corresponding to the first time period from the data on the change of bubble diameter over time in the total time period, and obtain the data on the change of bubble diameter over time in the first time period, thus completing the time alignment of bubble diameter and mass transfer impedance.

[0058] S3. Based on the data of bubble diameter changing with time in the first time period and the data of mass transfer impedance changing with time in the first time period, perform a correlation analysis between bubble diameter and mass transfer impedance.

[0059] like Figure 3 , 4 At 50℃, the average bubble diameter on the PTL surface was 566.5 μm, and simultaneous EIS testing showed a charge transfer resistance of 0.0330 Ω. As the electrolysis temperature increased from 50℃ to 80℃, the average bubble diameter on the PTL surface decreased from 566.5 μm to 435.8 μm; simultaneously, the charge transfer resistance measured by EIS significantly decreased, demonstrating that optimized bubble behavior (visualized) resulted in improved mass transfer (impedance). This result directly verifies that increasing the temperature refines the bubbles to optimize the gas-liquid mass transfer process, ultimately improving the electrode reaction kinetics.

[0060] Example 3

[0061] Based on the video sequence and electrochemical impedance spectroscopy obtained by electrolysis at 50°C in Example 2, the following analysis was performed:

[0062] The video sequence was used to obtain the curve of the bubble situation on the electrode surface changing with time: Abubble(t); the low-frequency part of the electrochemical impedance spectroscopy was used to obtain the curve of the mass transfer impedance changing with time: Rm(t); the normalized cross-correlation function of Abubble(t) and Rm(t) was calculated by software, and the lag time was found to be 0.03s and the correlation strength was 0.88.

[0063] The hysteresis time of 0.03 s indicates that changes in bubble behavior lead changes in mass transfer impedance by an average of approximately 0.03 s. This provides direct temporal causal evidence that "bubble behavior is the cause of mass transfer deterioration," and this 0.03 s may be the time required for bubble growth, coalescence, and eventual significant blockage of flow channels or coverage of active sites.

[0064] The correlation strength of 0.88 indicates that, after considering the 0.03s hysteresis effect, the trends of the two have a very strong positive linear correlation. This means that the increase or decrease of bubbles can explain most of the synchronous changes in mass transfer impedance.

[0065] Based on this, a quantitative relationship can be established: Rm(t) = k × Abubble(t - 0.03) + C, where k is the proportionality coefficient and C is the baseline impedance. This transforms a complex physicochemical process into a dynamic model that can be described and predicted.

[0066] Example 4

[0067] Based on the video sequence and electrochemical impedance spectroscopy obtained by electrolysis at 80°C in Example 2, the following analysis was performed:

[0068] The video sequence was used to obtain the curve of the bubble situation on the electrode surface changing with time: Abubble`(t); the low-frequency part of the electrochemical impedance spectroscopy was used to obtain the curve of the mass transfer impedance changing with time: Rm`(t); the normalized cross-correlation function of Abubble`(t) and Rm`(t) was calculated by software, and the lag time was found to be 0.01s and the correlation strength was 0.95.

[0069] Comparative analysis with Example 3:

[0070] As the electrolysis temperature increases, the correlation strength increases, indicating that the synchronicity between bubble behavior and changes in mass transfer impedance is stronger. This suggests that at high electrolysis temperatures, mass transfer loss is more directly and primarily driven by bubble behavior.

[0071] As the electrolysis temperature increases, the hysteresis time shortens, indicating that the response speed of bubble behavior to the influence of mass transfer impedance is greatly accelerated. This is because at higher electrolysis temperatures, bubbles are generated faster and more densely, reaching a state that affects mass transfer more quickly.

[0072] The specific embodiments described herein are merely illustrative of the spirit of the invention. Those skilled in the art to which this invention pertains may make various modifications or additions to the described specific embodiments or use similar methods to substitute them, without departing from the spirit of the invention or exceeding the scope defined by the appended claims.

Claims

1. An electrolytic analysis method that combines visualization of bubble behavior with synergistic characterization of impedance spectroscopy, characterized in that: Includes the following steps: S1. During electrolysis operation, electrochemical impedance spectroscopy testing and visualization observation of the electrode surface are started simultaneously; In the visualization observation, images of bubble behavior in the porous transport layer are continuously acquired to obtain data on how bubble behavior changes over time within the total time period. In the electrochemical impedance spectroscopy test, data on the changes of electrochemical parameters over time are obtained within a first time period. S2. From the data on the change of bubble behavior over time in the total time period, extract the data within the time period corresponding to the first time period to obtain the data on the change of bubble behavior over time in the first time period; S3. Based on the data of bubble behavior changing over time in the first time period and the data of electrochemical parameters changing over time in the first time period, a correlation analysis of bubble behavior and electrochemical parameters is performed.

2. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: The electrochemical parameter is the mass transfer impedance in the low-frequency region.

3. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: The bubble behavior is characterized by bubble dynamic parameters, which include at least one of the following: equivalent diameter, diameter distribution, roundness, projected area, generation frequency, growth rate, detachment frequency, and surface coverage.

4. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 3, characterized in that: The bubble dynamic parameters are extracted from the bubble behavior image using an adaptive threshold segmentation algorithm and morphological operations.

5. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: The correlation analysis includes at least: calculating the cross-correlation function between the data on the change of bubble behavior over time in the first time period and the data on the change of electrochemical parameters over time in the first time period, so as to determine the correlation strength and lag time between the two changes.

6. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1 or 5, characterized in that: In step S1, at least one external operating parameter controlling the electrolysis process operates at at least two different preset levels; The correlation analysis in step S3 includes at least: analyzing the dynamic response process of the bubble behavior and the electrochemical parameters based on changes in the external operating parameters.

7. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: The time synchronization error between the electrochemical impedance spectroscopy test and the visualization observation is less than 0.5 ms.

8. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: In the electrochemical impedance spectroscopy test, an electrochemical impedance spectroscopy scan was performed in the frequency range of 100 kHz to 0.1 Hz.

9. The electrolytic analysis method for combined visualization of bubble behavior and impedance spectroscopy characterization according to claim 1, characterized in that: Electrolysis was carried out in constant current mode with a current density of 100–400 mA / cm².

10. A system for performing an electrolytic analysis method for visualizing bubble behavior and synergistic characterization by impedance spectroscopy as described in any one of claims 1 to 9, characterized in that: include: An electrolytic cell (1) with a transparent observation window, an image acquisition unit (2) and an impedance detection unit (4) set in the transparent observation window, and a synchronization trigger (5) for controlling the image acquisition unit (2) and the impedance detection unit (4) to work synchronously.

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