Experimental system and method for analyzing single phase bubble dynamics

Abstract

The invention provides an experimental system and method for analyzing single phase bubble dynamics. The system comprises a light source module, a galvanometer module, a beam expanding module, a light splitting module, an objective lens, a reaction module, an imaging module and a camera. According to the system, an incidence angle and an azimuth angle of first laser are adjusted through a galvanometer module according to a preset modulation frequency, and the preset modulation frequency is an integral multiple of a preset sampling frequency of a camera. Then, the camera can collect the first reflected light and the first scattered light corresponding to different first azimuth angles within 0-360 degrees, and the first reflected light and the first scattered light are superposed to generate a target body phase bubble image. The system has the imaging capability of high penetration depth and high resolution. Moreover, the interference of trailing in the image can be eliminated, the image noise is also remarkably reduced, the imaging resolution and the imaging quality of the target volume phase bubble image are effectively improved, and the accuracy of analyzing single volume phase bubble dynamics can be effectively improved based on the target volume phase bubble image.

Description

Technical Field

[0001] The present invention relates to the technical field of bubble dynamics analysis, and in particular to an experimental system and method for analyzing the dynamics of a single bulk bubble. Background Art

[0002] Hydrogen is a clean energy source with broad application prospects, offering the advantages of zero carbon emissions, high energy density, and sustainability. Water electrolysis is an important path for scalable hydrogen production, but bubbles generated during the electrolysis process can adhere to the electrode surface, masking active sites and reducing electrolysis efficiency. Therefore, accurately analyzing the growth and dissolution dynamics of bulk bubbles at the scale of individual bubbles is crucial for a deeper understanding and manipulation of bubble behavior.

[0003] However, there is still a lack of technologies and methods that can achieve real-time, high-resolution imaging of the evolutionary behaviors of individual bulk bubbles, such as growth, dissolution, and detachment, in aqueous solutions. Interference scattering imaging is a related technique that is extremely sensitive to weak signals. It uses vertical or near-vertical illumination from a single-directional laser of a specific wavelength. The scattered light from the particles and the reflected light from the substrate interfere with each other and are collected by the camera's CCD.

[0004] However, this interference scattering imaging technology still has problems in the application of imaging single bulk bubbles: there are problems of tailing, noise and strong direction dependence. Specifically, due to the interference of reference light and sample scattered light, traditional interference scattering imaging causes nanoparticles to produce interference tails on the image. The tails of different particles may overlap and interfere with each other, reducing the detection flux of the system. In addition, there is serious noise in the image, which greatly reduces the imaging quality. Moreover, for samples such as non-spherical particles, bubbles, and nanowires, their scattered light is anisotropic, resulting in the inability of interference scattering imaging with single-direction incidence to obtain complete angular information of the scatterer, making it difficult to study the morphology and composition changes of its catalytic conversion process. In this way, it is impossible to accurately capture the image of a single bulk bubble, which leads to low accuracy in the dynamic analysis of a single bulk bubble. Summary of the Invention

[0005] The technical problem to be solved by the present invention is the inability to accurately analyze the dynamics of a single bulk bubble.

[0006] To solve the above technical problems, the present invention provides an experimental system and method for analyzing the dynamics of a single bulk bubble, which specifically adopts the following technical solutions:

[0007] In a first aspect, the present invention provides an experimental system for analyzing the dynamics of a single bulk bubble, comprising: a light source module, a galvanometer module, a beam expander module, a spectrometer module, an objective lens, a reaction module, an imaging module, and a camera. The reaction module includes an imaging substrate. The light source module can be configured to emit a first laser beam of a preset wavelength to the galvanometer module. The galvanometer module can be configured to adjust the incident angle and azimuth of the first laser beam according to a preset modulation frequency, and then transmit a second laser beam corresponding to the adjusted first incident angle and first azimuth angle to the beam expander module, where the first azimuth angle ranges from 0° to 360°. The beam expander module can be configured to expand the second laser beam and transmit a third laser beam after expansion to the spectrometer module. The spectrometer module can be configured to reflect the third laser beam to the objective lens, so that the third laser beam, through the objective lens, illuminates the imaging substrate and a target bulk bubble at the first incident angle and first azimuth angle. The reaction module can be configured to conduct an experiment to generate the target bulk bubble. The spectrometer module can also be configured to transmit the first reflected light from the imaging substrate and the first scattered light from the target bulk bubble to the imaging module. The imaging module can be configured to transmit the first reflected light and the first scattered light to the camera. The camera can be used to generate a target volume bubble image at a preset sampling frequency based on the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360°, for use in volume bubble dynamics analysis; wherein the preset modulation frequency is an integer multiple of the preset sampling frequency.

[0008] This system uses a galvanometer module to adjust the incident angle and azimuth of the first laser, and then uses a camera to collect the first reflected light and the first scattered light. This system can achieve a new type of low-angle rotational interference scattering microscopic imaging with a micron-level imaging depth, and has high penetration depth and high-resolution imaging capabilities. In addition, when the galvanometer module adjusts the incident angle and azimuth of the first laser according to a preset modulation frequency, and this preset modulation frequency is an integer multiple of the camera's preset sampling frequency, the camera can collect the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360°, and superimpose them to generate a target volume phase bubble image. In this way, the interference of tailing in the image can be eliminated, and image noise is also significantly reduced, effectively improving the imaging resolution and imaging quality of the target volume phase bubble image. In addition, based on this target volume phase bubble image, the accuracy of analyzing the dynamics of a single volume phase bubble can be effectively improved.

[0009] In conjunction with the first aspect, in an optional implementation, the light source module includes: a laser and a first lens. The laser can be used to emit a first laser beam according to a preset wavelength. The first lens can be used to collimate the first laser beam.

