CN220154260U - Heating electrochemical in-situ Raman spectrum pool - Google Patents
Heating electrochemical in-situ Raman spectrum pool Download PDFInfo
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- CN220154260U CN220154260U CN202321366980.8U CN202321366980U CN220154260U CN 220154260 U CN220154260 U CN 220154260U CN 202321366980 U CN202321366980 U CN 202321366980U CN 220154260 U CN220154260 U CN 220154260U
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- inner cavity
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- heating
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 58
- 238000010438 heat treatment Methods 0.000 title claims abstract description 53
- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 20
- 238000001069 Raman spectroscopy Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 9
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 4
- 229920002530 polyetherether ketone Polymers 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000012512 characterization method Methods 0.000 abstract description 15
- 238000012360 testing method Methods 0.000 abstract description 13
- 238000003487 electrochemical reaction Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 11
- 238000002474 experimental method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000003792 electrolyte Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000006056 electrooxidation reaction Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 210000005056 cell body Anatomy 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000012634 optical imaging Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000003332 Raman imaging Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000000155 in situ X-ray diffraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The utility model discloses a heating electrochemical in-situ Raman spectrum pool, which relates to the field of in-situ characterization instruments and comprises a window assembly, a counter electrode, a heating binding post, a reference electrode, an inner cavity, a heating furnace, a working electrode, an outer shell, a temperature measuring element and a temperature control box; the inner cavity is arranged in the outer shell, and the counter electrode, the reference electrode and the working electrode are respectively connected into the inner cavity; the window component is arranged on the outer shell and corresponds to the interior of the inner cavity; the heating furnace is arranged inside the outer shell and contacts the outside of the inner cavity; the heating terminal sets up on the heating furnace, and temperature measuring element sets up on the inner chamber, and temperature control box is all connected to heating terminal and temperature measuring element. The utility model has the advantages that: the method has the in-situ Raman spectrum testing function in the electrochemical reaction process at high temperature, and can explore the influence of temperature on the in-situ Raman spectrum characterization experiment of the object to be tested.
Description
Technical Field
The utility model relates to the field of in-situ characterization instruments, in particular to a heating electrochemical in-situ Raman spectrum pool.
Background
In the field of electrochemical basic research, the study of eigendynamics about related reactions has been a question of considerable interest to researchers. The traditional ex-situ characterization method cannot realize in-situ real-time analysis of the electrochemical reaction process to ascertain the reaction mechanism, and can only be combined with the state of the material at the initial stage of the reaction and the final state information after the reaction is completed to supposedly demonstrate the reaction mechanism, so that the analysis of the intermediate state of the reaction is greatly hindered. The advent of in situ characterization has addressed this troublesome problem, and Jia-XingZheng et al have discovered that electrochemical oxidation of Cr in alkaline solutions involves two steps by combining electrochemical and in situ raman spectroscopy to investigate the electrochemical oxidation behavior of Cr in 0.5M NaOH solutions to obtain in situ characterization data in order to elucidate the mechanism of Cr electrodeposition, electrochemical oxidation and corrosion, and developed a method for detecting CrO in chrome plating solutions based on this mechanism 4 2- Electrochemical method of concentration. In order to analyze the adsorption and desorption mechanism of the catalyst in the electrocatalytic reaction, the problems of hydrogen evolution and oxygen evolution in the reaction process, the phase change of the surface interface of the battery electrode material and the like, a plurality of technologies such as in-situ infrared spectroscopy, in-situ Raman spectroscopy, in-situ X-ray diffraction and the like are generally required to be used, and the development of a relevant in-situ cell body is a key for carrying out relevant in-situ experimental characterization.
The raman spectroscopy technology is widely used as a spectroscopic technology applied to material structure analysis, and is used for realizing structural research on materials by measuring scattering signals generated by incident light acting on the surfaces of the materials and providing data support for researching reaction mechanisms. Currently, there has been great interest in the design of in situ electrochemical raman spectroscopy cells and related devices have been successfully developed. For example, patent document CN112285173a discloses a method and related device for optical/electrochemical in-situ raman detection, and by introducing a light source, an in-situ raman detection device suitable for photochemical, electrochemical and photoelectrochemical reactions is designed, and connection with a raman spectrometer is completed, so as to realize in-situ optical/electrochemical raman detection. The conventional electrochemical in-situ detection device considers the influence of illumination on electrochemical reaction, and for most electrochemical experiments, the temperature is also an important consideration for developing in-situ spectrum experiments, and the conventional electrochemical in-situ detection device cannot detect the influence of the temperature on the in-situ spectrum experiments.
Disclosure of Invention
The utility model aims to solve the technical problems of realizing the in-situ Raman spectrum test function of the electrochemical reaction process at high temperature and exploring the influence of temperature on the in-situ Raman spectrum characterization experiment of an object to be tested.
