In-situ raman electrochemical cell for powder, thin film and gas diffusion electrodes
By designing a modular in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes, the problem of insufficient applicability of existing equipment is solved, enabling low-cost and efficient testing of multiple sample formats.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-14
- Publication Date
- 2026-03-20
AI Technical Summary
Existing in-situ Raman electrochemical cells are usually only applicable to one type of catalyst, which cannot meet the testing needs of multiple sample types, resulting in the need for multiple sets of equipment in the laboratory, which is costly and inconvenient to operate.
An in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes was designed. Multi-sample testing is achieved through modular sample stage replacement modules, including powder sample stage, thin film sample stage, and gas diffusion electrode sample stage, which are matched with the electrochemical cell module respectively. The modules are made of polyetheretherketone, polytetrafluoroethylene, or resin materials to achieve sealing and connection.
It enables a single device to meet the testing needs of various sample types, reduces costs and improves operational convenience, and is suitable for in-situ Raman testing of powder, thin film and gas diffusion electrodes.
Smart Images

Figure HDA0003999560760000011 
Figure HDA0003999560760000012 
Figure HDA0003999560760000013
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the field of spectral instrument accessories and instrumental analysis, and relates to an in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode. BACKGROUND
[0002] With the development of high-resolution spectroscopy and in-situ technology, the development and application of in-situ Raman spectroscopy technology greatly promote the research of a series of in-situ micro-physical and chemical behavior mechanisms. In-situ Raman spectroscopy technology has the advantages of rapid detection, high sensitivity, wide test range, small sample amount, non-destructive testing, fingerprint identification and the like, and has a wide application in the fields of materials, physics, chemistry, biological medicine and the like. Among them, in the application related to electrochemistry, in-situ Raman spectroscopy technology can provide molecular or even atomic level observation for the mechanism research of electrocatalytic reactions such as electrocatalytic decomposition of water reaction, electrocatalytic reduction of carbon dioxide reaction and electrocatalytic reduction of nitrogen reaction.
[0003] In the test and research of electrocatalytic reactions by using in-situ Raman spectroscopy technology, an in-situ Raman electrochemical cell is needed as a place for the occurrence of electrocatalytic reactions, and at the same time meets the needs of in-situ Raman spectrum signal collection. The catalyst forms of electrocatalytic reactions are various, which can be generally divided into powder samples, thin film samples and gas diffusion electrode samples. At present, the common in-situ Raman electrochemical cell is usually only suitable for in-situ Raman spectroscopy test of a certain catalyst form. In practice, different in-situ Raman electrochemical cells are often needed to meet the in-situ Raman test needs of different sample forms in large laboratories or research testing institutions. Therefore, an in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode samples is needed to meet the use needs of low cost, multi-scene application (applicable to various sample forms) and quick and convenient operation in actual test. SUMMARY
[0004] In order to overcome the problems in the prior art, the purpose of the present application is to provide an in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode, so as to simultaneously apply to in-situ Raman test of powder, thin film and gas diffusion electrode samples to study the micro-mechanism of related electrocatalytic reactions, and meet the use needs of low cost, multi-scene application (applicable to various sample forms) and quick and convenient operation in actual test.
[0005] In order to achieve the above purpose, the present application adopts the following scheme:
[0006] The in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode includes an electrochemical cell module, and a module for in-situ Raman test of different samples is arranged on the electrochemical cell module. The module includes a powder sample stage replacement module, a thin film sample stage replacement module and a gas diffusion electrode sample stage replacement module.
[0007] Further, the powder sample stage replacement module, the thin film sample stage replacement module and the gas diffusion electrode sample stage replacement module are all in the shape of a convex character, the electrochemical cell module is provided with a groove matching the shape of the convex character, and the powder sample stage replacement module, the thin film sample stage replacement module and the gas diffusion electrode sample stage replacement module are connected with the electrochemical cell module through fastening screws.
[0008] Further, the electrochemical cell module comprises a first liquid chamber cavity, a second liquid chamber cavity, a liquid chamber cavity sealing screw, a diaphragm gasket, a diaphragm, a light window sealing screw, a light window cover plate, a quartz light window and a light window sealing gasket; wherein the bottom surface of the first liquid chamber cavity is provided with a groove, the front and rear walls of the first liquid chamber cavity are each provided with a threaded hole communicating with the internal cavity of the first liquid chamber cavity, and a pipeline hollow screw is arranged in the threaded hole.