[0010] In conjunction with the first aspect, in one optional implementation, the galvanometer module includes an x-axis scanning galvanometer and a y-axis scanning galvanometer. Specifically, the x-axis scanning galvanometer and the y-axis scanning galvanometer can be configured to rotate according to a preset modulation frequency to adjust the incident angle and azimuth angle of the first laser to generate the second laser.

[0011] In conjunction with the first aspect, in an optional implementation, the beam expansion module includes: a second lens, a third lens, and a fourth lens arranged sequentially along the same optical axis. The second, third, and fourth lenses are all plano-convex lenses; the convex surface of the second lens is arranged in the direction of incidence of the second laser, the convex surface of the third lens is arranged in the opposite direction to the convex surface of the second lens, and the convex surface of the fourth lens is arranged opposite to the convex surface of the third lens. The second and third lenses are used to expand the second laser beam, and the fourth lens is used to converge the diffused second laser beam to emit the third laser beam.

[0012] In combination with the first aspect, in an optional implementation, the objective lens is an oil immersion objective lens, and the numerical aperture of the objective lens is greater than or equal to 0.9.

[0013] In conjunction with the first aspect, in one optional implementation, the reaction module further comprises: a reaction cell, an electrode assembly, and a potential control device. The reaction cell is disposed on an imaging substrate, the electrode assembly is disposed on the imaging substrate and within the reaction cell, and the potential control device is connected to the electrode assembly. Specifically, the reaction cell is used to hold an experimental medium for generating target bulk bubbles. The potential control device is used to control the electrode assembly to output a preset potential.

[0014] In conjunction with the first aspect, in an optional implementation, the imaging module includes a reflector and a fifth lens. The reflector can be configured to reflect the first reflected light and the first scattered light to the fourth lens. The fifth lens can be configured to converge the first reflected light and the first scattered light to the camera.

[0015] In conjunction with the first aspect, in an optional implementation, the imaging module further includes: a sixth lens, a seventh lens, and an aperture; the sixth and seventh lenses are disposed between the reflector and the fourth lens, forming a 4f optical path system; and the aperture is disposed between the sixth and seventh lenses. The sixth and seventh lenses can be configured to transmit the first reflected light and the first scattered light. The aperture can be configured to filter the first reflected light and the first scattered light.

[0016] In combination with the first aspect, in an optional implementation, the imaging substrate is one of the following: a glass sheet, a gold-plated glass sheet, indium tin oxide, or a metal film.

[0017] In a second aspect, the present invention provides an experimental method for analyzing the dynamics of a single bulk bubble. The method comprises: first, establishing the experimental system provided by the first aspect and any optional implementation described above. Then, conducting an experiment using a reaction module to generate a target bulk bubble. Next, moving the reaction module to determine a sampling area of ​​an objective lens, wherein the sampling area includes the target bulk bubble. Next, a light source module emits a first laser beam of a preset wavelength to a galvanometer module. The galvanometer module adjusts the incident angle and azimuth of the first laser beam according to a preset modulation frequency, and directs a second laser beam corresponding to the adjusted first incident angle and first azimuth angle into a beam expansion module, wherein the first azimuth angle ranges from 0° to 360°. The beam expansion module expands the second laser beam, and the expanded third laser beam is directed into a spectrometer module. The spectrometer module reflects the third laser beam to the objective lens, so that the third laser beam illuminates an imaging substrate and the target bulk bubble through the objective lens at the first incident angle and first azimuth angle. The spectrometer transmits the first reflected light from the imaging substrate and the first scattered light from the target bulk bubble to the imaging module. The imaging module transmits the first reflected light and the first scattered light to a camera. Finally, a target volume bubble image is generated by the camera at a preset sampling frequency based on the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360° for volume bubble dynamics analysis; wherein the preset modulation frequency is an integer multiple of the preset sampling frequency.

[0018] In a third aspect, the present invention provides an electronic device comprising: a memory, one or more processors; the memory is coupled to the processor; wherein the memory stores computer program code, the computer program code comprises computer instructions, and when the computer instructions are executed by the processor, the electronic device executes the method provided in the second aspect above.

[0019] In a fourth aspect, the present invention provides a computer-readable storage medium comprising computer instructions. When the computer instructions are executed on an electronic device, the electronic device executes the method provided in the second aspect.

[0020] It can be understood that the beneficial effects that can be achieved by the experimental method for analyzing the dynamics of a single bulk bubble provided in the second aspect, the electronic device in the third aspect, and the computer-readable storage medium in the fourth aspect can be referred to the beneficial effects in the first aspect and any possible design method thereof, and will not be repeated here. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A schematic diagram of the framework of an experimental system for analyzing the dynamics of a single bulk bubble provided in an embodiment of the present application;

[0022] Figure 2 Schematic diagram of the structure of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application Figure 1 ;

[0023] Figure 3 A schematic diagram of the structure of the reaction module provided in the embodiment of the present application;

[0024] Figure 4 Schematic diagram of the structure of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application Figure 2 ;

[0025] Figure 5 A schematic diagram of the imaging results of silver nanoparticles provided in an embodiment of the present application;

[0026] Figure 6 A schematic diagram of a silver nanowire imaging test provided in an embodiment of the present application;

[0027] Figure 7 A schematic flow chart of an experimental method for analyzing the dynamics of a single bulk bubble provided in an embodiment of the present application;

[0028] Figure 8 A schematic diagram of a target bulk bubble image collected during the bulk bubble growth process during the electrocatalytic hydrogen evolution process provided in an embodiment of the present application;

[0029] Figure 9 A schematic diagram of the growth dynamics analysis results of a single bulk bubble provided in an embodiment of the present application;

[0030] Figure 10 A schematic diagram of the results of regulating the growth process of bulk bubbles at the same position provided in an embodiment of the present application;

[0031] Figure 11 Schematic diagram of the results of analyzing and measuring the dissolution kinetics of a single bulk bubble provided in the examples of this application. DETAILED DESCRIPTION

[0032] The following embodiments are described in detail, with examples illustrated in the accompanying drawings. When the following description refers to the drawings, identical numerals in different figures represent identical or similar elements unless otherwise indicated. The embodiments described in the following embodiments are not intended to represent all possible implementations consistent with the present application. They are merely examples of systems and methods consistent with certain aspects of the present application, as detailed in the claims.

