CN115932017A - In-situ Raman electrochemical cell suitable for powder, film and gas diffusion electrode - Google Patents
In-situ Raman electrochemical cell suitable for powder, film and gas diffusion electrode Download PDFInfo
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Abstract
The invention discloses an in-situ Raman electrochemical cell suitable for powder, a film and a gas diffusion electrode, which comprises an electrochemical cell module, wherein the electrochemical cell module is provided with a module for carrying out in-situ Raman testing on different samples, and the module comprises a powder sample stage replacing module, a film sample stage replacing module and a gas diffusion electrode sample stage replacing module. According to the in-situ Raman electrochemical cell, the powder sample stage replacing module, the film sample stage replacing module and the gas diffusion electrode sample stage replacing module are used, so that the in-situ Raman test requirements of the powder sample, the film sample and the gas diffusion electrode sample are met respectively, and the module replaceable design of the in-situ Raman electrochemical cell realizes low cost, multi-scene applicability and rapid and convenient operation in use of the in-situ Raman electrochemical cell.
Description
Technical Field
The invention belongs to the technical field of accessories of spectroscopic instruments and instrument analysis, and relates to an in-situ Raman electrochemical cell suitable for powder, films and gas diffusion electrodes.
Background
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 microscopic physical and chemical behavior mechanisms, and the in-situ Raman spectroscopy technology has the advantages of high detection speed, high sensitivity, wide test range, small required sample amount, nondestructive testing, fingerprint identification and the like, and is widely applied to various fields of materials, physics, chemistry, biomedicine and the like. In the relevant electrochemical application, the in-situ Raman spectrum technology can provide molecular and even atomic level observation for the mechanism research of electrocatalysis reactions such as electrocatalysis water decomposition reaction, electrocatalysis carbon dioxide reduction reaction and electrocatalysis nitrogen reduction reaction.
In the test research of the electro-catalytic reaction by utilizing the in-situ Raman spectrum technology, an in-situ Raman electrochemical cell is required to be used as a place for generating the electro-catalytic reaction, and the requirement of acquiring in-situ Raman spectrum signals is met. The form of the catalyst for electrocatalytic reactions is various and can be generally divided into powder samples, thin film samples and gas diffusion electrode samples. At present, a common in-situ raman electrochemical cell is generally only suitable for in-situ raman spectrum testing in a certain catalyst form, and in practice, a plurality of different in-situ raman electrochemical cells are often needed to meet the in-situ raman testing requirements of a large-scale laboratory or a scientific research testing institution for different sample forms. Therefore, an in-situ raman electrochemical cell which can be simultaneously suitable for powder, thin film and gas diffusion electrode samples is needed to meet the use requirements of low cost, multi-scenario applicability (applicable to various sample forms) and quick and convenient operation in practical tests.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide an in-situ raman electrochemical cell suitable for powder, films and gas diffusion electrodes, so as to be simultaneously suitable for in-situ raman testing of powder, film and gas diffusion electrode samples to research the micro mechanism of related electrocatalytic reactions, and meet the use requirements of low cost, multi-scenario applicability (applicable to various sample forms) and quick and convenient operation in practical testing.
In order to achieve the purpose, the invention adopts the following scheme:
the in-situ Raman electrochemical cell suitable for powder, films and gas diffusion electrodes comprises an electrochemical cell module, wherein the electrochemical cell module is provided with a module for carrying out in-situ Raman testing on different samples, and the module comprises a powder sample stage replacing module, a film sample stage replacing module and a gas diffusion electrode sample stage replacing module.
Furthermore, the powder sample stage replacement module, the film sample stage replacement module and the gas diffusion electrode sample stage replacement module are all in a convex shape, grooves matched with the convex shape are formed in the electrochemical cell module, and the powder sample stage replacement module, the film sample stage replacement module and the gas diffusion electrode sample stage replacement module are connected with the electrochemical cell module through fastening screws.
