Electrochemical Raman microscope and control method

Abstract

The invention relates to the technical field of analytical chemical instruments and equipment, in particular to an electrochemical Raman microscope. The electrochemical Raman microscope comprises a light path assembly, a microscopic assembly, a laser assembly, a main control board assembly, a Raman spectrometer assembly and an electrochemical analysis assembly, a microreactor for accommodating a sample to be detected is arranged below the microscopic assembly, and the microreactor is used for collecting image information of the sample to be detected; the laser assembly irradiates a to-be-tested sample with laser through the light path assembly; the Raman spectrometer assembly collects a Raman signal of the sample to be detected through the light path assembly; the electrochemical analysis assembly is electrically connected with the microreactor and is used for acquiring an electrochemical signal of the sample to be detected; and the main control board assembly is electrically connected with each assembly so as to control the acquisition of the electrochemical signal and the Raman signal at the same moment. According to the electrochemical Raman microscope provided by the invention, the Raman spectrometer, the electrochemical workstation and the microscopic light path are highly integrated, the synchronous time delay is effectively eliminated, and the real-time performance is improved, so that higher experimental requirements are met.

Description

Technical Field

[0001] The invention relates to the technical field of analytical chemical instruments and equipment, and in particular to an electrochemical Raman microscope and a control method thereof. Background Art

[0002] In the field of analytical chemistry, Raman spectroscopy is widely used in material characterization and chemical analysis because of its non-destructive, rapid, and ability to provide molecular vibration information. Micro-Raman spectroscopy combines traditional optical microscopes and Raman spectrometers, combining spectral information with spatial information to achieve in-situ analysis of samples. Electrochemical analysis, as another analytical technique, is recognized in micro and trace analysis for its rapid, sensitive and accurate characteristics, and is widely used in materials, energy, environment and other fields.

[0003] However, the traditional Raman scattering process has low efficiency, resulting in insufficient detection sensitivity, which limits the application of Raman spectroscopy in the field of analytical characterization. By organically combining electrochemical analysis with micro-Raman spectroscopy, the Raman signal can be greatly enhanced by utilizing the electric field and chemical enhancement effects, significantly improving the detection sensitivity of Raman spectroscopy. Micro-Raman spectroscopy can provide in-situ information on molecular structure and material composition, while electrochemical analysis provides information on the electrochemical properties and reaction kinetics of materials. This combination helps to gain a deeper understanding of the changes in material structure at specific locations on the interface during the electrochemical process, forming electrochemical micro-Raman spectroscopy.

[0004] At present, when conducting electrochemical micro-Raman experiments, independent electrochemical workstations and micro-Raman spectrometers are usually used. Through their own independent software and hardware systems, experimental parameters are set to control the instrument actions. In electrochemical micro-Raman experiments, the method of using a trigger device to connect the micro-Raman spectrometer and the electrochemical workstation has problems of unstable synchronization and complex operation. The main reason is that each independent instrument can only be controlled by its own control system, and synchronous work requires effective and low-latency triggering. Different control systems are difficult to be compatible and can only be triggered by external hardware after being connected by cables. This working method makes the synchronization between different instruments unstable and complicated to operate, especially in some specific electrochemical experimental modes that require high response speed. Therefore, it is difficult for a system using a combination of independent instruments to meet the requirements of modern more precise experiments. Summary of the invention

[0005] In view of the shortcomings of the above-mentioned prior art, the present invention aims to provide a novel electrochemical Raman microscope and control method, which highly integrates the Raman spectrometer, electrochemical workstation and microscope optical path, thereby eliminating synchronization delay and improving real-time performance to meet higher experimental requirements; the chemical Raman microscope provided by the present invention has the advantages of high stability, simple operation and low cost, and can meet the growing needs of scientific research and industrial fields.

[0006] An electrochemical Raman microscope provided by the present invention comprises at least a frame and an optical path component, a microscope component, a laser component, a main control board component, a Raman spectrometer component and an electrochemical analysis component located on the frame, wherein a microreactor for accommodating a sample to be tested is provided below the microscope component; The microscope component is used to observe and collect image information of the sample to be tested; the laser output by the laser component is irradiated by the laser through the optical path component to the sample to be tested; the Raman spectrometer component collects the Raman signal generated by the sample to be tested after laser excitation through the optical path component; the electrochemical analysis component is connected to the microreactor and is used to collect the electrochemical signal from the sample to be tested in the microreactor; the main control board component is electrically connected to the laser component, the Raman spectrometer component, the electrochemical analysis component, and the optical path component respectively to synchronously control the laser component, the Raman spectrometer component, the electrochemical analysis component, and the optical path component to operate in a unified manner, so that the acquired electrochemical signal corresponds to the collected Raman signal one by one.