[0009] The front wall of the first liquid chamber cavity is provided with a threaded hole communicating with the internal cavity of the first liquid chamber cavity, and a reference electrode hollow screw is arranged in the threaded hole.
[0010] The first liquid chamber cavity is sequentially provided, from bottom to top, with a light window sealing gasket, a quartz light window and a light window cover plate.
[0011] The second liquid chamber cavity is internally provided with a cavity, and the side wall and the top surface of the second liquid chamber cavity are provided with threaded holes communicating with the cavity, and a pipeline hollow screw is arranged in the threaded hole.
[0012] The front wall of the second liquid chamber cavity is provided with a threaded hole communicating with the cavity, and a counter electrode hollow screw is arranged in the threaded hole.
[0013] The first liquid chamber cavity is sequentially provided, from bottom to top, with a diaphragm and a second liquid chamber cavity; and diaphragm gaskets are arranged on both sides of the diaphragm.
[0014] Further, the first liquid chamber cavity, the second liquid chamber cavity and the light window cover plate are processed from polyether ether ketone, polytetrafluoroethylene or resin materials.
[0015] Further, the diaphragm is a proton exchange membrane or an ion exchange membrane.
[0016] Further, the light window sealing gasket and the light window cover plate are in the shape of a circular ring.
[0017] Further, the light window cover plate and the light window sealing gasket are connected with the first liquid chamber cavity through a light window sealing screw.
[0018] Further, the powder sample stage replacement module comprises a powder sample stage, the top surface of the powder sample stage is provided with a first gasket, and the bottom surface is provided with a glassy carbon electrode hollow screw for mounting a glassy carbon electrode.
[0019] Further, the powder sample stage is processed from polyether ether ketone, polytetrafluoroethylene or resin materials.
[0020] Further, the powder sample is prepared into a slurry, and is drop-coated on a glassy carbon electrode to form the test electrode 8.
[0021] Further, the thin film sample stage replacement module comprises a thin film sample stage for arranging a thin film sample, and a second gasket arranged on the thin film sample.
[0022] Further, the thin film sample stage is made of polyether ether ketone, polytetrafluoroethylene or resin material.
[0023] Further, the thin film sample is connected with a conductive tape or a wire to form the test electrode 8.
[0024] Further, the gas diffusion electrode sample stage replacement module comprises a gas diffusion electrode sample stage, and a cross-shaped cavity is arranged in the gas diffusion electrode sample stage.
[0025] Further, the gas diffusion electrode sample stage and the observation window cover plate are made of polyether ether ketone, polytetrafluoroethylene or resin material.
[0026] A threaded hole in communication with the cross-shaped cavity is arranged on a side wall of the gas diffusion electrode sample stage, and a third gasket is arranged on a top surface and a bottom surface of a gas diffusion electrode sample arranged on the gas diffusion electrode sample stage.
[0027] The bottom surface of the gas diffusion electrode sample stage is sequentially provided with an observation window gasket, a quartz observation window and an observation window cover plate.
[0028] Further, the gas diffusion electrode sample is connected with a conductive tape or a wire to form a test electrode.
[0029] Compared with the prior art, the in-situ Raman electrochemical cell has the following beneficial effects:
[0030] The in-situ Raman electrochemical cell provided by the application is suitable for powder, thin film and gas diffusion electrode, and the powder sample stage replacement module, the thin film sample stage replacement module and the gas diffusion electrode sample stage replacement module are designed according to the powder sample, the thin film sample and the gas diffusion electrode sample respectively, and the corresponding sample stage replacement module and the electrochemical cell module are assembled for in-situ Raman spectrum test when the powder sample, the thin film sample and the gas diffusion electrode sample are tested. The replaceable design of the module of the in-situ Raman electrochemical cell realizes that most sample forms (powder sample, thin film sample and gas diffusion electrode sample) can be tested by using only one in-situ Raman electrochemical cell, the use cost of the in-situ Raman electrochemical cell is reduced, and the operation convenience of the in-situ Raman test is improved. BRIEF DESCRIPTION OF DRAWINGS
[0031] Figure 1Figure 1 is a structural exploded view of the in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode of the present application. Wherein, (a) is the electrochemical cell module combined with the powder sample stage replacement module mode, suitable for in-situ Raman testing of powder samples; (b) is the electrochemical cell module combined with the thin film sample stage replacement module mode, suitable for in-situ Raman testing of thin film samples; (c) is the electrochemical cell module combined with the gas diffusion electrode sample stage replacement module mode, suitable for in-situ Raman testing of gas diffusion electrode samples.