Furthermore, 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, an optical window sealing screw, an optical window cover plate, a quartz optical window and an optical window sealing gasket; the bottom surface of the cavity of the first liquid chamber is provided with a groove, the front wall and the rear wall of the cavity of the first liquid chamber are respectively provided with a threaded through hole communicated with the cavity of the first liquid chamber, and a pipeline hollow screw is arranged in the threaded through hole;
the front wall of the cavity of the first liquid chamber is provided with a threaded through hole communicated with the cavity inside the cavity of the first liquid chamber, and a reference electrode hollow screw is arranged in the threaded through hole;
an optical window sealing gasket, a quartz optical window and an optical window cover plate are sequentially arranged on the first liquid chamber cavity from bottom to top;
a cavity is formed in the second liquid chamber cavity, a threaded through hole communicated with the cavity is formed in the side wall and the top surface of the second liquid chamber cavity, and a pipeline hollow screw is arranged in the threaded through hole;
the front wall of the second liquid chamber cavity is provided with a threaded through hole communicated with the cavity, and a counter electrode hollow screw is arranged in the threaded through hole;
a diaphragm and a second liquid chamber are sequentially arranged on one side of the first liquid chamber cavity; diaphragm gaskets are arranged on two sides of the diaphragm.
Furthermore, the first liquid chamber cavity, the second liquid chamber cavity and the optical window cover plate are processed by polyether-ether-ketone, polytetrafluoroethylene or resin materials.
Further, the diaphragm is a proton exchange membrane or an ion exchange membrane.
Furthermore, the sealing gasket and the cover plate are circular.
Further, the optical window cover plate and the optical window sealing gasket are connected with the first liquid chamber cavity through optical window sealing screws.
Further, the powder sample stage replacement module comprises a powder sample stage, a first gasket is arranged on the top surface of the powder sample stage, and a glassy carbon electrode hollow screw for mounting a glassy carbon electrode is arranged on the bottom surface of the powder sample stage.
Furthermore, the powder sample platform is made of polyether-ether-ketone, polytetrafluoroethylene or resin materials.
Further, the powder sample is prepared into slurry, and the slurry is dripped on a glassy carbon electrode to prepare a test electrode 8.
Further, the film sample stage replacing module comprises a film sample stage for arranging a film sample, and a second gasket is arranged on the film sample.
Further, the film sample table is made of polyether-ether-ketone, polytetrafluoroethylene or resin materials;
further, the film sample is connected to a conductive tape or wire to make the test electrode 8.
Further, the gas diffusion electrode sample stage replacing module comprises a gas diffusion electrode sample stage, and a cross-shaped cavity is formed in the gas diffusion electrode sample stage;
furthermore, the gas diffusion electrode sample stage and the observation window cover plate are processed by polyether-ether-ketone, polytetrafluoroethylene or resin materials.
A threaded through hole communicated with the cross-shaped cavity is formed in the side wall of the gas diffusion electrode sample table, a gas diffusion electrode sample is arranged on the gas diffusion electrode sample table, and third gaskets are arranged on the top surface and the bottom surface of the gas diffusion electrode sample;
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.
Further, the gas diffusion electrode sample is connected with a conductive tape or a lead to make a test electrode.
Compared with the prior art, the invention has the beneficial effects that:
the in-situ Raman electrochemical cell applicable to the powder, the film and the gas diffusion electrode, provided by the invention, is characterized in that a powder sample stage replacing module, a film sample stage replacing module and a gas diffusion electrode sample stage replacing module are correspondingly designed aiming at the powder, the film and the gas diffusion electrode samples, and when the testing requirements of the powder, the film and the gas diffusion electrode samples are met, the corresponding sample stage replacing module and the electrochemical cell module are assembled for in-situ Raman spectrum testing. The module replaceable design of the in-situ Raman electrochemical cell realizes that the testing requirements of most sample forms (powder samples, film samples and gas diffusion electrode samples) can be met by 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 also improved.
Drawings
Figure 1 is an exploded view of an in situ raman electrochemical cell of the present invention suitable for use with powder, membrane and gas diffusion electrodes. The device comprises an electrochemical cell module, a powder sample table, a power supply module and a power supply module, wherein (a) is a combined mode of the electrochemical cell module and the powder sample table replacing module, and is suitable for in-situ Raman testing of a powder sample; (b) The combined mode of the electrochemical cell module and the membrane sample stage replacement module is suitable for in-situ Raman testing of a membrane sample; (c) The combined mode of the electrochemical cell module and the gas diffusion electrode sample stage replacing module is suitable for in-situ Raman testing of a gas diffusion electrode sample.