[0007] In one embodiment, the optical path component includes a white light optical path component, a laser optical path component, a Raman optical path component and an optical path adjustment component; The white light optical path component includes an illumination optical path component and an imaging optical path component, wherein the illumination optical path component is used to output white light to the microscope component so that the sample to be tested receives the irradiation of the white light, and the imaging optical path component is used to receive the white light image information output by the microscope component through the diffuse reflection of the sample to be tested; The laser optical path component is used to output the laser light emitted by the laser component to the microscope component so that the sample to be tested receives the irradiation of the laser light; The Raman optical path component is used to receive the Raman signal generated by the laser excitation of the sample to be tested by the laser optical path component and transmit the Raman signal to the Raman spectrometer component; The optical path adjustment component is used to switch the Raman optical path between the Raman optical path component and the laser optical path component to the microreactor or to switch the white light optical path between the white light optical path component and the microreactor.

[0008] In one embodiment, the illumination optical path component includes a white light source, a white light collimating lens group, and a white light focusing lens group; the white light emitted by the white light source is sequentially transmitted through the white light collimating lens group, the white light focusing lens group, and the optical path adjustment component to the microscope component; the imaging optical path component includes an imaging lens group and an image acquisition component, and the microscope component receives the diffusely reflected light emitted by the sample to be tested, and sequentially passes through the optical path adjustment component and the imaging lens group to converge on the image acquisition component.

[0009] In one embodiment, the laser optical path component includes a beam expander, a first reflector group, and a dichroic mirror. The laser emitted by the laser component passes through the beam expander, the first reflector group, and the dichroic mirror in sequence and is then transmitted to the microscope component.

[0010] In one embodiment, the Raman optical path component includes a dichroic mirror, a second reflector group, and a signal light collecting mirror group. The microscope component receives the Raman signal generated by the sample to be tested after laser excitation, and transmits the Raman signal to the Raman spectrometer component through the dichroic mirror, the second reflector group and the signal light collecting mirror group in sequence.

[0011] In one embodiment, the electrochemical Raman microscope further includes an external interface component, and the external interface component includes a power interface, a switch, and a data transmission interface.

[0012] In one embodiment, the electrochemical Raman microscope further comprises a degree of freedom component, wherein the degree of freedom component comprises a linear motion module, and the linear motion module drives the microreactor to adjust the spatial orientation.

[0013] In one embodiment, the microreactor is an electrochemical reaction cell.

[0014] In one embodiment, the optical path adjustment component includes a beam splitter and a moving component, wherein the moving component is connected to the beam splitter to provide position control for the beam splitter.

[0015] The present invention also provides an electrochemical Raman microscope control method, using the electrochemical Raman microscope as described in the above embodiment, and further comprising the following steps: The sample to be tested is placed in a microreactor; Observe the sample to be tested in the microreactor through the microscope component and collect image information; The main control board component simultaneously sends synchronization signals to the Raman spectrometer component and the electrochemical analysis component; The Raman spectrometer component and the electrochemical analysis component respectively collect the Raman signal and the electrochemical signal of the sample to be tested in the microreactor at the same time according to the synchronization signal, and feed the Raman signal and the electrochemical signal back to the main control board component; After acquiring the Raman signal and the electrochemical signal, the main control board component continues to send a synchronization signal, and this cycle continues until the acquisition is completed.

[0016] Based on the above, compared with the prior art, the electrochemical Raman microscope provided by the present invention highly integrates the Raman spectrometer component, the electrochemical analysis component and the microscope optical path, effectively improving the stability and real-time performance of the test and simplifying the operation.

[0017] Other features and beneficial effects of the present invention will be described in the following description, and partly become apparent from the description, or understood by practicing the present invention. The purpose and other beneficial effects of the present invention can be realized and obtained by the structures particularly pointed out in the description, claims and drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. The positional relationships shown in the drawings in the following description are based on the directions in which the components are drawn in the diagrams, unless otherwise specified.