[0032] Figure 2 Figure 2 is a sectional view of the in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode of the present application. Wherein, (a) is the electrochemical cell module combined with the powder sample stage replacement module mode, suitable for in-situ Raman testing of powder samples; (b) is the electrochemical cell module combined with the thin film sample stage replacement module mode, suitable for in-situ Raman testing of thin film samples; (c) is the electrochemical cell module combined with the gas diffusion electrode sample stage replacement module mode, suitable for in-situ Raman testing of gas diffusion electrode samples.
[0033] Figure 3 Figure 3 is a structural schematic diagram of the electrochemical cell module. Wherein, (a) is a structural exploded view of the electrochemical cell module, (b) is a sectional view of the electrochemical cell module.
[0034] Figure 4 Figure 4 is a structural exploded view of the powder sample stage replacement module.
[0035] Figure 5 Figure 5 is a structural exploded view of the thin film sample stage replacement module.
[0036] Figure 6 Figure 6 is a structural schematic diagram of the gas diffusion electrode sample stage replacement module. Wherein, (a) is a structural exploded view of the gas diffusion electrode sample stage replacement module, (b) is a sectional view of the gas diffusion electrode sample stage replacement module.
[0037] Figure 7 Figure 7 is a working schematic diagram of Example 1.
[0038] Figure 8 Figure 8 is a working schematic diagram of Example 2.
[0039] Figure 9 Figure 9 is a working schematic diagram of Example 3.
[0040] Figure 10 is a legend of the reference signs.
[0041] 1, electrochemical cell module, 2, powder sample stage replacement module, 3, thin film sample stage replacement module, 4, gas diffusion electrode sample stage replacement module, 5, fastening screw, 1-1, first liquid chamber cavity, 1-2, pipeline hollow screw, 1-3, reference electrode hollow screw, 1-4, counter electrode hollow screw, 1-5, second liquid chamber cavity, 1-6, liquid chamber cavity sealing screw, 1-7, diaphragm gasket, 1-8, diaphragm, 1-9, light window sealing screw, 1-10, light window cover plate, 1-11, quartz light window, 1-12, light window sealing gasket, 2-1, first gasket, 2-2, powder sample stage, 2-3, glassy carbon electrode hollow screw, 2-4, glassy carbon electrode, 3-1, second gasket, 3-2, thin film sample, 3-3, thin film sample stage, 4-1, third gasket, 4-2, gas diffusion electrode sample, 4-3, gas diffusion electrode sample stage, 4-4, sample stage hollow screw, 4-5, observation window gasket, 4-6, quartz observation window, 4-7, observation window cover plate, 4-8, observation window sealing screw, 6 is a reference electrode, 7 is a counter electrode, 8 is a test electrode, 9 is a Raman spectrometer lens. DETAILED DESCRIPTION
[0042] The present application is further illustrated by the following examples.
[0043] The present application can be better understood according to the following examples, but does not limit the present application in any form. It should be noted that, without departing from the concept of the present application, the device can be modified and improved in several ways, which are within the scope of the present application.
[0044] Referring to Figures 1-9 The present application is a kind of in-situ Raman electrochemical cell suitable for powder, thin film and gas diffusion electrode, comprising electrochemical cell module 1, powder sample stage replacement module 2, thin film sample stage replacement module 3, gas diffusion electrode sample stage replacement module 4 and fastening screw 5.
[0045] Referring to Figure 1 And Figure 2 (a), (b) and (c) in the above, powder sample stage replacement module 2 is used for in-situ Raman test of powder sample, thin film sample stage replacement module 3 is used for in-situ Raman test of thin film sample, and gas diffusion electrode sample stage replacement module 4 is used for in-situ Raman test of gas diffusion electrode sample; powder sample stage replacement module 2, thin film sample stage replacement module 3 and gas diffusion electrode sample stage replacement module 4 are used respectively in corresponding sample test; the three kinds of sample stage replacement modules are all in the shape of a convex character, a plurality of through holes are formed in the periphery of the bottom of the three kinds of sample stage replacement modules, fastening screw 5 is connected with the threaded hole formed in the corresponding position of electrochemical cell module 1 through the through holes on the three kinds of sample stage replacement modules, and the sealing assembly of the three kinds of sample stage replacement modules and electrochemical cell module 1 is realized.