Figure 2 is a cross-sectional view of an in-situ raman electrochemical cell of the present invention suitable for use with powder, membrane and gas diffusion electrodes. The device comprises an electrochemical cell module, a powder sample table, a power supply module and a power supply module, wherein (a) is a combined mode of the electrochemical cell module and the powder sample table replacing module, and is suitable for in-situ Raman testing of a powder sample; (b) The combination mode of the electrochemical cell module and the membrane sample stage replacement module is suitable for in-situ Raman testing of the membrane sample; (c) The in-situ Raman spectrometer is a combined mode of an electrochemical cell module and a gas diffusion electrode sample stage replacement module, and is suitable for in-situ Raman testing of a gas diffusion electrode sample.
Fig. 3 is a schematic structural view of an electrochemical cell module. Wherein (a) is a structural exploded view of the electrochemical cell module, and (b) is a sectional view of the electrochemical cell module.
Fig. 4 is a structural exploded view of a powder sample stage replacement module.
Fig. 5 is a structural exploded view of a membrane sample stage replacement module.
FIG. 6 is a schematic structural diagram of a gas diffusion electrode sample stage replacement module. The gas diffusion electrode sample stage replacement module comprises a gas diffusion electrode sample stage replacement module body, a gas diffusion electrode sample stage replacement module body and a gas diffusion electrode sample stage replacement module body, wherein (a) is a structural disassembly drawing of the gas diffusion electrode sample stage replacement module body, and (b) is a cross-sectional drawing of the gas diffusion electrode sample stage replacement module body.
Fig. 7 is a schematic diagram of the operation of embodiment 1.
FIG. 8 is a schematic diagram showing the operation of example 2.
FIG. 9 is a schematic diagram showing the operation of example 3.
Description of reference numerals:
1. an electrochemical cell module, 2, a powder sample stage replacing module, 3, a film sample stage replacing module, 4, a gas diffusion electrode sample stage replacing module, 5, a fastening screw, 1-1, a first liquid chamber cavity, 1-2, a pipeline hollow screw, 1-3, a reference electrode hollow screw, 1-4, a counter electrode hollow screw, 1-5, a second liquid chamber cavity, 1-6, a liquid chamber cavity sealing screw, 1-7, a diaphragm gasket, 1-8, a diaphragm, 1-9, an optical window sealing screw, 1-10, an optical window cover plate, 1-11, a quartz optical window, 1-12 and an optical window sealing gasket, 2-1 parts of a first gasket, 2-2 parts of a powder sample table, 2-3 parts of a glassy carbon electrode hollow screw, 2-4 parts of a glassy carbon electrode, 3-1 parts of a second gasket, 3-2 parts of a film sample, 3-3 parts of a film sample table, 4-1 parts of a third gasket, 4-2 parts of a gas diffusion electrode sample, 4-3 parts of a gas diffusion electrode sample table, 4-4 parts of a sample table hollow screw, 4-5 parts of an observation window gasket, 4-6 parts of a quartz observation window, 4-7 parts of an observation window cover plate, 4-8 parts of an observation window sealing screw, 6 parts of a reference electrode, 7 parts of a counter electrode, 8 parts of a test electrode and 9 parts of a Raman spectrometer lens.
Detailed Description
The invention is further illustrated by the following examples.
The invention will be better understood from the following examples, which are not intended to limit the invention in any way. It should be noted that several variants and modifications of the device can be made without departing from the inventive concept, which shall fall within the scope of protection of the present invention.
Referring to fig. 1-9, the in-situ raman electrochemical cell suitable for powder, membrane and gas diffusion electrode according to the present invention comprises an electrochemical cell module 1, a powder sample stage replacement module 2, a membrane sample stage replacement module 3, a gas diffusion electrode sample stage replacement module 4 and a fastening screw 5.
Referring to fig. 1 and 2 (a), (b) and (c), the powder sample stage replacement module 2 is used for in-situ raman testing of a powder sample, the membrane sample stage replacement module 3 is used for in-situ raman testing of a membrane sample, and the gas diffusion electrode sample stage replacement module 4 is used for in-situ raman testing of a gas diffusion electrode sample; the three sample stage replacing modules, namely the powder sample stage replacing module 2, the film sample stage replacing module 3 and the gas diffusion electrode sample stage replacing module 4, are respectively used in corresponding sample tests; three kinds of sample platform replacement modules all are the type of dogbone, and a plurality of through-holes have been seted up around its bottom, and fastening screw 5 is connected with the screw hole that electrochemical cell module 1 corresponding position was seted up through the through-hole on three kinds of sample platform replacement modules, realizes three kinds of sample platform replacement modules and electrochemical cell module 1's sealed assembly.