[0019] Figure 1 A schematic diagram of the exploded structure of an electrochemical Raman microscope provided by an embodiment of the present invention; Figure 2 A schematic diagram of the structure of an illumination optical path component of an electrochemical Raman microscope provided in an embodiment of the present invention; Figure 3 A schematic diagram of the structure of an imaging optical path component of an electrochemical Raman microscope provided in an embodiment of the present invention; Figure 4 A schematic diagram of the structure of the laser optical path component of the electrochemical Raman microscope provided by an embodiment of the present invention; Figure 5 A schematic diagram of the structure of the Raman optical path components of the electrochemical Raman microscope provided in an embodiment of the present invention; Figure 6a , Figure 6b A schematic diagram of the optical path of an electrochemical Raman microscope provided in an embodiment of the present invention; Figure 7 A schematic diagram of the circuit connection between the electrochemical analysis component and the microreactor provided in an embodiment of the present invention; Figure 8 A schematic diagram of a control flow of an electrochemical Raman microscope control method provided in an embodiment of the present invention.

[0020] Reference numerals: 10. Optical path component; 11. White light optical path component; 111. Illumination optical path component; 1111. White light source; 1112. White light collimating lens group; 1113. White light focusing lens group; 112. Imaging optical path component; 1121. Imaging lens group; 1122. Image acquisition lens group; 12. Laser optical path component; 121. Beam expander; 122. First reflector group; 123. Dichroic mirror; 13. Raman optical path component; 131. Dichroic mirror; 132. Second reflector group; 133. Signal light collection lens group; 14. Optical path adjustment component; 141. Beam splitter; 142. Moving component; 20. Microscope component; 30. Laser component; 40. Raman spectrometer component; 50. Electrochemical analysis component; 60. Microreactor; 70. External interface component; 80. Degree of freedom component; 90. Main control board component; 100. Rack. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all the embodiments; the technical features designed in different implementation modes of the present invention described below can be combined with each other as long as they do not conflict with each other; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0022] In the description of the present invention, it should be noted that all terms used in the present invention have the same meanings as those generally understood by ordinary technicians in the field to which the present invention belongs, and should not be understood as limitations on the present invention; it should be further understood that the terms used in the present invention should be understood to have the same meanings as these terms in the context of this specification and in the relevant field, and should not be understood in an idealized or overly formal sense, unless explicitly defined in this invention.

[0023] The present invention provides an electrochemical Raman microscope. Figures 1 to 7 The electrochemical Raman microscope comprises an optical path component 10, a microscope component 20, a laser component 30, a Raman spectrometer component 40 and an electrochemical analysis component 50. A microreactor 60 for accommodating a sample to be tested is disposed below the microscope component 20.

[0024] Specifically, the microscope assembly 20 is used to observe and collect image information of the sample to be tested; the laser output by the laser assembly 30 is irradiated by the laser via the optical path assembly 10; the Raman spectrometer assembly 40 collects the Raman signal generated by the laser excitation of the sample to be tested via the optical path assembly 10; the electrochemical analysis assembly 50 is connected to the microreactor 60, and is used to collect the electrochemical signal from the sample to be tested in the microreactor 60; The main control board assembly 90 is electrically connected to the laser assembly 30, the Raman spectrometer assembly 40, the electrochemical analysis assembly 50, and the optical path assembly 10, respectively, so as to control the laser assembly 30, the Raman spectrometer assembly 40, the electrochemical analysis assembly 50, and the optical path assembly 10 to act in a unified manner, thereby synchronously acquiring the electrochemical signal and the Raman signal at the same time.

[0025] The optical path component 10 includes a white light optical path component 11 , a laser optical path component 12 and a Raman optical path component 13 ; the white light optical path component 11 includes an illumination optical path component 111 and an imaging optical path component 112 .

[0026] The illumination optical path component 111 is used to output white light to the microscope component 20 so that the sample to be tested receives the irradiation of white light. In a specific embodiment, the illumination optical path component 111 includes a white light source 1111, a white light collimating lens group 1112, a white light focusing lens group 1113, and an optical path adjustment component 14.