[0046] Referring to Figure 3 In (a) and (b), the electrochemical cell module 1 comprises a first liquid chamber cavity 1-1, a pipeline hollow screw 1-2, a reference electrode hollow screw 1-3, a counter electrode hollow screw 1-4, a second liquid chamber cavity 1-5, a liquid chamber cavity sealing screw 1-6, a diaphragm gasket 1-7, a diaphragm 1-8, a light window sealing screw 1-9, a light window cover plate 1-10, a quartz light window 1-11, and a light window sealing gasket 1-12. Among them, the first liquid chamber cavity 1-1, the second liquid chamber cavity 1-5, and the light window cover plate 1-10 are processed by using polyether ether ketone, polytetrafluoroethylene, or resin material; the bottom surface of the first liquid chamber cavity 1-1 is provided with a through hole 1-13, and the through hole 1-13 is provided with a sealing ring 1-14. Figure 1The first liquid chamber cavity 1-1 is provided with a concave cavity, and the front and rear walls of the first liquid chamber cavity 1-1 are each provided with a threaded hole communicating with the internal cavity of the first liquid chamber cavity 1-1, which is connected with a pipeline hollow screw 1-2 for sealing assembly of the electrolyte delivery pipeline, wherein one pipeline hollow screw 1-2 is used for electrolyte input, and the other pipeline hollow screw 1-2 is used for electrolyte output; the front wall of the first liquid chamber cavity 1-1 is provided with a threaded hole communicating with the internal cavity of the first liquid chamber cavity 1-1, which is connected with a reference electrode hollow screw 1-3 for assembling a reference electrode 6 (such as Ag / AgCl electrode or Hg / HgO electrode); the first liquid chamber cavity 1-1 is sequentially provided above from bottom to top with a light window sealing gasket 1-12, a quartz light window 1-11 and a light window cover plate 1-10; the light window sealing gasket 1-12 and the light window cover plate 1-10 are circular rings, and a plurality of through holes are uniformly arranged on the circumferential direction of the light window sealing gasket 1-12 and the light window cover plate 1-10; a plurality of threaded holes are uniformly arranged on the circumferential direction of the top surface of the first liquid chamber cavity 1-1; a light window sealing screw 1-9 is sequentially connected with the threaded holes on the top of the first liquid chamber cavity 1-1 through the through holes on the light window cover plate 1-10 and the light window sealing gasket 1-12, so as to realize sealing assembly of each component; the second liquid chamber cavity 1-5 is internally provided with a cubic cavity, and the left side wall and the top surface of the second liquid chamber cavity 1-5 are each provided with a threaded hole communicating with the internal cavity, which is connected with a pipeline hollow screw 1-2 for sealing assembly of the electrolyte delivery pipeline, wherein the pipeline hollow screw 1-2 located on the side wall is used for electrolyte input, and the pipeline hollow screw 1-2 located on the top surface is used for electrolyte output; the front wall of the second liquid chamber cavity 1-5 is provided with a threaded hole communicating with the internal cavity, which is connected with a counter electrode hollow screw 1-4 for assembling a counter electrode 7 (such as carbon rod electrode or platinum wire electrode); the first liquid chamber cavity 1-1 is sequentially provided with a diaphragm gasket 1-7 and a diaphragm 1-8, another diaphragm gasket 1-7 and the second liquid chamber cavity 1-5 on the left side; a plurality of through holes are uniformly arranged on the second liquid chamber cavity 1-5 and the diaphragm gasket 1-7, and a plurality of threaded holes are arranged on the corresponding position of the left side of the first liquid chamber cavity 1-1; a liquid chamber cavity sealing screw 1-6 is sequentially connected with the threaded holes on the left side of the first liquid chamber cavity 1-1 through the through holes on the second liquid chamber cavity 1-5 and the two diaphragm gaskets 1-7, so as to realize sealing assembly of each component. The diaphragm 1-8 is a proton exchange membrane or an ion exchange membrane.
[0047] Referring to Figure 4 The powder sample table replacement module 2 comprises a first gasket 2-1 and a powder sample table 2-2, a glassy carbon electrode hollow screw 2-3 and a glassy carbon electrode 2-4 which are sequentially arranged below the first gasket 2-1. The powder sample table 2-2 is made of polyether ether ketone, polytetrafluoroethylene or resin material; the powder sample is prepared as slurry, which is dropped and coated on the glassy carbon electrode 2-4 to form a test electrode 8; the glassy carbon electrode hollow screw 2-3 is connected with the threaded hole provided below the powder sample table 2-2 for assembling the glassy carbon electrode 2-4.