[0033] Hydrogen is a clean energy source with broad application prospects, offering the advantages of zero carbon emissions, high energy density, and sustainability. Water electrolysis is an important path for scalable hydrogen production, but bubbles generated during the electrolysis process can adhere to the electrode surface, masking active sites and reducing electrolysis efficiency. Therefore, accurately analyzing the growth and dissolution dynamics of bulk bubbles at the scale of individual bubbles is crucial for a deeper understanding and manipulation of bubble behavior.

[0034] However, there is still a lack of technologies and methods that can achieve real-time, high-resolution imaging of the evolutionary behaviors of individual bulk bubbles, such as growth, dissolution, and detachment, in aqueous solutions. Interference scattering imaging is a related technique that is extremely sensitive to weak signals. It uses vertical or near-vertical illumination from a single-directional laser of a specific wavelength. The scattered light from the particles and the reflected light from the substrate interfere with each other and are collected by the camera's CCD.

[0035] However, this interference scattering imaging technology still has problems in the application of imaging single bulk bubbles: there are problems of tailing, noise and strong direction dependence. Specifically, due to the interference of reference light and sample scattered light, traditional interference scattering imaging causes nanoparticles to produce interference tails on the image. The tails of different particles may overlap and interfere with each other, reducing the detection flux of the system. In addition, there is serious noise in the image, which greatly reduces the imaging quality. Moreover, for samples such as non-spherical particles, bubbles, and nanowires, their scattered light is anisotropic, resulting in the inability of interference scattering imaging with single-direction incidence to obtain complete angular information of the scatterer, making it difficult to study the morphology and composition changes of its catalytic conversion process. In this way, it is impossible to accurately capture the image of a single bulk bubble, which leads to low accuracy in the dynamic analysis of a single bulk bubble.

[0036] In order to solve the above problems, the embodiments of the present application provide an experimental system and method for analyzing the dynamics of a single bulk bubble. The experimental system and method can realize a new type of microscopic imaging of low-angle rotational interference scattering with a micron-level imaging depth, have high penetration depth and high-resolution imaging capabilities, and can effectively eliminate the influence of tailing and noise, improve the imaging quality of bulk bubbles, and thus effectively improve the accuracy of analyzing the dynamics of a single bulk bubble.

[0037] The following describes the solution provided by the embodiments of the present application in conjunction with the accompanying drawings.

[0038] Specifically, Figure 1 A schematic diagram of the framework of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application is shown in FIG. Figure 1 As shown, the experimental system for analyzing the dynamics of a single bulk bubble provided in an embodiment of the present application specifically includes: a light source module 1, a galvanometer module 2, a beam expansion module 3, a spectrometer module 4, an objective lens 5, a reaction module 6, an imaging module 7 and a camera 8.

[0039] Continue to see Figure 1First, the light source module 1 emits a first laser. The first laser is modulated at a preset modulation frequency by the galvanometer module 2 to adjust the incident angle and azimuth angle, and then outputs a second laser. The second laser is then expanded by the beam expansion module 3 to output a third laser. The third laser is then reflected by the spectroscopic module 4 and irradiated through the objective lens 5 onto the imaging substrate 61 and the target bulk bubble A of the reaction module 6. Furthermore, the reflected light from the imaging substrate 61 and the scattered light (i.e., mixed light) from the target bulk bubble A are transmitted through the spectroscopic module 4 and then transferred through the imaging module 7 to the camera 8. The camera 8 generates an image of the target bulk bubble at a preset sampling frequency for use in bulk bubble dynamics analysis.

[0040] Specifically, the light source module 1 can be used to emit a first laser of a preset wavelength to the galvanometer module 2. For example, the preset wavelength can be 660nm or 532nm. The preset wavelength can be set according to the actual experimental requirements and is not specifically limited in this application.

[0041] In some embodiments, Figure 2 Schematic diagram of the structure of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application Figure 1 ,like Figure 2 As shown, the light source module 1 specifically includes: a laser 11 and a first lens 12. The laser 11 can be used to emit a first laser according to a preset wavelength; the first lens 12 can be used to collimate the first laser.

[0042] The galvanometer module 2 can be used to adjust the incident angle and azimuth angle of the first laser according to a preset modulation frequency, and emit the second laser corresponding to the adjusted first incident angle and first azimuth angle into the beam expansion module 3, and the range of the first azimuth angle is 0°-360°. Specifically, the incident angle (or first incident angle) is the angle between the laser (i.e., the third laser) emitted by the objective lens 5 and the normal direction perpendicular to the imaging substrate 61. The azimuth angle (or first azimuth angle) is the azimuth angle of the laser (i.e., the third laser) emitted by the objective lens 5 projected on the plane of the imaging substrate 61. The galvanometer module 2 can change the first azimuth angle within 0°-360° within a modulation cycle of the preset modulation frequency, and make the first azimuth angle change one circle (i.e., 360°) within one modulation cycle. In addition, the preset modulation frequency is an integer multiple of the preset sampling frequency. In this way, the effects of trailing and noise in the target body phase bubble imaging can be eliminated.

[0043] In some embodiments, as Figure 2 As shown, the galvanometer module 2 includes an x-axis scanning galvanometer 21 and a y-axis scanning galvanometer 22. The x-axis scanning galvanometer 21 and the y-axis scanning galvanometer 22 are used to rotate according to a preset modulation frequency to adjust the incident angle and azimuth angle of the first laser to obtain the second laser.

[0044] In one implementation, the galvanometer module 2 further includes a data acquisition card and a galvanometer module software control program. For example, the galvanometer module software control program, written in MATLAB code, can control the rotation of the x-axis scanning galvanometer mirror 21 and the y-axis scanning galvanometer mirror 22 to achieve periodic modulation of the galvanometer mirror angles, thereby varying the incident angle and azimuth angle of the first laser beam.

