CN114002483B - A Transient Photovoltage Measurement System in Liquid In Situ Reactions - Google Patents

Abstract

The application provides a transient photovoltage measurement system in a liquid in-situ reaction, including: a test base, a light source module, and an electrode module, wherein: the test base is provided with a light incident module and a sample test module, and the sample test module includes a test platform A bracket, a test platform and a quartz test plate, the electrode module includes a mesh electrode and a probe electrode, and the mesh electrode is arranged in the cavity; during measurement, a first test sample and a second test sample will be formed on the mesh of the mesh electrode during measurement. 2. Test the sample liquid film, so that the laser beam emitted by the light source module is transmitted to the cavity through the light incident module, and the probe electrode is used to contact the liquid film, so that the laser beam stimulates the test sample to have an in-situ reaction, and obtains the transient light Voltage. Due to the use of mesh electrodes, it constitutes a natural electromagnetic shield, which ensures the relative independence and stability of each time the probe electrode is used to contact the liquid film for testing, and realizes the transient photovoltage measurement in the liquid in-situ reaction.

Description

A Transient Photovoltage Measurement System in Liquid In Situ Reactions

technical field

The application relates to the field of photochemistry, and in particular, the application relates to a transient photovoltage measurement system in a liquid in-situ reaction.

Background technique

At present, the measurement of the transient photovoltage is only the measurement of the electronic properties of the material itself. For example, after the surface of the material or device is excited by the external excitation signal, the distribution of the surface charge will change. Measurement can detect the surface properties of materials or devices to test the surface properties of materials. However, the existing transient photovoltage techniques cannot measure the charge transport changes during the in situ reaction either in terms of working principle or time scale; that is, the existing transient photovoltage techniques can only be measured by The method of applying bias voltage modulation or perturbation modulation of the material/substance light source, to study the change of charge in the material itself, is the measurement of the electronic properties of the material itself; it cannot study the in-situ reaction between different materials/substances. The process of charge generation, separation, transport and recombination, especially the charge transport kinetics at the interface of the in situ reaction process of different materials/substances cannot be studied.

Further, in the prior art, it is impossible to measure the transient photovoltage of the in-situ reaction between samples in a liquid state, so it is necessary to provide a solution for the transient photovoltage measurement in the in-situ reaction in a liquid state.

SUMMARY OF THE INVENTION

The purpose of this application is to solve at least one of the above-mentioned technical defects, and the technical solutions provided by the embodiments of this application are as follows:

In a first aspect, an embodiment of the present application provides a transient photovoltage measurement system in a liquid in-situ reaction, including: a test base, a light source module, an electrode module, and a processing module, wherein:

The test base is provided with a light incident module and a sample test module. The sample test module includes a test platform bracket, a test platform with a light-transmitting hole, and a quartz test board with a cavity. The quartz test board is set on the test platform and has a container. The bottom of the cavity faces the light-transmitting hole, the electrode module includes a mesh electrode and a probe electrode, the mesh electrode is arranged in the cavity, and the processing module is electrically connected to the mesh electrode and the probe electrode respectively;

During measurement, a liquid film containing the first test sample and the second test sample is formed on the grid of the mesh electrode, and the probe electrode is in contact with the liquid film, and the laser beam emitted by the light source module is transmitted to the capacitor through the light incident module. a cavity, so that the laser beam excites the first test sample and the second test sample to generate an in-situ reaction, and the processing module obtains the transient light in the in-situ reaction according to the received voltage values of the mesh electrode and the probe electrode Voltage.

In an optional embodiment of the present application, a cover plate is further arranged above the cavity of the quartz test plate, and an opening is arranged on the cover plate. During measurement, the probe electrode is used to pass through the opening and then contact the liquid film.

In an optional embodiment of the present application, during measurement, a liquid film containing the first test sample and the second test sample is formed on the grid of the mesh electrode in the following manner:

A first liquid film containing the first test sample is formed on the grid of the mesh electrode, and then the solution containing the second test sample is sprayed on the first liquid film to obtain the first test sample and the liquid film of the second test sample; or,

A second liquid film containing the second test sample is formed on the grid of the mesh electrode, and the probe electrode is adhered to the first test sample and then contacted with the second liquid film to obtain the first test sample and the second liquid film. liquid film of the test sample;

Wherein, the first test sample is the solid particles in the in-situ reaction, and the second test sample is the gas or liquid in the in-situ reaction.