[0027] For easier understanding, please also refer to Figure 2 , Figure 6a , Figure 7 The white light emitted by the white light source 1111 is sequentially transmitted to the microscope component 20 through the white light collimating lens group 1112, the white light focusing lens group 1113, and the optical path adjustment component 14. Figure 6a A in the figure is a schematic diagram of the illumination light path.

[0028] Specifically, the white light source 1111 emits a composite light composed of a mixture of multiple colored lights. This light is emitted when a thermoluminescent body is heated to a high temperature, or is generated through artificial synthesis technology. For example, the white light source 1111 can be an LED light source, a halogen lamp, a xenon lamp, etc.; after the white light is emitted from the light source, it enters the white light collimator group 1112, and the white light collimator group 1112 is used to adjust the direction of the light so that the white light becomes parallel light, ensuring that the subsequent optical elements can receive light with consistent directions and parallel light, which helps to improve the imaging quality and accuracy; the white light passing through the white light collimator group 1112 enters the white light focusing lens group 1113, and the white light focusing lens group 1113 is used to focus the parallel light to a small focus, or to form a clear light spot in a certain area, so as to ensure that the energy of the white light can be concentrated on the sample to be observed, so as to improve the utilization of light energy. In order to improve the clarity of the image and the resolution of the image, in some preferred embodiments, the white light focusing lens group 1113 may also include a variable focal length lens to achieve observations at different magnifications; the focused white light is divided into multiple beams of light by the optical path adjustment component 14, so that these beams of light can continue to propagate in a predetermined direction or angle. For example, in an embodiment of the present invention, the function of the optical path adjustment component 14 is to distribute the white light to different optical paths, for example, one path may be used to form a reference light, and the other path is guided to the microscope component 20 to irradiate the sample surface to form a measurement light; the multiple beams of light processed by the optical path adjustment component 14 are continuously transmitted to the microscope component 20; the white light passing through the optical path adjustment component 14 finally reaches the microscope component 20, specifically the objective lens part of one of the components of the microscope component 20, which is used to collect diffuse reflected light from the sample to be measured, and amplify and image it onto subsequent optical elements.

[0029] The imaging optical path component 112 is used to receive the white light image information of the diffuse reflection of the sample to be tested outputted by the microscope component 20. In a specific embodiment, the imaging optical path component 112 includes an optical path adjustment component 14, an imaging lens group 1121 and an image acquisition component 1122; For easier understanding, please also refer to Figure 3 , Figure 6a , Figure 7 The microscope component 20 receives the diffuse reflected light emitted by the sample to be tested, and the diffuse reflected light passes through the optical path adjustment component 14 and the imaging lens group 1121 in sequence and converges to the image acquisition component 1122. Figure 6a B in the figure is a schematic diagram of the imaging light path.

[0030] Specifically, when the white light beam is irradiated onto the sample to be tested, the morphology, color, texture and other information on the sample surface will be emitted as diffuse reflection light, which is collected by the objective lens of the microscope component 20 and under the action of the objective lens, the tiny details on the sample surface are magnified and projected onto the subsequent imaging light path; the imaging light passes through the optical path adjustment component 14 again and continues to propagate to the imaging lens group 1121, while blocking the interference of the illumination light, so that the imaging light path and the illumination light path are completely separated. After the imaging light enters the imaging lens group 1121, it is further magnified and focused by a series of lenses, and finally converges on the photosensitive surface of the image acquisition component 1122. The setting of the imaging lens group 1122 is conducive to improving the resolution, contrast and signal-to-noise ratio of the image, thereby ensuring that the imaging light can be received and processed by the image acquisition component 1122 in the best way; the imaging light converged by the imaging lens group 1121 finally reaches the image acquisition component 1122; the image acquisition component 1122 can convert the optical image into an electrical signal or a digital signal, which can then be transmitted to a computer or other processing device for further analysis and processing.

[0031] The laser optical path component 12 is used to output the laser light emitted by the laser component 30 to the microscope component 20 so that the sample to be tested can be irradiated by the laser light.

[0032] In a specific embodiment, the laser optical path component 12 includes a beam expander 121, a first reflector group 122, and a dichroic mirror 123. For ease of understanding, please also refer to Figure 4 , Figure 6b , Figure 7 The laser light emitted by the laser assembly 30 is transmitted to the microscope assembly 20 after passing through the beam expander 121, the first reflector group 122, and the dichroic mirror 123 in sequence. Figure 6b C in the figure is a schematic diagram of the laser light path.