[0045] The beam expansion module 3 can be used to expand the second laser beam and emit the expanded third laser beam into the beam splitting module 4 .

[0046] In some embodiments, as Figure 2 As shown, the beam expansion module 3 specifically includes: a second lens 31, a third lens 32, and a fourth lens 33 arranged in sequence along the same optical axis; the second lens 31, the third lens 32, and the fourth lens 33 are all plano-convex lenses; the convex surface of the second lens 31 is arranged in the direction of incidence of the second laser, the convex surface of the third lens 32 is arranged in the opposite direction to the convex surface of the second lens 31, and the convex surface of the fourth lens 33 is arranged opposite to the convex surface of the third lens 32. The second lens 31 and the third lens 32 can be used to expand the second laser beam, and the fourth lens 33 is used to converge the diffused second laser beam to expand the beam and emit the third laser beam.

[0047] For example, the focal lengths of the second lens 31, the third lens 32, and the fourth lens 33 can be 60 mm, 250 mm, and 500 mm, respectively. In order to achieve beam expansion of the second laser, the focal length of the third lens 32 needs to be greater than that of the second lens 31. The specific beam expansion factor can be determined based on actual experimental requirements and system design. For example, the beam expansion factor is generally between 1.5 and 5 times. The lower limit of the focal length of the fourth lens 33 is determined by the physical distance from the fourth lens 33 to the objective lens 5. The specific focal length of the fourth lens 33 can be determined based on the spot size of the incident light focused on the imaging substrate 61. The spot size must meet the requirements of the actual experiment.

[0048] The light splitting module 4 can be used to reflect the third laser light to the objective lens 5 , so that the third laser light irradiates the imaging substrate 61 and the target volume phase bubble at the first incident angle and the first azimuth angle through the objective lens 5 .

[0049] In some embodiments, the objective lens 5 may be an oil immersion objective lens, and the numerical aperture (NA) of the objective lens 5 may be greater than or equal to 0.9. For example, the NA of the objective lens 5 may be 1.49. Using an oil immersion objective lens for the objective lens 5 can effectively improve the imaging resolution and imaging contrast of the experimental system.

[0050] The reaction module 6 can be used to conduct experiments to generate target bulk bubbles. The reaction module 6 is a chemical reaction or electrochemical reaction module that can perform real-time observation of the growth and dissolution of bulk bubbles during the electrocatalytic hydrogen evolution process.

[0051] In some embodiments, Figure 3 The schematic diagram of the reaction module provided in the embodiment of the present application is as follows: Figure 3 As shown, the reaction module 6 may include an imaging substrate 61, a reaction cell 62, an electrode assembly 63, and a potential control device 64. The reaction cell 62 is disposed on the imaging substrate 61, the electrode assembly 63 is disposed on the imaging substrate 61 and within the reaction cell 62, and the potential control device 64 is connected to the electrode assembly 63. The reaction cell 62 is used to hold the experimental medium for generating target bulk bubbles. The potential control device 64 can be used to control the electrode assembly 63 to output a preset potential.

[0052] In some embodiments, the imaging substrate 61 is made of a material with high light transmittance. Specifically, the imaging substrate 61 can be one of the following: a glass sheet, a gold-coated glass sheet, indium tin oxide, or a metal film. The glass sheet can be a BK-7 glass sheet. The gold-coated glass sheet can be composed of a BK-7 glass sheet covered with a 2 nm thick Cr adhesion layer and a 5 nm thick Au film.

[0053] The reaction cell 62 may be a polydimethylsiloxane (PDMS) cell, the electrode device 63 may include a reference electrode (RE), a counter electrode (CE), and a working electrode (WE), and the potential control device 64 may be an electrochemical workstation.

[0054] The spectroscopic module 4 may also be configured to transmit the first reflected light of the imaging substrate 61 and the first scattered light of the target bulk bubbles to the imaging module 7 .

[0055] In some embodiments, the light splitting module 4 may be a non-polarized half-reflecting half-mirror lens. In this way, the light splitting module 4 can effectively reflect the third laser light and transmit the first reflected light and the first scattered light.

[0056] The imaging module 7 may be configured to transmit the first reflected light and the first scattered light to the camera 8 .

[0057] In some embodiments, as Figure 2 As shown, imaging module 7 may include a reflector 71 and a fifth lens 72. Fifth lens 72 may be a plano-convex lens, with the convex surface of fifth lens 72 facing the incident direction of the first reflected light and the first scattered light. Reflector 71 may be configured to reflect the first reflected light and the first scattered light toward fifth lens 72; fifth lens 72 may be configured to converge the first reflected light and the first scattered light toward camera 8.

[0058] In some embodiments, in order to implement filtering processing on the optical signal (eg, the first reflected light and the first scattered light). Figure 4Schematic diagram of the structure of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application Figure 2 ,like Figure 4 As shown, the imaging module 7 may further include a sixth lens 73, a seventh lens 74, and an aperture 75. The sixth and seventh lenses 73, 74 are disposed between the reflector 71 and the fifth lens 72, forming a 4f optical path system. The aperture 75 is disposed between the sixth and seventh lenses 73, 74. The sixth and seventh lenses 73, 74 may be used to transmit the first reflected light and the first scattered light; the aperture 75 may be used to filter the first reflected light and the first scattered light.

[0059] For example, the focal lengths of the fifth lens 72, the sixth lens 73, and the seventh lens 74 can be 200 mm, 100 mm, and 180 mm, respectively. The fifth lens 72 is an imaging lens, the sixth lens 73 serves as the objective lens in the imaging module 7, and the seventh lens 74 is another imaging lens. The sixth and seventh lenses 73 and 74 form an asymmetric 4f optical path system, facilitating optical path modification and signal filtering. An aperture 75 is added to the Fourier plane between the sixth and seventh lenses 73 and 74 to achieve high-frequency filtering.