Referring to (a) and (b) of fig. 3, an electrochemical cell module 1 includes 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, an optical window sealing screw 1-9, an optical window cover plate 1-10, a quartz optical window 1-11, and an optical window sealing gasket 1-12. The first liquid chamber cavity 1-1, the second liquid chamber cavity 1-5 and the optical window cover plate 1-10 are made of polyether-ether-ketone, polytetrafluoroethylene or resin materials; an inward concave cavity shown as b in the figure 1 is formed in the bottom surface of the first liquid chamber cavity 1-1, the front wall and the rear wall of the first liquid chamber cavity 1-1 are respectively provided with a threaded through hole communicated with the cavity inside the first liquid chamber cavity 1-1, the threaded through holes are respectively connected with pipeline hollow screws 1-2 and used for sealing assembly of an electrolyte conveying pipeline, one pipeline hollow screw 1-2 is used for inputting electrolyte, and the other pipeline hollow screw 1-2 is used for outputting electrolyte; the front wall of the first liquid chamber cavity 1-1 is provided with a threaded through hole communicated with the internal cavity of the first liquid chamber cavity 1-1, and the threaded through hole is connected with a reference electrode hollow screw 1-3 and used for assembling a reference electrode 6 (such as an Ag/AgCl electrode or an Hg/HgO electrode); an optical window sealing gasket 1-12, a quartz optical window 1-11 and an optical window cover plate 1-10 are sequentially arranged above the first liquid chamber cavity 1-1 from bottom to top; the optical window sealing gasket 1-12 and the optical window cover plate 1-10 are circular rings, a plurality of through holes are uniformly formed in the circumferential direction of the optical window sealing gasket 1-12 and the optical window cover plate 1-10, and a plurality of threaded holes are uniformly formed in the circumferential direction of the top surface of the first liquid chamber cavity 1-1; the optical window sealing screws 1-9 are connected with threaded holes above the first liquid chamber cavity 1-1 sequentially through holes in the optical window cover plate 1-10 and the optical window sealing gasket 1-12, and sealing assembly of all parts is achieved; a cubic cavity is formed in the second liquid chamber cavity 1-5, a threaded through hole communicated with the internal cavity is formed in each of the left side wall and the top surface of the second liquid chamber cavity 1-5, the threaded through holes are respectively connected with the pipeline hollow screws 1-2 and used for sealing and assembling an electrolyte conveying pipeline, wherein the pipeline hollow screws 1-2 on the side walls are used for inputting electrolyte, and the pipeline hollow screws 1-2 on the top surface are used for outputting electrolyte; the front wall of the second liquid chamber cavity 1-5 is provided with a threaded through hole communicated with the inner cavity, is connected with a hollow screw 1-4 of a counter electrode and is used for assembling a counter electrode 7 (such as a carbon rod electrode or a platinum wire electrode); the left side of the first liquid chamber cavity 1-1 is sequentially provided with a diaphragm gasket 1-7, a diaphragm 1-8, another diaphragm gasket 1-7 and a second liquid chamber cavity 1-5; the diaphragm gaskets 1-7 and the second liquid chamber cavity 1-5 are uniformly provided with a plurality of through holes, the corresponding position on the left side of the first liquid chamber cavity 1-1 is provided with a plurality of threaded holes, and liquid chamber cavity sealing screws 1-6 sequentially pass through the through holes on the second liquid chamber cavity 1-5 and the two diaphragm gaskets 1-7 and are connected with the threaded holes on the left side of the first liquid chamber cavity 1-1, so that the sealing assembly of each part is realized. The diaphragms 1-8 are diaphragms such as proton exchange membranes or ion exchange membranes.
Referring to fig. 4, the powder sample stage replacement module 2 comprises a first gasket 2-1, a powder sample stage 2-2, a glassy carbon electrode hollow screw 2-3 and a glassy carbon electrode 2-4 which are arranged below the first gasket in sequence. Wherein, the powder sample table 2-2 is processed by polyether-ether-ketone, polytetrafluoroethylene or resin material; preparing a powder sample into slurry, and dripping the slurry on a glassy carbon electrode 2-4 to prepare a test electrode 8; the glassy carbon electrode hollow screw 2-3 is connected with a threaded through hole arranged below the powder sample stage 2-2 and used for assembling the glassy carbon electrode 2-4.