[0033] Specifically, the laser assembly 30 is activated to emit a laser beam of a specific wavelength, which is usually highly monochromatic, highly coherent and highly bright, and is suitable for precisely controlled optical experiments and measurements; in a preferred embodiment, after the laser beam is emitted from the laser assembly 30, it may first pass through an attenuator, which is used to adjust the intensity of the laser to ensure that the laser will not be too strong when irradiating the sample to be tested and damage the sample or cause other adverse effects. By adjusting the parameters of the attenuator, the power output of the laser can be precisely controlled. The laser beam adjusted by the attenuator then enters the beam expander 121, which is used to expand the diameter of the laser beam, thereby reducing the divergence angle of the laser beam, improving the uniformity and stability of the laser irradiation on the sample, and facilitating the acquisition of a more reliable Raman signal. The expanded laser beam is guided by a first reflector group 122, which may be composed of one or more reflectors, which are arranged at a specific angle and position to ensure that the laser beam can be transmitted to the sample to be tested along a predetermined path. The first reflector group 122 also allows the direction of the laser beam to be fine-tuned to meet different experimental requirements. Before the laser beam reaches the microscope assembly 20, it passes through one or more dichroic mirrors 123, which are used to further purify the laser beam, highly reflect light of a specific wavelength, and highly transmit light of other wavelengths, so as to improve the purity and stability of the laser beam. At the same time, the dichroic mirror 123 can also prevent the laser beam from damaging the microscope assembly 20. Finally, the laser beam that has undergone multiple treatments is focused onto the sample to be tested through the objective lens of the microscope assembly 20, which is responsible for not only focusing the laser beam, but also ensuring that the laser beam can accurately irradiate a specific area of ​​the sample.

[0034] The Raman optical path component 13 is used to receive the Raman signal generated by the laser excitation of the sample to be tested by the laser optical path component 12 and transmit the Raman signal to the Raman spectrometer component 40 .

[0035] In a specific embodiment, the Raman optical path component 13 includes a dichroic mirror 131, a second reflector group 132, and a signal light collecting mirror group 133; for ease of understanding, please also refer to Figure 5 , Figure 6b , Figure 7 The microscope assembly 20 receives the Raman signal generated by the sample to be tested after laser excitation, and transmits the Raman signal to the Raman spectrometer assembly 40 through the dichroic mirror 131, the second reflector group 132 and the signal light collecting mirror group 133 in sequence. Figure 6b D in the figure is a schematic diagram of the Raman optical path.

[0036] Specifically, when the laser beam is irradiated onto the sample to be tested, the sample molecules absorb the laser energy and undergo a transition of vibration or rotation energy levels. Subsequently, the sample molecules emit scattered light, including sharp scattered light with the same frequency as the incident light and Raman scattered light with a changed frequency; since the frequency change of the Raman signal is related to the vibration or rotation energy level of the sample molecules, it can be used to analyze the chemical composition and structure of the sample. The objective lens of the microscope component 20 is not only used to focus the laser beam, but also responsible for collecting the Raman signals from the sample and focusing and transmitting these Raman signals to subsequent optical elements; before the Raman signal enters the second reflector group 132 and the signal light collection mirror group 133, it first passes through one or more dichroic mirrors 131, which are used to remove sharp scattered light and other unnecessary background light signals to ensure that only the Raman signal is transmitted to the Raman spectrometer component 40. The Raman signal processed by the dichroic mirror 131 then enters the second reflector group 132, which can be composed of one or more reflectors arranged at specific angles and positions to ensure that the Raman signal can be transmitted to the signal light collection mirror group 133 along a predetermined path. The second reflector group 132 also allows the transmission direction of the Raman signal to be fine-tuned to ensure that the signal can be efficiently transmitted to the signal light collection mirror group 133; the signal light collection mirror group 133 can be composed of one or more lenses or reflectors, which are responsible for focusing and collecting the Raman signal and transmitting it to the detector of the Raman spectrometer assembly 40. The detector located on the Raman spectrometer assembly 40 can convert the Raman signal into an electrical signal or a digital signal, and transmit it to a computer or other processing device for further analysis and processing. The Raman spectrometer assembly 40 is capable of measuring the frequency and intensity distribution of the Raman signal, thereby providing important information about the chemical composition and structure of the sample.