[0060] Camera 8 is an inductively coupled device that can be used to generate a target volume bubble image at a preset sampling frequency based on the first reflected light and first scattered light corresponding to different first azimuth angles between 0° and 360° for volume bubble dynamics analysis. The target volume bubble image can include a single volume bubble or multiple volume bubbles. In other words, the experimental system can simultaneously capture images of multiple volume bubbles, improving the efficiency of analyzing the dynamics of a single volume bubble.

[0061] Specifically, because the first reflected light and the first scattered light are simultaneously captured by camera 8, they interfere with each other, resulting in parabolic smearing in the image. Therefore, in this embodiment of the present application, camera 8 collects the first reflected light and the first scattered light corresponding to different first azimuth angles within a range of 0°-360° at a preset sampling frequency, superimposing them to generate a target volume phase bubble image. This way, the smears generated by single-angle incidence cancel each other out, thereby improving the imaging quality of the target volume phase bubble image.

[0062] The experimental system for analyzing the dynamics of a single bulk bubble provided by the embodiment of the present application (hereinafter referred to as: the experimental system) is used. The experimental system adjusts the incident angle and azimuth angle of the first laser through the galvanometer module, and then collects the first reflected light and the first scattered light through the camera, which can realize a new type of low-angle rotational interference scattering microscopic imaging with a micron-level imaging depth, and has high penetration depth and high-resolution imaging capabilities. In addition, the galvanometer module adjusts the incident angle and azimuth angle of the first laser according to a preset modulation frequency, and when the preset modulation frequency is an integer multiple of the preset sampling frequency of the camera, the camera can collect the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360°, and superimpose them to generate a target bulk bubble image. In this way, the interference of tailing in the image can be eliminated, and the image noise is also significantly reduced, effectively improving the imaging resolution and imaging quality of the target bulk bubble image, and then based on the target bulk bubble image, the accuracy of analyzing the dynamics of a single bulk bubble can be effectively improved.

[0063] In some embodiments, this experimental system is used to compare imaging effects. Specifically, this experimental system can adjust the incident angle and azimuth angle of the first laser through the galvanometer module 2, that is, control the angle at which the first laser is focused on the rear focal plane of the objective lens 5 to achieve illumination at different azimuth angles. Then, by setting the exposure time of the camera 8 (i.e., presetting the sampling frequency), an image of the target bulk bubble without tailing interference is obtained, thereby achieving high-resolution imaging at the single nanoparticle level.

[0064] Figure 5 This is a schematic diagram of the imaging results of silver nanoparticles provided in the examples of this application. Specifically, Figure 5 (a) is a schematic diagram of the imaging results of silver nanoparticles when the first azimuth angles are 0°, 90°, 180° and 270° respectively. Figure 5 As shown in (a), for the same silver nanoparticle, when incident at a single azimuth angle, there is obvious tailing and severe noise in the image, and the azimuth angle of the incident light has a significant effect on the tailing direction. Figure 5 (b) is a schematic diagram of the imaging results of silver nanoparticles generated by superimposing the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360°. Figure 5 As shown in (b), after averaging the signals from multiple frames at different azimuth angles, the target bulk bubble image eliminates smearing and significantly reduces noise. For the same silver nanoparticle, the contrast and resolution of the target bulk bubble image generated by this application are significantly improved compared to imaging at a single azimuth angle. Therefore, this experimental system can effectively achieve high-resolution and high-throughput imaging at the single nanoparticle level.

[0065] In some embodiments, the present experimental system is used to perform silver nanowire imaging tests. Specifically, the present experimental system can adjust the incident angle and azimuth angle of the first laser through the galvanometer module 2, that is, control the angle at which the first laser is focused on the rear focal plane of the objective lens 5, and realize illumination at different azimuth angles. Different degrees of filtering processing is performed through the imaging module 7, and then the first reflected light and the first scattered light corresponding to different first azimuth angles are collected by setting the camera 8 to be superimposed to generate a target bulk bubble image, thereby achieving high-contrast imaging at the level of single nanoparticles. After imaging testing, the incident angle used by the present experimental system is 18.1°, which is much lower than the total internal reflection incident angle of 61.8°. Taking the tilted silver nanowires in a low ionic strength solution as the probe, the imaging depth of the present experimental system is significantly improved compared to that of the total internal reflection incident, and it has great application potential in the research of particle sedimentation, nanoparticle reaction and bulk bubble growth.

[0066] For example, Figure 6 This is a schematic diagram of the silver nanowire imaging test provided in the embodiment of the present application. Specifically, Figure 6 (a) shows the geometric parameters and interference diagram of a tilted silver nanowire. The tilt angle of the silver nanowire is γ, and the height from the other end of the silver nanowire to the imaging substrate is h. Figure 6 (b) is a comparison of the imaging effects of a single tilted silver nanowire and a horizontal silver nanowire. Figure 6 Figure (c) shows the intensity distribution of a single tilted silver nanowire. In this experimental system, the incident light (i.e., the third laser, Ei) illuminates the nanoparticles at an angle far below the angle of total internal reflection. For a single tilted silver nanowire, the image captured by the camera in this invention includes information about the reflected light (Er) from the imaging substrate and the scattered light (Es) at different heights along the nanowire. Combining the principles of interference and the angle of incidence, it can be calculated that the height h at the other end of the silver nanowire is approximately 6.06 μm, and the tilt angle γ is approximately 15.82°.

[0067] The present invention also provides an experimental method for analyzing the dynamics of a single bulk bubble. Figure 7 A schematic flow chart of the experimental method for analyzing the dynamics of a single bulk bubble provided in the embodiments of the present application is shown in FIG. Figure 7 As shown, the method includes the following steps S701-S705:

[0068] S701. Build an experimental system for analyzing the dynamics of a single bulk bubble as described in the above embodiment.