In an optional embodiment of the present application, the mesh electrode is formed by cross-connecting a plurality of electrode lines laterally and longitudinally, and the electrode lines are made of Ag and AgCl composite materials, and the mesh size of the mesh electrode is the same or according to The specified order decreases sequentially.

In an optional embodiment of the present application, the probe electrode includes a glass protective layer and a micro-electrode, the glass protective layer is wrapped around the micro-electrode, and one end of the probe electrode is a micro-electrode end, which is used for contacting the liquid film. The other end of the electrode is a wire end, which is used for electrical connection with the processing module through the wire, and the diameter of the probe electrode gradually decreases from the wire end to the micro-electrode end.

In an optional embodiment of the present application, the protective glass layer is coated with an electromagnetic shielding material.

In an optional embodiment of the present application, the electrode module further includes a three-dimensional moving platform, and the lead end of the probe electrode is connected to the three-dimensional moving platform. During measurement, the three-dimensional moving platform drives the probe electrode to move, so that the probe The microelectrode end of the electrode is in contact with the liquid membrane.

In an optional embodiment of the present application, the light incident module includes a lens support on which an optical fiber module, a lens module and a reflection module are mounted. During measurement, the laser beam emitted by the light source module is conducted to the lens module through the optical fiber module And emit to the reflection module, and then conduct to the cavity through the reflection module.

In an optional embodiment of the present application, the lens module is rotatably mounted on the lens holder, and the lens module is provided with an angle sensor. During measurement, the lens module is rotated according to the reading of the angle sensor to adjust the laser beam. Optical path, so that the laser beam is conducted to the cavity.

In an optional embodiment of the present application, the system further includes a shielding box, and the test base, the light source module and the electrode module are arranged in the shielding box.

In an optional embodiment of the present application, both the test base and the test platform are coated with electromagnetic shielding material.

The beneficial effects brought by the technical solution provided by the application are:

A mesh electrode and a probe electrode are used, and the probe electrode is perpendicular to the surface where the mesh electrode is located. By forming a stable liquid film containing the first test sample and the second test sample on the mesh of the mesh electrode, the probe The electrode contacts the liquid film, extends into the middle of a grid of the mesh electrode, and has a predetermined interval with the periphery of the mesh electrode of the mesh electrode. Since each mesh of the mesh electrode is a separate environment, it has a closed characteristic. , each grid can meet the requirements of electromagnetic shielding and constitute a natural electromagnetic shielding, which ensures the relative independence and stability of the in-situ reaction measurement when the probe electrode is used to contact the liquid film, and realizes the transient light in the liquid in-situ reaction. The voltage measurement provides a basis for studying the process of charge generation, separation, transport and recombination in the in-situ reaction in the liquid state, as well as the charge transport kinetics at the interface during the in-situ reaction.

Description of drawings

In order to illustrate the technical solutions in the embodiments of the present application more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments of the present application.

1 is a schematic side view of a transient photovoltage measurement system in a liquid in-situ reaction in an example of an embodiment of the present application;

2 is a schematic top view of a transient photovoltage measurement system in a liquid in-situ reaction in an example of an embodiment of the present application;

3 is a schematic structural diagram of a cover plate of a quartz test plate in an example of the embodiment of the present application;

4 is a schematic structural diagram of a mesh electrode in an example of an embodiment of the present application;

5 is a schematic structural diagram of a probe electrode in an example of an embodiment of the present application;

6 is a schematic side view of a transient photovoltage measurement system in a liquid in-situ reaction with a shielding box in an example of an embodiment of the present application;

Reference number:

1-test base; 2-light source module; 3-electrode module; 4-processing module; 5-shielding box;

11-light incident module; 12-sample testing module; 31-mesh electrode; 32-probe electrode;

121-test platform bracket; 122-test platform; 123-quartz test plate; 311-electrode wire;

312-grid; 313-wire; 321-glass protective layer; 322-microelectrode; 323-microelectrode end;

324-lead end; 1221-light-transmitting hole; 1231-cavity; 1232-cover; 1233-opening.

Detailed ways

The following describes in detail the embodiments of the present application, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present application, but not to be construed as a limitation on the present application.