[0037] It should be noted that the dichroic mirror 123 and the dichroic mirror 131 may be the same dichroic mirror, so as to further improve the integration of the electrochemical Raman microscope of the present invention and make full use of the internal space of the instrument.

[0038] In addition, the electrochemical Raman microscope provided in the preferred embodiment of the present invention includes a frame 100 to support the fixing of the above components to each other through fasteners such as screws and integration in a smaller space, thereby reducing the loss in the intermediate signal transmission process to achieve better measurement accuracy.

[0039] It should also be noted that in the embodiment of the present invention, the sample to be tested is contained in a microreactor 60 below the microscopic component 20, and the microreactor 60 is connected to the electrochemical analysis component 50. Figure 7As shown, it is a schematic diagram of the connection between the electrochemical analysis component 50 and the microreactor 60. The three output ports of the electrochemical analysis component 60 are connected to the wiring terminals of the microreactor 60 through wires a, b, and c, so as to realize precise control of the chemical reaction process in the microreactor 60 and signal collection.

[0040] In a preferred embodiment, the optical path adjustment component 14 includes a beam splitter 141 and a moving component 142, wherein the moving component 142 is connected to the beam splitter 141 to provide position control for the beam splitter 141. Figure 6a and Figure 6b According to the optical path requirements, the position of the beam splitter 141 is moved to meet the operation needs of the instrument and further improve the integration of the instrument.

[0041] In a preferred embodiment, the microreactor 60 is an electrochemical reaction cell. Therefore, the electrochemical Raman microscope provided by the present invention can realize that the optical system works synchronously during electrochemical analysis to provide real-time images and Raman spectrum information of the sample. This information is combined with the electrochemical data collected by the electrochemical analysis component 50 to fully reveal the changes in the morphology, structure and chemical composition of the sample during the electrochemical reaction.

[0042] For example, by comparing the visible light images and Raman spectra of samples at different potentials, the morphological changes and chemical structure changes of the samples during electrochemical oxidation or reduction can be observed. At the same time, combined with the data from the electrochemical workstation, the relationship between these changes and electrochemical parameters can be further analyzed.

[0043] The present invention combines the optical system with the electrochemical analysis component to achieve a comprehensive analysis of the sample to be tested in the electrochemical reaction cell. This combination not only provides information on the morphology, structure and chemical composition of the sample, but also reveals the dynamic changes of the sample during the electrochemical reaction process, providing strong support for a deep understanding of the electrochemical reaction mechanism.

[0044] In some embodiments, the electrochemical Raman microscope also includes an external interface component 70, which includes a power interface, a switch, and a data transmission interface. The power interface is used to provide a stable power supply for the electrochemical Raman microscope, the switch is used to control the opening and closing of the electrochemical Raman microscope, and the data transmission interface includes but is not limited to a USB interface, etc., so that the electrochemical Raman microscope can be connected to a computer and various internal components can be controlled simultaneously through a client program to ensure good synchronization and stability.

[0045] In some embodiments, the electrochemical reaction cell may be located on the stage of the microscope assembly 20, and a transparent window is provided on the top of the electrochemical reaction cell. Preferably, the electrochemical Raman microscope further comprises a degree of freedom assembly 80, wherein the degree of freedom assembly 80 comprises a linear motion module, wherein the linear motion module drives the microreactor 60 to adjust the spatial orientation, and is used to observe the microscopic image of the sample surface when adjusting the microreactor 60. Preferably, the degree of freedom assembly 80 may output at least one linear degree of freedom obtained by the linear motion module and a rotational degree of freedom obtained by the rotational module, wherein the linear motion module may be used to adjust the height of the rotational degree of freedom, and the rotational module may be used to adjust the spatial angle of the microreactor 60, thereby achieving a wider range of spatial position adjustment.

[0046] In some embodiments, the electrochemical Raman microscope also includes a main control board assembly 90, and the main control board assembly 90 is respectively connected to the optical path assembly 10, the Raman spectrometer assembly 40 and the electrochemical analysis assembly 50. Through unified control by the main control board assembly 90, the working electrode parameter conditions and the Raman spectrometer action and sampling instructions can be generated simultaneously. Compared with the current system of independent instrument combination, the synchronization delay is eliminated, and it has the advantages of good stability, simple operation and low cost, which can better meet the growing needs of scientific research and industrial fields.