[0069] S702: Conducting an experiment through a reaction module to generate target bulk bubbles.

[0070] S703 , moving the reaction module to determine the sampling area of ​​the objective lens, where the sampling area includes the target bulk phase bubble.

[0071] S704. The first laser of a preset wavelength is emitted to the galvanometer module through the light source module. The incident angle and azimuth angle of the first laser are adjusted according to the preset modulation frequency through the galvanometer module, and the second laser corresponding to the adjusted first incident angle and first azimuth angle is emitted into the beam expansion module, and the range of the first azimuth angle is 0°-360°. The second laser is expanded by the beam expansion module, and the expanded third laser is emitted into the spectrometer module. The third laser is reflected to the objective lens by the spectrometer module, so that the third laser irradiates the imaging substrate and the target body phase bubble at the first incident angle and the first azimuth angle through the objective lens. The first reflected light of the imaging substrate and the first scattered light of the target body phase bubble are transmitted to the imaging module through the spectrometer module. The first reflected light and the first scattered light are transmitted to the camera through the imaging module.

[0072] S705. Generate a target volume bubble image using a camera at a preset sampling frequency based on the first reflected light and the first scattered light corresponding to different first azimuth angles within a range of 0°-360° for volume bubble dynamics analysis; wherein the preset modulation frequency is an integer multiple of the preset sampling frequency.

[0073] By adopting the experimental method for analyzing the dynamics of a single bulk bubble provided in an embodiment of the present application, the incident angle and azimuth angle of the first laser are adjusted by the galvanometer module, and the first reflected light and the first scattered light are collected by the camera, so that a new type of low-angle rotational interference scattering microscopic imaging with a micron-level imaging depth can be achieved, which has a high penetration depth and high-resolution imaging capability. In addition, by adjusting the incident angle and azimuth angle of the first laser according to a preset modulation frequency by the galvanometer module, and when the preset modulation frequency is an integer multiple of the preset sampling frequency of the camera, the camera can collect the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360° and superimpose them to generate a target bulk bubble image. In this way, the method can eliminate the interference of tailing in the image, and the image noise is also significantly reduced, effectively improving the imaging resolution and imaging quality of the target bulk bubble image, and then based on the target bulk bubble image, the accuracy of analyzing the dynamics of a single bulk bubble can be effectively improved.

[0074] In some embodiments, the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiments of the present application can be used to analyze and measure the growth dynamics of a single bulk bubble during electrocatalytic hydrogen evolution. The specific steps include:

[0075] First, Pt nanoparticles were loaded onto the gold film. Specifically, the Pt nanoparticles were dispersed in a 0.1M Na2SO4 solution and allowed to settle for 10 minutes. The salt solution was then removed, and the substrate was rinsed with deionized water and finally dried with nitrogen.

[0076] Next, build an electrochemical reaction cell and complete focusing. Specifically, adhere the reaction cell (e.g., a PDMS cell, polydimethylsiloxane cell, 0.8 cm × 0.8 cm × 0.9 cm) to the Pt particle-loaded gold-coated glass imaging substrate, add 0.05M H2SO4 as the electrolyte solution, set the parameters of the galvanometer module 2 (i.e., the rotation angles of the x-axis scanning galvanometer and the y-axis scanning galvanometer), and complete focusing.

[0077] Next, conduct an electrochemical experiment and determine the sampling area. Using a potential control device (e.g., an electrochemical workstation), set the cathode (working electrode) potential to -0.8 V (vs. Ag / AgCl). Continue moving the reaction module's translation stage to identify the area where bulk bubbles are generated and secure it as the sampling area.

[0078] Finally, a first laser with a preset wavelength is emitted through the light source module, and a target body phase bubble image is generated according to the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360° through the camera at a preset sampling frequency.

[0079] For example, Figure 8 A schematic diagram of a target bulk bubble image collected during the bulk bubble growth process during the electrocatalytic hydrogen evolution process provided in an embodiment of the present application is shown in FIG. Figure 8 As shown in the figure, when the voltage is -0.8V (relative to the Ag / AgCl reference), a single bulk bubble grows and detaches near the Pt nanoparticle cluster in the sampling area. Due to the interference between the light reflected from the bubble at different heights, the bubble exhibits a Newton's ring interference pattern. The continuous changes in the bubble height and radius also cause the size of the Newton's ring and the brightness of the center to change.

[0080] For example, Figure 9 This is a schematic diagram of the results of the analysis of the growth dynamics of a single bulk bubble provided in the examples of this application. Specifically, Figure 9 (a) is a graph showing the change of bubble radius over time during the growth of four consecutive bulk bubbles at the same position at -0.8V. Figure 9 As shown in (a), using the Newton ring model, the change of bubble radius with time during the growth of four consecutive phase bubbles at the same position is obtained. Figure 9 (b) is Figure 9 The kinetic fitting diagram of the growth process of the first bulk bubble in (a) is as follows: Figure 9 As shown in (b), the growth process of the first bulk bubble was dynamically fitted, and it was found that the bulk bubble satisfies R = β·t 0.5 (R represents the bubble radius; β represents the growth coefficient; t represents the growth time), indicating that the growth of the bulk bubble is controlled by diffusion. Figure 9 (b) is Figure 9 The motion trajectory of the four bulk bubble centers in the x / y plane in (c) is as follows: Figure 9 As shown in (c), the movement trajectories of the bubble centers during the growth of four consecutive bulk bubbles at the same position were statistically analyzed. It can be seen that the growth and detachment of the bulk bubbles show significant periodicity. The effective observation of this phenomenon is based on the high penetration depth of the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiment of the present application.

[0081] In some embodiments, the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiments of the present application can be used to implement a method for regulating the growth process of a bulk bubble at the same location using the cathode potential (e.g., working electrode WE). The specific steps include:

[0082] First, Pt nanoparticles were loaded onto the gold film.