It will be understood by those skilled in the art that the singular forms "a", "an", "the" and "the" as used herein can include the plural forms as well, unless expressly stated otherwise. It should be further understood that the word "comprising" used in the specification of this application refers to the presence of stated features, integers, steps, operations, elements and/or components, but does not preclude the presence or addition of one or more other features, Integers, steps, operations, elements, components and/or groups thereof. It will be understood that when we refer to an element as being "connected" or "coupled" to another element, it can be directly connected or coupled to the other element or intervening elements may also be present. Furthermore, "connected" or "coupled" as used herein may include wirelessly connected or wirelessly coupled. As used herein, the term "and/or" includes all or any element and all combination of one or more of the associated listed items.

In order to make the objectives, technical solutions and advantages of the present application clearer, the embodiments of the present application will be further described in detail below with reference to the accompanying drawings.

Due to the transient photovoltage measurement, after the transient excitation, a relatively stable test environment and test process are required, no major changes are allowed, and the system environment needs to be uniform. Such a test environment is difficult to control. Once the test environment has some large changes Changes will cause certain errors in the test results. Therefore, a stable test environment is required that can reflect the transient state in the in situ reaction of the material.

In view of the above problems, embodiments of the present application provide a transient photovoltage measurement system in a liquid in-situ reaction. The technical solutions of the present application and how the technical solutions of the present application solve the above-mentioned technical problems will be described in detail below with specific examples. The following specific embodiments may be combined with each other, and the same or similar concepts or processes may not be repeated in some embodiments. The embodiments of the present application will be described below with reference to the accompanying drawings.

1-2 are schematic structural diagrams of a transient photovoltage measurement system in a liquid in-situ reaction provided by an embodiment of the present application. As shown in the figures, the system may include: a test base 1, a light source module 2, and an electrode module 3 and processing module 4.

The test base 1 is provided with a light incident module 11 and a sample test module 12. The sample test module 12 includes a test platform support 121, a test platform 122 with a light-transmitting hole 1221, and a quartz test plate 123 with a cavity 1231. The quartz test plate 123 is set on the test platform 122, and the bottom of the cavity 1231 faces the light-transmitting hole 1221. The electrode module 3 includes a mesh electrode 31 and a probe electrode 32. The mesh electrode 31 is set in the cavity 1231. The module 4 is electrically connected to the mesh electrode 31 and the probe electrode 32, respectively.

Specifically, the test base 1 provides an installation basis for each component of the system, which can be made of metal. The light incident module 11 and the sample test module 12 are both arranged on the test base 1, and both modules include a support structure (ie a test support and a lens support), one end of the support structure is connected with the test base 1 through threads, etc., and the other end Connected with the corresponding components, specifically, the light incident module 11 is used to control the optical path of the laser beam emitted by the light source module 2, so that the laser beam is finally transmitted to the test sample, and used to excite the test sample participating in the reaction to occur in situ. reaction. The sample test module 12 includes a test platform support 121, a test platform 122 and a quartz test plate 123, wherein the test platform support 121 can be a plurality of metal support rods, one end of each metal support rod is connected to the test base 1, and the other end is connected to the test platform 122 , a quartz test board 123 is set on the test platform 122 . Further, the test platform 122 is provided with a light-transmitting hole 1221, and the quartz test plate 123 is provided with a cavity 1231. When the quartz test plate 123 is set on the test platform 122, the bottom of the cavity 1231 and the light-transmitting hole are ensured. 1221 is facing, so that the laser beam can be irradiated into the cavity 1231 through the light-transmitting hole 1221. The cavity 1231 is a groove on the quartz test plate 123 , and the shape and size of the groove can be set according to requirements, so as to ensure that the mesh electrode 31 can be inserted. It can be understood that, since the quartz test plate 123 is transparent, during measurement, the laser beam can be irradiated into the cavity 1231 through the light-transmitting hole 1221, that is, the test sample in the cavity can be irradiated, ensuring the accuracy of the test sample. excitation. In addition, the mesh electrode 31 and the probe electrode 32 are respectively electrically connected to the processing module 4. During measurement, the mesh electrode 31 and the probe electrode 32 respectively feed back the measured voltage values to the processing module 4, and the processing module 4 according to The received voltage value is calculated to obtain the transient photovoltage.