[0047] The present invention further provides an electrochemical Raman microscope control method. The electrochemical Raman microscope control method adopts the electrochemical Raman microscope described in the above embodiments. Its specific structural design, functions and effects can be referred to above and will not be described in detail here.

[0048] The electrochemical Raman microscope control method comprises the following steps: The sample to be tested is placed in the microreactor 60; the sample to be tested in the microreactor 60 is observed and image information is collected through the microscope component 20; the main control board component 90 simultaneously sends a synchronization signal to the Raman spectrometer component 40 and the electrochemical analysis component 50; the Raman spectrometer component 40 and the electrochemical analysis component 50 respectively collect the Raman signal and the electrochemical signal of the sample to be tested in the microreactor 60 at the same time according to the synchronization signal, and feed the Raman signal and the electrochemical signal back to the main control board component 90; after obtaining the Raman signal and the electrochemical signal, the main control board component 90 continues to send the synchronization signal, and the cycle is repeated until the collection is completed.

[0049] For specific implementation, please refer to Figure 8The electrochemical Raman microscope can be connected to the host computer by wired or wireless communication to achieve data interaction, so that the electrochemical Raman microscope can work as a separate Raman spectrometer or electrochemical device to obtain Raman signals or electrochemical signals separately, and can also work as a whole to synchronously obtain Raman signals and electrochemical signals at the same time. For example, the electrochemical Raman microscope is connected to the host computer via a USB interface. The specific control can be set using the corresponding software program.

[0050] As an example, the host computer first sends the configuration information of the target experiment to the main control board component 90, the Raman spectrometer component 40, and the electrochemical analysis component 50 respectively, and then sends a start command to the main control board component 90. The main control board component 90 simultaneously sends a synchronization signal to the Raman spectrometer component 40 and the electrochemical analysis component 50 according to the configuration information, so that the Raman spectrometer component 40 and the electrochemical analysis component 50 start working according to the configuration information, collect the Raman signal and the electrochemical signal of the sample to be tested in the microreactor 60 at the same time, and after completion, each feeds back the Raman signal and the electrochemical signal to the main control board component 90. After obtaining the feedback of the Raman signal and the electrochemical signal, the main control board component 90 continues to send the synchronization signal, and repeats this cycle until the collection is completed.

[0051] The above-mentioned synchronous control method can realize completely synchronous acquisition of Raman signals and electrochemical signals, effectively eliminating the communication delay existing in the control of the host computer under the general method, effectively reducing the error caused by signal asynchrony, improving the credibility of the data, and realizing high-precision analysis.

[0052] In addition, those skilled in the art should understand that, although there are many problems in the prior art, each embodiment or technical solution of the present invention can be improved in only one or several aspects, without having to solve all the technical problems listed in the prior art or background technology at the same time. Those skilled in the art should understand that the content not mentioned in a claim should not be used as a limitation on the claim.

[0053] Although the terms such as optical path component, white light optical path component, illumination optical path component, white light source, white light collimating lens group, white light focusing lens group, imaging optical path component, imaging lens group, image acquisition lens group, laser optical path component, beam expander, first reflector group, dichroic mirror, Raman optical path component, second reflector group, signal light collection lens group, optical path adjustment component, beam splitter, moving component, microscope component, laser component, Raman spectrometer component, electrochemical analysis component, microreactor, external interface component, degree of freedom component, main control board component, degree of freedom, etc. are used more frequently in this article, the possibility of using other terms is not excluded. The use of these terms is only to more conveniently describe and explain the essence of the present invention; interpreting them as any additional limitation is contrary to the spirit of the present invention; the terms "first", "second", etc. in the description and claims of the embodiments of the present invention and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence.