[0048] See Figure 5 The thin film sample stage replacement module 3 includes a second gasket 3-1 and a thin film sample 3-2 and a thin film sample stage 3-3 arranged sequentially below it. The thin film sample stage 3-3 is made of polyetheretherketone, polytetrafluoroethylene or resin material; the thin film sample 3-2 is connected to conductive tape or wire to form a test electrode 8.
[0049] See Figure 6 The gas diffusion electrode sample stage replacement module 4 includes a third gasket 4-1, a gas diffusion electrode sample 4-2, a gas diffusion electrode sample stage 4-3, a hollow screw 4-4 for the sample stage, an observation window washer 4-5, a quartz observation window 4-6, an observation window cover 4-7, and an observation window sealing screw 4-8. The gas diffusion electrode sample stage 4-3 and the observation window cover 4-7 are made of polyetheretherketone (PEEK), polytetrafluoroethylene (PTFE), or resin. The gas diffusion electrode sample stage 4-3 has a cross-shaped cavity inside, and each of its left and right side walls has a threaded through hole communicating with the internal cavity, which connects to the hollow screw 4-4 for sealing the gas delivery pipeline. One hollow screw 4-4 is used for gas input, and the other for gas output. The gas diffusion electrode sample stage 4-3 is topped with... Place a third gasket 4-1, a gas diffusion electrode sample 4-2, and another third gasket 4-1. Connect the gas diffusion electrode sample 4-2 to conductive tape or wires to form a test electrode. Below the gas diffusion electrode sample stage 4-3, install an observation window gasket 4-5, a quartz observation window 4-6, and an observation window cover plate 4-7 in sequence. Through holes are opened at the four corners of the observation window cover plate 4-7. The observation window sealing screw 4-8 is connected to the threaded hole opened at the corresponding position below the gas diffusion electrode sample stage 4-3 through the through hole of the observation window cover plate 4-7 to achieve sealed assembly of each component.
[0050] Example 1
[0051] The in-situ Raman electrochemical cell provided by this invention, suitable for powder, thin film, and gas diffusion electrodes, is used to perform in-situ Raman testing on nano-copper powder samples. The specific steps include:
[0052] 1. According to Figure 3 As shown, the electrochemical cell module is assembled;
[0053] 2. Prepare the nano-copper powder sample into a slurry, drop-coat it onto a glassy carbon electrode, allow it to air dry naturally to form a test electrode, and then arrange it according to... Figure 4 As shown, assemble the powder sample stage replacement module;
[0054] 3. Replace the electrochemical cell module obtained in step 1 and the powder sample stage module obtained in step 2 according to... Figure 1 (a) andFigure 2 The in-situ Raman electrochemical cell is assembled as shown in Figure (a);
[0055] 4. According to Figure 7 As shown, the reference electrode and the counter electrode are sealed and assembled at the corresponding interfaces, and the reference electrode, the counter electrode and the test electrode are connected to the electrochemical workstation. The reference electrode is an Ag / AgCl electrode and the counter electrode is a carbon rod electrode.
[0056] 5. According to Figure 7 As shown, an electrolyte delivery pipeline is installed at the corresponding interface, and a peristaltic pump is used to deliver the electrolyte at a flow rate of 10 mL / min. The electrolyte is a 0.5 mol / L potassium bicarbonate aqueous solution saturated with carbon dioxide.
[0057] 6. Place the in-situ Raman electrochemical cell, which has been prepared as described above, in the sample measurement area of the Raman spectrometer, with the quartz window facing the lens of the Raman spectrometer.
[0058] 7. Turn on the electrochemical workstation and Raman spectrometer to test the in-situ Raman spectral signals of the nano-copper powder sample at different reduction potentials.