[0083] Then, build an electrochemical reaction cell to complete the focusing.

[0084] Next, conduct an electrochemical experiment and determine the sampling area. Using a potential control device (e.g., an electrochemical workstation), set the cathode (working electrode) potential to -0.8 V (vs. Ag / AgCl). Continue moving the reaction module's translation stage to identify the area where bulk bubbles are generated and secure it as the sampling area.

[0085] Finally, starting from -0.8 V, the cathode potential was set to -1.0 V, -1.2 V, -1.4 V, -1.6 V, -1.8 V, and -2.0 V, respectively, and samples were taken for 30-40 seconds. Each time the cathode potential was changed, air bubbles in the reaction cell needed to be manually removed using a pipette.

[0086] For example, Figure 10 This is a schematic diagram of the results of regulating the growth process of bulk bubbles at the same position provided in the embodiment of the present application. Specifically, Figure 10 (a) is the growth curve of a single bulk bubble under different voltages, such as Figure 10 As shown in (a), for the same position, the growth coefficient of the bulk bubble increases as the cathode potential decreases. However, when the cathode potential drops to -1.6 V, the growth of the bulk bubble begins to plateau, and even if the cathode potential continues to decrease, the growth coefficient hardly increases. Figure 10 (b) is a piano-shaped diagram of the detachment radius of multiple bulk bubbles at different voltages. Figure 10 (c) is a scatter plot of the y-direction coordinates of the bubble center when multiple bulk bubbles detach under different voltages. Figure 10 (d) is a scatter plot of the x-direction coordinates of the bubble center when multiple bulk bubbles detach under different voltages. Figure 10As shown in (b)-(d), as the cathode potential decreases to -1.6 V, the distribution range of the detachment radius of the bulk bubble when it leaves the imaging field of view begins to suddenly increase, and the center position of the bubble at the time of detachment also begins to oscillate violently, indicating that as the cathode potential decreases to -1.6 V, the bulk bubble gradually changes from the original periodic growth detachment to non-periodic.

[0087] In some embodiments, the experimental system for analyzing the dynamics of a single bulk bubble provided in the embodiments of the present application can be used to implement a method for analyzing and measuring the dissolution dynamics of a single bulk bubble during electrocatalytic hydrogen evolution. The specific steps include:

[0088] First, Pt nanoparticles were loaded onto the gold film.

[0089] Then, an electrochemical reaction cell was built, the PDMS cell was adhered to the gold film, 0.05 MH2SO4 was added as the electrolyte solution, the parameters of the galvanometer module 2 (i.e., the rotation angles of the x-axis scanning galvanometer and the y-axis scanning galvanometer) were set, and focusing was completed.

[0090] Next, the cathode (working electrode WE) potential is set to -0.8 V (relative to Ag / AgCl reference, vs. Ag / AgCl) through a potential control device (e.g., an electrochemical workstation). After running for a period of time, when the bulk bubble grows to a preset size, the electrochemical path is disconnected (i.e., the output potential is stopped), and the target bulk bubble image is collected until the bulk bubble is completely dissolved and the collection is stopped.

[0091] As no new hydrogen molecules are generated, hydrogen gradually escapes from the solution, the hydrogen supersaturation in the electrolyte solution decreases, and the bubbles previously present in the bulk phase gradually dissolve. The constant changes in the bubble radius and height cause the ring size and central brightness of the interference pattern to change.

[0092] For example, Figure 11 This is a schematic diagram of the results of analyzing and measuring the dissolution kinetics of a single bulk bubble provided in the examples of this application. Specifically, Figure 11 (a) is a graph showing the change of bubble radius over time for the dissolution of a single bulk bubble. Figure 11 As shown in (a), using the Newton ring model, the bubble radius is obtained as a function of time during the dissolution of bulk bubbles. Figure 11 (b) is the kinetic fitting result of the dissolution process of a single bulk bubble, as shown in Figure 11 As shown in (b), the kinetics of the dissolution process were fitted, and it was found that the bulk gas was still controlled by diffusion. Figure 11 (c) is the motion trajectory of the bubble center during the dissolution of a single bulk bubble, as shown in Figure 11As shown in (c), the center of the bulk bubble also undergoes lateral oscillation during the dissolution process. This is because the local dissolution difference on the surface of the bulk bubble leads to uneven distribution of surface tension of the bulk bubble, causing the bulk bubble to move or rotate under the driving force of the Marangoni force.

[0093] An embodiment of the present invention further provides an electronic device, which may include: a display screen, a memory, and one or more processors. The display screen, memory, and processor are coupled. The memory is configured to store computer program code, which includes computer instructions. When the processor executes the computer instructions, the electronic device can perform the various methods or steps described in the aforementioned embodiment of the experimental method for analyzing the dynamics of a single bulk bubble. Of course, the electronic device includes, but is not limited to, the aforementioned display screen, memory, and one or more processors.

[0094] An embodiment of the present invention further provides a computer-readable storage medium for storing computer instructions for executing the above-mentioned experimental method for analyzing the dynamics of a single bulk bubble.

[0095] Through the description of the above implementation methods, technical personnel in the relevant field can clearly understand that for the convenience and simplicity of description, only the division of the above-mentioned functional modules is used as an example. In actual applications, the above-mentioned functions can be assigned to different functional modules as needed, that is, the internal structure of the device can be divided into different functional modules to complete all or part of the functions described above.

[0096] In the description of the present invention, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of the technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include at least one of such features. In the description of the present invention, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0097] In the description of this specification, the reference terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" mean that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification and features of different embodiments or examples without contradiction.

[0098] Similar parts between the embodiments provided in this application can be referenced to each other. The specific implementation methods provided above are only a few examples under the overall concept of this application and do not constitute a limitation on the scope of protection of this application. For those skilled in the art, any other implementation methods expanded based on the scheme of this application without expending creative work shall fall within the scope of protection of this application.