It should be noted that the processing module 4 is also electrically connected to the light source module 2, and the processing module 4 includes an instruction output sub-module and a display sub-module. The instruction output sub-module can control the laser to emit laser light, and advance the parameters and interval time of the laser beam of the laser. After setting, control the laser to emit a laser beam of a predetermined wavelength and control the spot size of the laser. At the same time, the processing module 4 can also operate the movement of the stepping motor of the three-dimensional moving platform (the setting of the three-dimensional moving platform will be described in detail later), which can ensure that the probe electrode 32 controlled by the stepping motor can find the test particles. The display sub-module amplifies and fits the tested charge data, and then displays it.

When the measurement is performed, first, a liquid film containing the first test sample and the second test sample participating in the in-situ reaction is formed on the mesh of the mesh electrode 31, and the probe electrode 32 is brought into contact with the liquid film. Specifically, the contact mode of the probe electrode 32 and the liquid film is as follows: the probe electrode 32 is perpendicular to the plane where the mesh electrode 31 is located, the probe electrode 32 extends into the center of a grid of the mesh electrode 31 where the liquid membrane is located, and The electrode lines around the grid are spaced at a certain distance to ensure that a capacitance model is formed between the probe electrode 32 and the mesh electrode 31 when the in-situ reaction occurs.

In an optional embodiment of the present application, forming a liquid film containing the first test sample and the second test sample on the grid of the mesh electrode 31 can be performed in the following two ways:

In one way, the first liquid film containing the first test sample is formed on the grid of the mesh electrode, and then the solution containing the second test sample is sprayed on the first liquid film in the form of spray to obtain the first liquid film containing the first test sample. A liquid film of a test sample and a second test sample.

Specifically, first, the solution containing the particles of the first test sample (such as some catalysts in the in-situ reaction) is dropped on the grid of the network electrode in the form of droplets or liquid films. A first liquid film containing the first test sample is formed on the grid. Alternatively, the mesh electrode is immersed in the solution containing the first test sample and then taken out, and a first liquid film containing the first test sample is formed on the grid due to the effect of surface tension. Then, the non-conductive solution containing the second test sample (such as some gas, liquid, etc. in the in-situ reaction) is sprayed on the first liquid film in the form of a spray by using a spray system. In combination with the first liquid film, a liquid film containing the first test sample and the second test sample can be obtained.

In another way, a second liquid film containing the second test sample is formed on the grid of the mesh electrode, and then the probe electrode is adhered to the first test sample and then contacted with the second liquid film to obtain the first liquid film containing the first test sample. the liquid film of the test sample and the second test sample;

Specifically, first, a first test sample (eg, certain catalyst particles in an in situ reaction) is adhered to the probe electrode. Then, the non-conductive solution containing the second test sample (such as some gas, liquid, etc. in the in-situ reaction) is dropped on the grid of the network electrode in the form of droplets or liquid films. Due to the effect of surface tension, A second liquid film containing a second test sample is formed on the grid. Alternatively, the mesh electrode is immersed in the solution containing the second test sample and then taken out, and a second liquid film containing the second test sample is formed on the mesh due to the effect of surface tension. Finally, the probe electrode on which the first test sample is adhered is brought into contact with the second liquid film, so that a liquid film containing the first test sample and the second test sample can be obtained.

For example, in the process of photocatalytic oxygen reduction to generate hydrogen peroxide or carbon dioxide reduction or nitrogen reduction, photocatalyst particles are used as the first test sample, and inert liquid anhydrous acetonitrile is used as the second test sample. Oxygen or carbon dioxide or nitrogen was absorbed as a second test sample. Then, the above two ways can be used to form the liquid film including the first test sample and the second test sample. First, the solution containing the catalyst particles is formed on the grid of the mesh electrode to form a liquid film, and then the oxygen or carbon dioxide or nitrogen dissolved in liquid anhydrous acetonitrile is sprayed on the liquid film in the form of a spray to form a first test sample containing the liquid film. and the liquid film of the second test sample. Second, the oxygen or carbon dioxide or nitrogen dissolved in liquid anhydrous acetonitrile forms a liquid film on the grid of the mesh electrode, and then the probe electrode is used to stick the catalyst particles and then contact the liquid film to form the first test sample. and the liquid film of the second test sample.