[0059] Example 2
[0060] The in-situ Raman electrochemical cell provided by this invention, suitable for powder, thin film, and gas diffusion electrodes, is used to perform in-situ Raman testing on copper foil thin film samples. The specific steps include:
[0061] 1. According to Figure 3 As shown, the electrochemical cell module is assembled;
[0062] 2. Arrange the copper foil film samples according to... Figure 5 As shown, a thin film sample stage replacement module is assembled, in which a copper foil thin film sample is connected to a conductive tape to form a test electrode;
[0063] 3. Replace the electrochemical cell module obtained in step 1 and the thin film sample stage module obtained in step 2 according to... Figure 1 (b) and Figure 2 The in-situ Raman electrochemical cell is assembled as shown in Figure (b);
[0064] 4. According to Figure 8 As shown, the reference electrode and counter electrode are sealed and assembled at the corresponding interfaces, and the reference electrode, counter electrode and test electrode are connected to the electrochemical workstation. The reference electrode is an Ag / AgCl electrode and the counter electrode is a platinum wire electrode.
[0065] 5. According to Figure 8 As shown, an electrolyte delivery pipeline is installed at the corresponding interface, and a peristaltic pump is used to deliver the electrolyte at a flow rate of 10 mL / min. The electrolyte is a 0.5 mol / L potassium bicarbonate aqueous solution saturated with carbon dioxide.
[0066] 6. Place the in-situ Raman electrochemical cell, which has been prepared as described above, in the sample measurement area of the Raman spectrometer, with the quartz window facing the lens of the Raman spectrometer.
[0067] 7. Turn on the electrochemical workstation and Raman spectrometer to test the in-situ Raman spectral signals of the copper foil film sample at different reduction potentials.
[0068] Example 3
[0069] The in-situ Raman electrochemical cell provided by this invention, suitable for powder, thin film, and gas diffusion electrodes, is used to perform in-situ Raman testing on a gas diffusion electrode sample sputtered with copper nanoparticles. The specific steps include:
[0070] 1. According to Figure 3 As shown, the electrochemical cell module is assembled;
[0071] 2. The gas diffusion electrode sample sputtered with nano-copper was prepared according to... Figure 6 As shown, a gas diffusion electrode sample stage replacement module is assembled, wherein a gas diffusion electrode sample sputtered with nano-copper is connected to a conductive tape to form a test electrode.
[0072] 3. Replace the electrochemical cell module obtained in step 1 and the gas diffusion electrode sample stage module obtained in step 2 according to... Figure 1 (c) and Figure 2 The in-situ Raman electrochemical cell is assembled as shown in (c).
[0073] 4. According to Figure 9 As shown, the reference electrode and counter electrode are sealed and assembled at the corresponding interfaces, and the reference electrode, counter electrode and test electrode are connected to the electrochemical workstation. The reference electrode is an Hg / HgO electrode and the counter electrode is a platinum wire electrode.
[0074] 5. According to Figure 9 As shown, an electrolyte delivery pipeline is installed at the corresponding interface, and a peristaltic pump is used to deliver the electrolyte at a flow rate of 10 mL / min. The electrolyte is a 1 mol / L potassium hydroxide aqueous solution.
[0075] 6. According to Figure 9 As shown, a gas delivery pipeline is installed at the corresponding interface, and a gas cylinder and a gas flow controller are used to deliver the gas at a flow rate of 50 mL / min. The gas is high-purity carbon dioxide.
[0076] 7. Place the in-situ Raman electrochemical cell, which has been prepared as described above, in the sample measurement area of the Raman spectrometer, with the quartz window facing the lens of the Raman spectrometer.
[0077] 8. Turn on the electrochemical workstation and Raman spectrometer, and test the in-situ Raman spectrum signal of the gas diffusion electrode sample sputtered with nano-copper at different reduction potentials.
[0078] It is to be noted that the terms such as first and second, etc. are used herein merely to differentiate one entity or operation from another entity or operation, without necessarily requiring or implying any such actual relationship or order between such entities or operations. Moreover, the terms "comprising", "including", or any other variant thereof are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can also include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by an "including a" statement does not exclude the existence of additional identical elements in the process, method, article, or apparatus that includes the element.
[0079] It should be noted that the above description and preferred embodiments are not to be construed as limiting the design idea of the present application. Those skilled in the art can modify and change the technical idea of the present application in various forms, and such modifications and changes should be understood as falling within the scope of protection of the present application.