Claims

1. An experimental system for analyzing the dynamics of a single bulk bubble, characterized in that: include: A light source module (1), a galvanometer module (2), a beam expansion module (3), a light splitting module (4), an objective lens (5), a reaction module (6), an imaging module (7) and a camera (8), wherein the reaction module (6) comprises an imaging substrate (61); wherein, The light source module (1) is used to emit a first laser of a preset wavelength to the galvanometer module (2); The galvanometer module (2) is used to adjust the incident angle and azimuth of the first laser according to a preset modulation frequency, and to emit the second laser corresponding to the adjusted first incident angle and first azimuth into the beam expansion module (3), wherein the range of the first azimuth is 0°-360°; The beam expansion module (3) is used to expand the second laser beam and inject the expanded third laser beam into the light splitting module (4); The light splitting module (4) is used to reflect the third laser light to the objective lens (5), so that the third laser light irradiates the imaging substrate (61) and the target bulk phase bubble at the first incident angle and the first azimuth angle through the objective lens (5); The reaction module (6) is used to conduct an experiment to generate the target bulk bubbles; The light splitting module (4) is further used to transmit the first reflected light of the imaging substrate (61) and the first scattered light of the target body phase bubble to the imaging module (7); The imaging module (7) is used to transmit the first reflected light and the first scattered light to the camera (8); The camera (8) is used to generate a target volume bubble image based on the first reflected light and the first scattered light corresponding to different first azimuth angles within a range of 0°-360° at a preset sampling frequency, so as to perform volume bubble dynamics analysis; wherein the preset modulation frequency is an integer multiple of the preset sampling frequency.

2. The system according to claim 1, wherein: The light source module (1) comprises: a laser (11) and a first lens (12): The laser (11) is used to emit the first laser according to the preset wavelength; The first lens (12) is used for collimating the first laser.

3. The system according to claim 1, wherein: The galvanometer module (2) comprises: an x-axis scanning galvanometer (21) and a y-axis scanning galvanometer (22); The x-axis scanning galvanometer (21) and the y-axis scanning galvanometer (22) are used to rotate according to the preset modulation frequency to adjust the incident angle and azimuth angle of the first laser to obtain the second laser.

4. The system according to any one of claims 1 to 3, characterized in that: The beam expansion module (3) comprises: a second lens (31), a third lens (32) and a fourth lens (33) arranged in sequence on the same optical axis; the second lens (31), the third lens (32) and the fourth lens (33) are all plano-convex lenses; the convex surface of the second lens (31) is arranged toward the incident direction of the second laser, the convex surface of the third lens (32) is arranged in the opposite direction to the convex surface of the second lens (31), and the convex surface of the fourth lens (33) is arranged opposite to the convex surface of the third lens (32); The second lens (31) and the third lens (32) are used to expand the second laser beam, and the fourth lens (33) is used to converge the diffused second laser beam to emit the third laser beam.

5. The system according to claim 1, wherein: The objective lens (5) is an oil-immersion objective lens, and the numerical aperture of the objective lens (5) is greater than or equal to 0.

9.

6. The system according to claim 1, wherein: The reaction module (6) further comprises: a reaction pool (62), an electrode device (63) and a potential control device (64); the reaction pool (62) is arranged on the imaging substrate (61), the electrode device (63) is arranged on the imaging substrate (61) and inside the reaction pool (62), and the potential control device (64) is connected to the electrode device (63); The reaction pool (62) is used to load the experimental medium for generating the target bulk bubbles; The potential control device (64) is used to control the electrode device (63) to output a preset potential.

7. The system according to claim 1, wherein: The imaging module (7) comprises: a reflector (71) and a fifth lens (72); wherein, The reflector (71) is used to reflect the first reflected light and the first scattered light to the fifth lens (72); The fifth lens (72) is used to converge the first reflected light and the first scattered light to the camera (8).

8. The system according to claim 7, characterized in that The imaging module (7) further comprises: a sixth lens (73), a seventh lens (74) and an aperture (75); the sixth lens (73) and the seventh lens (74) are arranged between the reflector (71) and the fifth lens (72), the sixth lens (73) and the seventh lens (74) constitute a 4f optical path system, and the aperture (75) is arranged between the sixth lens (73) and the seventh lens (74); wherein, The sixth lens (73) and the seventh lens (74) are used to transmit the first reflected light and the first scattered light; The aperture (75) is used to filter the first reflected light and the first scattered light.

9. The system according to claim 1, wherein: The imaging substrate (61) is one of the following: a glass sheet, a gold-plated glass sheet, indium tin oxide, or a metal film.

10. An experimental method for analyzing the dynamics of a single bulk bubble, characterized in that: The method comprises: Building an experimental system according to any one of claims 1 to 9; Conducting an experiment through the reaction module to generate target bulk bubbles; Moving the reaction module to determine a sampling area of ​​the objective lens, wherein the sampling area includes the target bulk bubble; The light source module emits a first laser with a preset wavelength to the galvanometer module; Adjusting the incident angle and azimuth of the first laser by the galvanometer module according to a preset modulation frequency, and injecting the second laser corresponding to the adjusted first incident angle and first azimuth into the beam expansion module, wherein the first azimuth angle ranges from 0° to 360°; Expanding the second laser beam by the beam expansion module and injecting the expanded third laser beam into the light splitting module; Reflecting the third laser to the objective lens through the light splitting module, so that the third laser irradiates the imaging substrate and the target bulk bubble at the first incident angle and the first azimuth angle through the objective lens; Transmitting the first reflected light of the imaging substrate and the first scattered light of the target bulk bubble to the imaging module through the light splitting module; transmitting the first reflected light and the first scattered light to the camera through an imaging module; The camera generates a target volume bubble image at a preset sampling frequency based on the first reflected light and the first scattered light corresponding to different first azimuth angles within 0°-360° for volume bubble dynamics analysis; wherein the preset modulation frequency is an integer multiple of the preset sampling frequency.

Images