In the embodiment of the present application, the surface tension of the liquid film is used to provide a closed reaction environment between the first test sample and the second test sample, thereby providing a stable reaction microenvironment for the in-situ reaction. The state signal is weak, and the closed stable environment can improve the accuracy of the transient photovoltage measurement of the in situ reaction.

A liquid film including the first test sample and the second test sample is formed on the grid of the mesh electrode 31, and after the probe electrode 32 contacts the liquid film, the light source module 2 is activated to emit a laser beam, and the light incident module is adjusted by adjusting the liquid film. 11, so that the laser beam is finally transmitted to the cavity 1231. Since the cavity 1231 is transparent, and each grid of the mesh electrode 31 is also transparent, the laser beam will be irradiated on the liquid film of the grid to excite the first test sample and the second test sample. Two test samples react in situ, causing electron migration and change. The mesh electrode 31 and the probe electrode 32 respectively feed back the measured voltage values to the processing module 4, and the processing module 4 calculates the transient photovoltage in the in situ reaction according to the received voltage values. Specifically, the probe electrode 32 is perpendicular to the plane where the mesh electrode 31 is located, the probe electrode 32 extends into the center of a grid of the mesh electrode 31 where the liquid film is located, and is separated from the electrode lines around the grid by a certain distance, Thus, a capacitance model is formed between the mesh electrode 31 and the probe electrode 32, and the change of the transient voltage difference between the two is detected by the processing module 4, and the transient photovoltage in the in-situ reaction process can be measured, thereby It provides a basis for studying the process of charge generation, separation, transport and recombination in in situ reactions in liquid state and the charge transport kinetics at the interface during in situ reactions.

The solution provided in this application adopts a mesh electrode and a probe electrode, the probe electrode is perpendicular to the surface where the mesh electrode is located, and a stable electrode comprising the first test sample and the second test sample is formed on the mesh of the mesh electrode. Liquid film, the probe electrode is contacted with the liquid film, and extends into the middle of a grid of the mesh electrode, and has a predetermined interval with the periphery of the mesh electrode. Since each mesh of the mesh electrode is a separate It has a closed environment, and each grid can meet the requirements of electromagnetic shielding, forming a natural electromagnetic shielding, which ensures the relative independence and stability of the in-situ reaction measurement when the probe electrode contacts the liquid film each time, and realizes the liquid raw material. Transient photovoltage measurements in in-situ reactions provide a basis for studying the processes of charge generation, separation, transport, and recombination in in-situ reactions in liquid state, as well as charge transport kinetics at the interface during in-situ reactions.

In an optional embodiment of the present application, as shown in FIG. 3 , a cover plate 1232 is further arranged above the cavity 1231 of the quartz test plate 123, and an opening 1233 is arranged on the cover plate 1232. The probe electrode 32 contacts the liquid film after passing through the opening 1233 .

Specifically, the cover plate 1232 covers the cavity 1231, so that part of the mesh of the mesh electrode 31 is exposed through the opening 1233. This part of the mesh is generally a part of the mesh that forms a liquid film, and the probe electrode 32 can pass through the mesh. The opening 1233 contacts the liquid film. By arranging the cover plate 1232 with the opening 1233, on the premise that the probe electrode 32 can contact the liquid film, the stability of the in-situ reaction environment is further ensured.

In an optional embodiment of the present application, as shown in FIG. 4 , the mesh electrode 31 is formed by a plurality of electrode lines 311 that are cross-connected in the transverse and longitudinal directions, and the electrode lines 311 are made of Ag and AgCl composite materials. The grid sizes of the electrodes are the same or decrease sequentially in the specified order.

The mesh electrode 31 is formed by a plurality of electrode lines 311 crisscrossed to form a plurality of grids 312 , the ends of which are wires 313 for connecting with the processing module 4 .

Specifically, the grids 312 on the mesh electrode 31 can be of the same standard size. During measurement, liquid films of different test samples can be formed in different grids 312 , and then the movement of the probe electrode 32 can realize multiple groups of liquid films. Parallel measurements of test samples. The grids 312 on the mesh electrode 31 can also be of different sizes. For example, the size of each grid 312 gradually decreases in a certain order. During measurement, the influence of the size of the grid 312 on the transient photovoltage measurement results can be studied.

The material of the electrode lines 311 of the mesh electrode 31 can be Ag/AgCl composite materials, and further part of the meshes 312 of the mesh electrode 31 can be additionally processed. For example, a mesh 312 without chemical modification can be used as a The electrode, another grid 312 is chemically modified as a reference electrode, and formed with different materials, which is used to compare the transient photovoltage test performance results of different electrodes.