Referring to fig. 5, the film sample stage replacing module 3 includes a second pad 3-1, and a film sample 3-2 and a film sample stage 3-3 sequentially disposed thereunder. Wherein, the film sample stage 3-3 is processed by polyetheretherketone, polytetrafluoroethylene or resin material; the film sample 3-2 was connected to a conductive tape or wire to make a test electrode 8.
Referring to fig. 6, the gas diffusion electrode sample stage replacement module 4 comprises a third gasket 4-1, a gas diffusion electrode sample 4-2, a gas diffusion electrode sample stage 4-3, a sample stage hollow screw 4-4, an observation window gasket 4-5, a quartz observation window 4-6, an observation window cover plate 4-7 and an observation window sealing screw 4-8. Wherein, the gas diffusion electrode sample stage 4-3 and the observation window cover plate 4-7 are processed by polyether-ether-ketone, polytetrafluoroethylene or resin materials; a cross-shaped cavity is formed in the gas diffusion electrode sample table 4-3, the left side wall and the right side wall of the gas diffusion electrode sample table 4-3 are respectively provided with a threaded through hole communicated with the inner cavity, and the threaded through holes are respectively connected with the hollow screws 4-4 of the sample table and used for sealing and assembling of a gas conveying pipeline, wherein one hollow screw 4-4 of the sample table is used for gas input, and the other hollow screw is used for gas output; a third gasket 4-1, a gas diffusion electrode sample 4-2 and another third gasket 4-1 are sequentially arranged above the gas diffusion electrode sample table 4-3, and the gas diffusion electrode sample 4-2 is connected with a conductive adhesive tape or a lead to form a test electrode; an observation window gasket 4-5, a quartz observation window 4-6 and an observation window cover plate 4-7 are sequentially arranged below the gas diffusion electrode sample table 4-3; through holes are respectively formed in four corners of the observation window cover plate 4-7, and the observation window sealing screws 4-8 are connected with threaded holes formed in corresponding positions below the gas diffusion electrode sample stage 4-3 through the through holes of the observation window cover plate 4-7, so that sealing assembly of all parts is achieved.
Example 1
The in-situ Raman electrochemical cell applicable to the powder, the film and the gas diffusion electrode provided by the invention is used for carrying out in-situ Raman test on a nano copper powder sample, and the specific steps comprise:
1. as shown in fig. 3, the electrochemical cell module is assembled;
2. preparing a nano copper powder sample into slurry, dripping the slurry on a glassy carbon electrode, naturally airing to prepare a test electrode, and assembling a powder sample stage replacement module according to the diagram shown in FIG. 4;
3. assembling the electrochemical cell module obtained in the step 1 and the powder sample stage replacement module obtained in the step 2 into an in-situ Raman electrochemical cell as shown in (a) in FIG. 1 and (a) in FIG. 2;
4. according to the scheme shown in fig. 7, a reference electrode and a counter electrode are hermetically assembled at corresponding interfaces, and the reference electrode, the counter electrode and a test electrode are connected with an electrochemical workstation, wherein the reference electrode is an Ag/AgCl electrode, and the counter electrode is a carbon rod electrode;
5. according to the figure 7, an electrolyte conveying pipeline is assembled at a corresponding interface, and a peristaltic pump is used for conveying electrolyte, wherein the flow rate of the electrolyte is 10mL/min, and the electrolyte is a potassium bicarbonate aqueous solution with carbon dioxide saturation concentration of 0.5 mol/L;
6. the prepared in-situ Raman electrochemistry Chi Zhiyu Raman spectrometer sample measurement area is aligned to the lens of the Raman spectrometer through the quartz optical window;
7. and opening the electrochemical workstation and the Raman spectrometer, and testing the in-situ Raman spectrum signals of the nano-copper powder sample under different reduction potentials.