Claims
1. An in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes, characterized in that, It includes an electrochemical cell module (1), which is equipped with a module for in-situ Raman testing of different samples. The module includes a powder sample stage replacement module (2), a thin film sample stage replacement module (3), and a gas diffusion electrode sample stage replacement module (4). The powder sample stage replacement module (2), the thin film sample stage replacement module (3) and the gas diffusion electrode sample stage replacement module (4) are all convex in shape, with several through holes around the bottom. The electrochemical cell module (1) is provided with a groove that matches the convex shape. The fastening screw (5) is connected to the threaded hole at the corresponding position of the electrochemical cell module (1) through the through holes on the three sample stage replacement modules. The electrochemical cell module (1) includes a first liquid chamber (1-1), a second liquid chamber (1-5), a liquid chamber sealing screw (1-6), a diaphragm gasket (1-7), a diaphragm (1-8), a light window sealing screw (1-9), a light window cover plate (1-10), a quartz light window (1-11), and a light window sealing gasket (1-12); wherein, the bottom surface of the first liquid chamber (1-1) is provided with a groove, and the front and rear walls of the first liquid chamber (1-1) are each provided with a threaded through hole communicating with the internal cavity of the first liquid chamber (1-1), and a hollow pipe screw (1-2) is provided in the threaded through hole. The front wall of the first liquid chamber (1-1) is provided with a threaded through hole that communicates with the internal cavity of the first liquid chamber (1-1), and a hollow screw (1-3) for the reference electrode is provided in the threaded through hole. The first liquid chamber (1-1) is provided with a light window sealing gasket (1-12), a quartz light window (1-11) and a light window cover plate (1-10) arranged sequentially from bottom to top. The second liquid chamber (1-5) has an internal cavity. The side wall and top surface of the second liquid chamber (1-5) have threaded through holes that communicate with the cavity. A hollow pipe screw (1-2) is installed in the threaded through hole. The front wall of the second liquid chamber (1-5) is provided with a threaded through hole that communicates with the cavity, and a hollow screw (1-4) for the counter electrode is provided in the threaded through hole. A diaphragm (1-8) and a second liquid chamber (1-5) are sequentially arranged on one side of the first liquid chamber (1-1); diaphragm gaskets (1-7) are arranged on both sides of the diaphragm (1-8). The powder sample stage replacement module (2) includes a powder sample stage (2-2), a first gasket (2-1) is provided on the top surface of the powder sample stage (2-2), and a glassy carbon electrode hollow screw (2-3) for installing the glassy carbon electrode (2-4) is provided on the bottom surface; the powder sample is prepared into a slurry and dripped onto the glassy carbon electrode (2-4) to form a test electrode (8). The thin film sample stage replacement module (3) includes a thin film sample stage (3-3) for setting a thin film sample (3-2), and a second gasket (3-1) is set on the thin film sample (3-2). The gas diffusion electrode sample stage replacement module (4) includes a gas diffusion electrode sample stage (4-3), and a cross-shaped cavity is provided inside the gas diffusion electrode sample stage (4-3). A threaded through hole communicating with a cross-shaped cavity is provided on the side wall of the gas diffusion electrode sample stage (4-3), which is connected to the hollow screw (4-4) in the sample stage. A gas diffusion electrode sample (4-2) is placed on the gas diffusion electrode sample stage (4-3), and a third gasket (4-1) is provided on the top and bottom surfaces of the gas diffusion electrode sample (4-2). The bottom surface of the gas diffusion electrode sample stage (4-3) is provided with an observation window gasket (4-5), a quartz observation window (4-6), and an observation window cover plate (4-7).
2. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The first liquid chamber (1-1), the second liquid chamber (1-5), and the light window cover (1-10) are made of resin material.
3. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The first liquid chamber (1-1), the second liquid chamber (1-5), and the light window cover (1-10) are made of polyetheretherketone or polytetrafluoroethylene.
4. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The diaphragms (1-8) are proton exchange membranes.
5. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The diaphragms (1-8) are ion exchange membranes.
6. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The light window sealing gasket (1-12) and the light window cover plate (1-10) are annular.
7. The in-situ Raman electrochemical cell suitable for powder, thin film, and gas diffusion electrodes according to claim 1, characterized in that, The light window cover plate (1-10) and the light window sealing gasket (1-12) are connected to the first liquid chamber cavity (1-1) by the light window sealing screw (1-9).
Citation Information
Patent Citations
Spectral electrolytic cell suitable for in-situ characterization of Raman spectrum
CN103399000A
In-situ Raman detection electrochemical cell for synthesizing hydrocarbon fuel by electro-catalytic CO2 reduction
CN111896518A
In-situ Raman detection device and method for gas diffusion electrode
CN114280026A