It can be understood that the size of the mesh electrode is large enough, the light transmission will not be affected, and the excitation of the test sample by the external light will not be affected; when testing the liquid film, the mesh electrode is easy to form stability with the help of surface tension; therefore, this application implements The mesh electrode in the example can not only place the sample but also the working electrode and transmit light, and also has the function of electromagnetic shielding, which ensures the relative stability of the measurement environment.

In an optional embodiment of the present application, as shown in FIG. 5 , the probe electrode 32 includes a glass protective layer 321 and a micro-electrode 322 , the glass protective layer 321 is wrapped around the micro-electrode 322 , and one end of the probe electrode 32 is a micro-electrode 322 . The electrode end 323 is used for contacting the liquid film, the other end of the probe electrode is a wire end 324, which is used for electrical connection with the processing module 4 through the wire, and the diameter of the probe electrode 32 gradually changes from the wire end 324 to the micro-electrode end 323 Small.

Wherein, the glass protective layer 321 is coated with electromagnetic shielding material. The glass protective layer 321 can protect the micro-electrodes 322 , and coating an electromagnetic shielding material on it can prevent external interference to the micro-electrodes 322 .

Specifically, the probe electrode 32 is a micro-electrode 322 protected by an external glass protective layer 321. The glass protective layer 321 can protect the probe electrode 32, and can also prevent the outside world from affecting the micro-electrode by coating an electromagnetic shielding material. 322 interference; one end of the probe electrode 32 is the wire end 324 connecting the wire, and the other end of the probe electrode 32 is the micro-electrode end 323 protruding from the exposed glass protective layer 321, and the diameter gradually increases from the connecting wire end 324 to the micro-electrode end 323. becomes smaller, and the size of the microelectrode end 323 is in the range of tens of nanometers to millimeters.

In an optional embodiment of the present application, the electrode module further includes a three-dimensional moving platform, and the lead end of the probe electrode is connected to the three-dimensional moving platform. During measurement, the three-dimensional moving platform drives the probe electrode to move, so that the probe The microelectrode end of the electrode is in contact with the liquid membrane.

Specifically, the three-dimensional moving platform is controlled by a stepper motor, and can drive the probe electrode to move up, down, left, right, front, and back. Specifically, the three-dimensional mobile platform has a protruding bracket, and an installation platform is arranged at the end of the protruding bracket, the installation platform has a circuit board, and a clamp is also installed on the installation platform. The clamp is used to clamp the probe electrode. One end is placed in the fixture and connected to the circuit board in the fixture, and the charge signal tested by the probe electrode is exported to the processing module. The probe electrode can move a certain distance from the mesh electrode below through the movement of the three-dimensional motion platform. The material of the electrode wire is selected according to the work function.

There are functional modules on the circuit board. The functional modules include photoelectric detection module, signal amplification module, impedance module, etc. The photoelectric detection module can judge the preliminary position of the probe electrode and prevent the protrusion of the probe electrode front end during the movement process. Electrode end damage; signal amplification module, which can amplify the measured charge signal and export it; impedance module can reduce impedance to ensure accurate signal and impedance matching.

In an optional embodiment of the present application, the light incident module includes a lens support on which an optical fiber module, a lens module and a reflection module are mounted. During measurement, the laser beam emitted by the light source module is conducted to the lens module through the optical fiber module And emit to the reflection module, and then conduct to the cavity through the reflection module.

Further, the lens module is rotatably mounted on the lens bracket, and the lens module is provided with an angle sensor. During measurement, the lens module is rotated according to the reading of the angle sensor to adjust the optical path of the laser beam, so that the laser beam is conducted to the cavity. .

Specifically, the light source module can emit a laser beam, and the laser beam can excite the test sample. The laser beam emitted by the light source module is conducted to the lens module through the optical fiber module above the lens bracket. The lens module can determine the position through the reading of the angle sensor installed on it, and control the angle of the lens module through a mechanical device to control the propagation path of the laser beam. It is determined that the light is conducted into the cavity of the quartz plate through the lens, the test base reflecting metal, and the circular opening of the metal test platform, and the test sample in the cavity is excited. It can be understood that, during the measurement, by adjusting various components in the light incident module, it is ensured that the laser beam emitted by the light source module is conducted to the cavity, so as to stimulate the test sample to generate an in-situ reaction.