Example 2
The in-situ Raman electrochemical cell applicable to the powder, the film and the gas diffusion electrode provided by the invention is used for carrying out in-situ Raman test on a copper foil film sample, and the in-situ Raman electrochemical cell comprises the following specific steps:
1. as shown in fig. 3, the electrochemical cell module is assembled;
2. assembling a copper foil film sample according to a film sample stage replacement module shown in fig. 5, wherein the copper foil film sample is connected with a conductive adhesive tape to form a test electrode;
3. assembling the electrochemical cell module obtained in the step 1 and the membrane sample stage replacement module obtained in the step 2 into an in-situ Raman electrochemical cell as shown in (b) in FIG. 1 and (b) in FIG. 2;
4. according to the scheme shown in fig. 8, a reference electrode and a counter electrode are hermetically assembled at corresponding interfaces, and the reference electrode, the counter electrode and a test electrode are connected with an electrochemical workstation, wherein the reference electrode is an Ag/AgCl electrode, and the counter electrode is a platinum wire electrode;
5. according to the figure 8, an electrolyte conveying pipeline is assembled at the corresponding interface, the electrolyte is conveyed by a peristaltic pump, the flow rate of the electrolyte is 10mL/min, and the electrolyte is a potassium bicarbonate aqueous solution with the carbon dioxide saturation concentration of 0.5 mol/L;
6. the prepared in-situ Raman electrochemistry Chi Zhiyu Raman spectrometer sample measurement area is aligned to the lens of the Raman spectrometer through the quartz optical window;
7. and opening the electrochemical workstation and the Raman spectrometer, and testing the in-situ Raman spectrum signals of the copper foil film sample under different reduction potentials.
Example 3
The in-situ Raman electrochemical cell applicable to the powder, the film and the gas diffusion electrode provided by the invention is used for carrying out in-situ Raman test on a gas diffusion electrode sample sputtered with nano-copper, and the in-situ Raman electrochemical cell specifically comprises the following steps:
1. as shown in fig. 3, the electrochemical cell module is assembled;
2. assembling a gas diffusion electrode sample stage replacement module for the gas diffusion electrode sample sputtered with the nano-copper according to the figure 6, wherein the gas diffusion electrode sample sputtered with the nano-copper is connected with a conductive adhesive tape to manufacture a test electrode;
3. assembling the electrochemical cell module obtained in the step 1 and the gas diffusion electrode sample stage replacement module obtained in the step 2 into an in-situ Raman electrochemical cell as shown in (c) in FIG. 1 and (c) in FIG. 2;
4. according to the illustration in fig. 9, a reference electrode and a counter electrode are hermetically assembled at the corresponding interfaces, and the reference electrode, the counter electrode and the test electrode are connected to an electrochemical workstation, wherein the reference electrode is an Hg/HgO electrode, and the counter electrode is a platinum wire electrode;
5. according to the illustration in fig. 9, an electrolyte conveying pipeline is assembled at the corresponding interface, and a peristaltic pump is used for conveying electrolyte, wherein the flow rate of the electrolyte is 10mL/min, and the electrolyte is a potassium hydroxide aqueous solution with the concentration of 1 mol/L;
6. according to FIG. 9, a gas delivery pipeline is installed at the corresponding interface, and a gas cylinder and a gas flow controller are used for delivering gas with the gas flow rate of 50mL/min, wherein the gas is high-purity carbon dioxide;
7. the prepared in-situ Raman electrochemistry Chi Zhiyu Raman spectrometer sample measurement area is aligned to the lens of the Raman spectrometer through the quartz optical window;
8. and opening the electrochemical workstation and the Raman spectrometer, and testing the in-situ Raman spectrum signals of the gas diffusion electrode sample sputtered with the nano-copper under different reduction potentials.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation 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 may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
It should be noted that the above description and the preferred embodiments are not to be construed as limiting the design concept of the present invention. Those skilled in the art can modify the technical idea of the present invention in various forms, and such modifications and changes are understood to fall within the scope of the present invention.
Claims (10)
1. The in-situ Raman electrochemical cell suitable for powder, films and gas diffusion electrodes is characterized by comprising an electrochemical cell module (1), wherein the electrochemical cell module (1) is provided with a module for carrying out in-situ Raman testing on different samples, and the module comprises a powder sample stage replacing module (2), a film sample stage replacing module (3) and a gas diffusion electrode sample stage replacing module (4).
2. The in-situ Raman electrochemical cell applicable to the powder, the membrane and the gas diffusion electrode according to claim 1, wherein the powder sample stage replacement module (2), the membrane sample stage replacement module (3) and the gas diffusion electrode sample stage replacement module (4) are all in a convex shape, grooves matched with the convex shape are formed in the electrochemical cell module (1), and the powder sample stage replacement module (2), the membrane sample stage replacement module (3), the gas diffusion electrode sample stage replacement module (4) and the electrochemical cell module (1) are connected through fastening screws (5).