[0054] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An electrochemical Raman microscope, characterized in that: It comprises a frame and an optical path component, a microscope component, a laser component, a main control board component, a Raman spectrometer component and an electrochemical analysis component located on the frame, wherein a microreactor for accommodating a sample to be tested is provided below the microscope component; The microscopic component is used to observe and collect image information of the sample to be tested; The laser output by the laser assembly is irradiated by the laser through the optical path assembly so that the sample to be tested receives the laser light; the Raman spectrometer assembly collects the Raman signal generated by the sample to be tested after laser excitation through the optical path assembly; the electrochemical analysis assembly is connected to the microreactor to collect the electrochemical signal from the sample to be tested in the microreactor; The main control board component is electrically connected to the laser component, Raman spectrometer component, electrochemical analysis component, and optical path component, respectively, to control the laser component, Raman spectrometer component, electrochemical analysis component, and optical path component to act in a unified manner, thereby synchronously acquiring electrochemical signals and Raman signals at the same time.

2. The electrochemical Raman microscope according to claim 1, characterized in that: The optical path components include a white light optical path component, a laser optical path component, a Raman optical path component and an optical path adjustment component; The white light optical path component includes an illumination optical path component and an imaging optical path component, wherein the illumination optical path component is used to output white light to the microscope component so that the sample to be tested receives the irradiation of the white light, and the imaging optical path component is used to receive the white light image information output by the microscope component through the diffuse reflection of the sample to be tested; The laser optical path component is used to output the laser light emitted by the laser component to the microscope component so that the sample to be tested receives the irradiation of the laser light; The Raman optical path component is used to receive the Raman signal generated by the laser excitation of the sample to be tested by the laser optical path component and transmit the Raman signal to the Raman spectrometer component; The optical path adjustment component is used to switch the Raman optical path between the Raman optical path component and the laser optical path component to the microreactor or to switch the white light optical path between the white light optical path component and the microreactor.

3. The electrochemical Raman microscope according to claim 2, characterized in that: The illumination optical path component includes a white light source, a white light collimating lens group, and a white light focusing lens group; the white light emitted by the white light source is sequentially transmitted to the microscope component through the white light collimating lens group, the white light focusing lens group, and the optical path adjustment component; the imaging optical path component includes an imaging lens group and an image acquisition component, and the microscope component receives the diffuse reflected light emitted by the sample to be tested, and sequentially passes through the optical path adjustment component and the imaging lens group to converge on the image acquisition component.

4. The electrochemical Raman microscope according to claim 2, characterized in that: The laser optical path component comprises a beam expander, a first reflector group, and a dichroic mirror. The laser emitted by the laser component passes through the beam expander, the first reflector group, and the dichroic mirror in sequence and is then transmitted to the microscope component.

5. The electrochemical Raman microscope according to claim 2, characterized in that: The Raman optical path component includes a dichroic mirror, a second reflector group, and a signal light collecting mirror group. The microscope component receives the Raman signal generated by the sample to be tested after laser excitation, and transmits the Raman signal to the Raman spectrometer component through the dichroic mirror, the second reflector group and the signal light collecting mirror group in sequence.

6. The electrochemical Raman microscope according to claim 1, characterized in that: The electrochemical Raman microscope also includes an external interface component, which includes a power supply interface, a switch and a data transmission interface.

7. The electrochemical Raman microscope according to claim 1, characterized in that: The electrochemical Raman microscope further comprises a degree of freedom component, wherein the degree of freedom component comprises a linear motion module, and the linear motion module drives the microreactor to adjust the spatial orientation.

8. The electrochemical Raman microscope according to claim 1, characterized in that: The microreactor is an electrochemical reaction cell.

9. The electrochemical Raman microscope according to claim 2, characterized in that: The optical path adjustment component includes a beam splitter and a moving component, wherein the moving component is connected to the beam splitter to provide position control for the beam splitter.

10. A method for controlling an electrochemical Raman microscope, characterized in that: The electrochemical Raman microscope according to any one of claims 1 to 9 further comprises the following steps: The sample to be tested is placed in a microreactor; Observe the sample to be tested in the microreactor through the microscope component and collect image information; The main control board component simultaneously sends synchronization signals to the Raman spectrometer component and the electrochemical analysis component; The Raman spectrometer component and the electrochemical analysis component respectively collect the Raman signal and the electrochemical signal of the sample to be tested in the microreactor at the same time according to the synchronization signal, and feed the Raman signal and the electrochemical signal back to the main control board component; After acquiring the Raman signal and the electrochemical signal, the main control board component continues to send a synchronization signal, and this cycle continues until the acquisition is completed.

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