In an optional embodiment of the present application, as shown in FIG. 6 , the system further includes a shielding box 5 , and the test base 1 , the light source module 2 and the electrode module 3 are arranged in the shielding box 5 .

Specifically, the test base 1, the light source module 2 and the electrode module 3 in the measurement system are placed in the shielding box 5, and the outer shell of the shielding box 5 is a metal structure. Since the signal of the transient photovoltage is very sensitive to the external electromagnetic signal, The surface of the outer shell of the shielding box 5 is coated with electromagnetic shielding material, and the connection part of the outer shell is provided with sealing strips and/or sealants, which can seal the test chamber and prevent the influence of the external environment.

In an optional embodiment of the present application, both the test base and the test platform are coated with electromagnetic shielding material.

Specifically, in order to further enhance the electromagnetic shielding effect of the system, both the test base and the test platform are coated with electromagnetic shielding materials, so that the test platform, the test base, and the test cavity are realized for the in-situ reaction that occurs on the metal test platform. The three-layer shielding of the room (that is, the shielding box) improves the shielding effect and improves the detection accuracy.

The transient photovoltage measurement process in the liquid in-situ reaction in the present application is further described below in conjunction with the above-mentioned system structure, including:

(1) Place the test sample (including the two kinds of test samples involved in the in situ reaction) in the cavity of the quartz test plate. The bottom of the cavity is provided with a mesh electrode, and a mesh electrode containing the test sample is formed on the mesh of the mesh electrode. Liquid film (the liquid film can be formed in the way described above), the mesh electrode is electrically connected to the processing module, the quartz test board is placed on the test platform of the sample test module of the test base, and the light incident module of the test base is set There is a lens holder, connect the optical fiber in the optical fiber module on the lens holder, and then place the test base in the test chamber (ie, the shielding box), on the circuit board of the protruding holder on the three-dimensional mobile platform in the test chamber Clamp the probe electrode on the clamp, then close the test chamber.

(2) The stepper motor of the three-dimensional moving platform is controlled by the processing module to move up and down, left and right, so that the probe electrode can be in contact with the liquid film. The probe electrode is damaged by collision.

(3) After the probe electrode is in contact with the liquid film, the laser in the light source module is activated, the laser beam enters the chamber through the optical fiber, and the laser beam is reflected to the particle to be tested through the lens and the test base, and the laser beam is treated by the laser beam. The test sample is stimulated, the stimulated signal is derived through the data line, and the measured signal is displayed on the display unit after modulation, amplification and fitting.

(4) When it is necessary to measure samples at different positions, the three-dimensional moving platform is manipulated to make the probe electrodes align with the grids of different mesh electrodes to realize the measurement of samples at different positions.

Using the mesh electrode and the reflected laser light path to test the sample particles, it is possible to measure the transient photovoltage in the in-situ reaction of the particles in the liquid state. The solution of the present application adopts a mesh electrode, and the mesh electrode has the following advantages:

In the test in the prior art, block electrodes or strip electrodes are usually used for electrical connection. When using external light excitation, on the one hand, the block electrodes or strip electrodes will have a certain blocking effect on the excitation light, which will affect the excitation light. The test excitation has a certain influence; on the other hand, the test sample is easily affected by the electromagnetic influence of the external environment in an open environment. In the embodiment of the present application, a mesh electrode is used. The mesh electrode has a plurality of meshes, and the space holes of each mesh can be used as a separate environment. The electrode can meet electromagnetic shielding, which is natural electromagnetic shielding; when there are multiple sample test particles in different positions above the mesh electrode, parallel testing of multiple samples can be realized by moving the probe electrode; at the same time, because the mesh electrode is large enough , Compared with the upper electrode, the light transmission is not affected, and it will not affect the excitation of the test sample by the external light; it ensures that the mass transfer of each test chemical substance is relatively independent and stable; when testing the liquid film, the mesh electrode is easy to use the surface tension, The liquid film is stable and reliable.