3. The in-situ raman electrochemical cell suitable for use with powder, thin film and gas diffusion electrodes according to claim 1, characterized in that the electrochemical cell module (1) comprises a first liquid chamber cavity (1-1), 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); the bottom surface of the first liquid chamber cavity (1-1) is provided with a groove, the front wall and the rear wall of the first liquid chamber cavity (1-1) are respectively provided with a threaded through hole communicated with the inner cavity of the first liquid chamber cavity (1-1), and a pipeline hollow screw (1-2) is arranged in the threaded through hole;
the front wall of the first liquid chamber cavity (1-1) is provided with a threaded through hole communicated with the inner cavity of the first liquid chamber cavity (1-1), and a reference electrode hollow screw (1-3) is arranged in the threaded through hole;
an optical window sealing gasket (1-12), a quartz optical window (1-11) and an optical window cover plate (1-10) are sequentially arranged on the first liquid chamber cavity (1-1) from bottom to top;
a cavity is formed in the second liquid chamber cavity (1-5), a threaded through hole communicated with the cavity is formed in the side wall and the top surface of the second liquid chamber cavity (1-5), and a pipeline hollow screw (1-2) is arranged in the threaded through hole;
the front wall of the second liquid chamber cavity (1-5) is provided with a threaded through hole communicated with the cavity, and a counter electrode hollow screw (1-4) is arranged in the threaded through hole;
a diaphragm (1-8) and a second liquid chamber cavity (1-5) are sequentially arranged on one side of the first liquid chamber cavity (1-1); diaphragm gaskets (1-7) are arranged on two sides of the diaphragms (1-8).
4. The in-situ raman electrochemical cell suitable for use with powder, film and gas diffusion electrodes according to claim 3, characterized in that the first liquid chamber cavity (1-1), the second liquid chamber cavity (1-5) and the optical window cover plate (1-10) are processed using polyetheretherketone, polytetrafluoroethylene or a resin material.
5. In-situ raman electrochemical cell suitable for powder, film and gas diffusion electrodes according to claim 3, characterized in that the diaphragms (1-8) are proton exchange membranes or ion exchange membranes.
6. The in-situ raman electrochemical cell suitable for use with powder, film and gas diffusion electrodes according to claim 3, wherein the optical window sealing gaskets (1-12) and the optical window cover plates (1-10) are circular rings.
7. The in-situ raman electrochemical cell suitable for use with powder, film and gas diffusion electrodes according to claim 3, characterized in that the optical window cover plate (1-10) and the optical window sealing gasket (1-12) are connected to the first liquid chamber cavity (1-1) by optical window sealing screws (1-9).
8. The in-situ raman electrochemical cell suitable for powder, membrane and gas diffusion electrodes according to claim 1, characterized in that the powder sample stage replacement module (2) comprises a powder sample stage (2-2), the top surface of the powder sample stage (2-2) is provided with a first gasket (2-1), and the bottom surface is provided with a glassy carbon electrode hollow screw (2-3) for mounting a glassy carbon electrode (2-4).
9. The in-situ raman electrochemical cell suitable for use with powder, membrane and gas diffusion electrodes according to claim 1, characterized in that the membrane sample stage replacement module (3) comprises a membrane sample stage (3-3) for disposing the membrane sample (3-2), the membrane sample (3-2) having disposed thereon the second gasket (3-1).
10. The in-situ raman electrochemical cell suitable for use with powder, film and gas diffusion electrodes according to claim 1, characterized in that the gas diffusion electrode sample stage replacement module (4) comprises a gas diffusion electrode sample stage (4-3), the interior of the gas diffusion electrode sample stage (4-3) being provided with a cross-shaped cavity;
a threaded through hole communicated with the cross-shaped cavity is formed in the side wall of the gas diffusion electrode sample table (4-3), a gas diffusion electrode sample (4-2) is arranged on the gas diffusion electrode sample table (4-3), and third gaskets (4-1) are arranged on the top surface and the bottom surface of the gas diffusion electrode sample (4-2);
an observation window gasket (4-5), a quartz observation window (4-6) and an observation window cover plate (4-7) are sequentially arranged on the bottom surface of the gas diffusion electrode sample table (4-3).
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