It should be understood that although the various steps in the flowchart of the accompanying drawings are sequentially shown in the order indicated by the arrows, these steps are not necessarily executed in sequence in the order indicated by the arrows. Unless explicitly stated herein, the execution of these steps is not strictly limited to the order and may be performed in other orders. Moreover, at least a part of the steps in the flowchart of the accompanying drawings may include multiple sub-steps or multiple stages, and these sub-steps or stages are not necessarily executed at the same time, but may be executed at different times, and the execution sequence is also It does not have to be performed sequentially, but may be performed alternately or alternately with other steps or at least a portion of sub-steps or stages of other steps.

The above are only some embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications can be made. It should be regarded as the protection scope of the present invention.

Claims (10)

1. a transient photovoltage measurement system in a liquid in-situ reaction, is characterized in that, comprising: a test base, a light source module, an electrode module and a processing module, wherein: The test base is provided with a light incident module and a sample test module. The sample test module includes a test platform bracket, a test platform with a light-transmitting hole, and a quartz test plate with a cavity, and the quartz test plate is set on the on the test platform, and the bottom of the cavity faces the light-transmitting hole, the electrode module includes a mesh electrode and a probe electrode, the mesh electrode is arranged in the cavity, and the processing module respectively electrically connected to the mesh electrode and the probe electrode; During measurement, a liquid film containing a first test sample and a second test sample is formed on the grid of the mesh electrode, the probe electrode is in contact with the liquid film, and the laser light emitted by the light source module The beam is conducted to the cavity through the light incident module, so that the laser beam stimulates the first test sample and the second test sample to have an in-situ reaction, and causes the processing module to react according to the received The voltage values of the mesh electrode and the probe electrode obtain the transient photovoltage in the in situ reaction. 2 . The system according to claim 1 , wherein a cover plate is further arranged above the cavity of the quartz test plate, and an opening is arranged on the cover plate, and the probe is used during measurement. 3 . The electrode contacts the liquid film after passing through the opening. 3. The system according to claim 1, characterized in that, during the measurement, a liquid film comprising the first test sample and the second test sample is formed on the grid of the mesh electrode in the following manner: A first liquid film containing the first test sample is formed on the grid of the mesh electrode, and then the solution containing the second test sample is sprayed on the first liquid film in the form of spray to obtain a liquid film containing the second test sample. There is a liquid film of the first test sample and the second test sample; or, A second liquid film containing the second test sample is formed on the grid of the mesh electrode, and the probe electrode is then adhered to the first test sample and then contacted with the second liquid film to obtain a liquid film containing the second test sample. There is a liquid film of the first test sample and the second test sample; Wherein, the first test sample is the solid particles in the in-situ reaction, and the second test sample is the gas or liquid in the in-situ reaction. 4 . The system according to claim 1 , wherein the mesh electrode is formed by a plurality of electrode lines that are cross-connected with each other laterally and longitudinally, the electrode lines are made of Ag and AgCl composite materials, and the mesh electrode is made of Ag and AgCl composite materials. The grids of electrodes are either the same size or decrease sequentially in the specified order. 5 . The system according to claim 1 , wherein the probe electrode comprises a glass protective layer and a microelectrode, the glass protective layer is wrapped around the microelectrode, and one end of the probe electrode is a microelectrode. 6 . The extreme end is used for contacting the liquid film, the other end of the probe electrode is a wire end, which is used for electrical connection with the processing module through a wire, and the probe electrode is connected from the wire end to the microelectronics The extreme diameters are progressively smaller. 6. The system of claim 5, wherein the protective glass layer is coated with an electromagnetic shielding material. 7 . The system according to claim 5 , wherein the electrode module further comprises a three-dimensional moving platform, and the wire ends of the probe electrodes are connected to the three-dimensional moving platform, and during measurement, the three-dimensional moving platform is used for the measurement. 8 . The platform drives the probe electrode to move, so that the microelectrode end of the probe electrode is in contact with the liquid film. 8 . The system according to claim 1 , wherein the light incident module comprises a lens support, the optical fiber module, the lens module and the reflection module are mounted on the lens support, and during measurement, the laser beam emitted by the light source module It is transmitted to the lens module through the optical fiber module and emitted to the reflection module, and then transmitted to the cavity through the reflection module. 9 . The system according to claim 1 , wherein the system further comprises a shielding box, and the test base, the light source module and the electrode module are arranged in the shielding box. 10 . 10. The system of claim 1, wherein the test base and the test platform are each coated with an electromagnetic shielding material.

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