The utility model solves the technical problems by the following technical means: a heating electrochemical in-situ Raman spectrum pool comprises a window component, a counter electrode, a heating binding post, a reference electrode, an inner cavity, a heating furnace, a working electrode, an outer shell, a temperature measuring element and a temperature control box; the inner cavity is arranged in the outer shell, and the counter electrode, the reference electrode and the working electrode are respectively connected into the inner cavity; the window component is arranged on the inner cavity and corresponds to the through hole on the outer shell; the heating furnace is arranged in the outer shell and contacts the outer part of the inner cavity, the heating wiring terminal is arranged on the heating furnace, the temperature measuring element is arranged on the inner cavity, and the heating wiring terminal and the temperature measuring element are both connected with the temperature control box. The heating electrochemical in-situ Raman spectrum pool can be combined with various spectrum instruments such as a Raman spectrometer to carry out in-situ characterization test through a window assembly, has the in-situ Raman spectrum test function of an electrochemical reaction process at high temperature, and is widely applied to the fields of chemistry, materials and related fields; the temperature regulation and monitoring functions are provided, the influence of temperature on the in-situ Raman spectrum characterization experiment of the object to be detected can be explored, the range of the existing electrochemical reaction system is greatly expanded, and the study thought of temperature factors in the electrochemical reaction process is provided for researchers.
Preferably, the heating electrochemical in-situ Raman spectrum pool further comprises a connecting pipe and a peristaltic pump, the inner cavity is provided with a liquid inlet and a liquid outlet, the liquid inlet and the liquid outlet are respectively connected with the electrochemical workstation through the connecting pipe, and the peristaltic pump is arranged on the connecting pipe. Electrolyte is introduced into and discharged from the liquid inlet and the liquid outlet to the inner cavity for electrochemical performance test, so that the electrolyte can circulate during the reaction.
Preferably, the outer shell comprises a lower shell and an upper cover, the inner cavity is arranged in the lower shell and is fixedly connected with the lower shell, and openings are formed in the tops of the lower shell and the inner cavity; the window assembly covers the top opening of the inner cavity; the upper cover is pressed on the window assembly and is fixedly connected to the top of the lower shell through screws, and a through hole is formed in the upper cover at a position corresponding to the window assembly; the working electrode is arranged in the inner cavity and is fixedly connected to the bottom of the inner cavity through a screw. The window component and the working electrode are convenient to detach, so that the window component and the working electrode are convenient to replace, sample loading and other operations are performed on the working electrode, and the window component with the optical lenses made of different materials is convenient to select according to different in-situ optical test requirements.
Preferably, a sealing ring is arranged between the window assembly and the inner cavity. The upper cover can enable the inner portion of the inner cavity to form a sealing environment by extruding the sealing ring through the window assembly, and the sealing performance is good.
Preferably, the counter electrode and the reference electrode both pass through the lower housing and are screwed on the inner cavity. The replacement is convenient.
Preferably, the heating furnace is formed by winding a resistance wire around the outer periphery of the inner cavity. The heat conduction can be directly carried out on the inner cavity, the occupied space is small, the heating module is integrated in the limited space, and the heating mode of the heating module around the periphery of the inner cavity also enables the heating temperature of the sample to be more uniform and accurate.
Preferably, the temperature measuring element adopts a Pt100 temperature sensor or a K-type thermocouple.
Preferably, the optical lens on the window assembly adopts CaF 2 Or a quartz material. CaF (CaF) 2 The optical lens made of the material can be used for infrared spectrum testing, and the optical lens made of quartz can be used for Raman spectrum characterization and optical imaging experiments.
Preferably, the inner cavity is made of polyether-ether-ketone. Has the performances of high mechanical strength, high temperature resistance, chemical corrosion resistance, good insulation and the like.
Preferably, the counter electrode is a platinum wire electrode, and the reference electrode is a silver chloride electrode.
The utility model has the advantages that:
1. the heating electrochemical in-situ Raman spectrum pool can be combined with various spectrum instruments such as a Raman spectrometer to carry out in-situ characterization test through a window assembly, has the in-situ Raman spectrum test function of an electrochemical reaction process at high temperature, and is widely applied to the fields of chemistry, materials and related fields; the temperature regulation and monitoring functions are provided, the influence of temperature on the in-situ Raman spectrum characterization experiment of the object to be detected can be explored, the range of the existing electrochemical reaction system is greatly expanded, and the study thought of temperature factors in the electrochemical reaction process is provided for researchers.
2. Electrolyte is introduced into and discharged from the liquid inlet and the liquid outlet to the inner cavity for electrochemical performance test, so that the electrolyte can circulate during the reaction.
3. The window component and the working electrode are convenient to detach in a mean square, so that sample loading and other operations can be conveniently carried out on the working electrode, and the window component with the optical lenses made of different materials can be conveniently selected according to different in-situ optical test requirements.
4. The heating furnace is formed by winding the resistance wire around the periphery of the inner cavity, can directly conduct heat to the inner cavity, occupies small space, realizes the integration of the heating module in a limited space, and also ensures that the heating temperature of the sample is more uniform and accurate in a heating mode around the periphery of the inner cavity.
Drawings
FIG. 1 is a schematic top view of a heating electrochemical in situ Raman spectroscopy cell according to an embodiment of the utility model.
FIG. 2 is a schematic cross-sectional view of a heating electrochemical in situ Raman spectroscopy cell according to an embodiment of the utility model.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions in the embodiments of the present utility model will be clearly and completely described below in conjunction with the embodiments of the present utility model, and it is apparent that the described embodiments are some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to fall within the scope of the utility model.
As shown in fig. 1 and 2, the embodiment of the utility model discloses a heating electrochemical in-situ raman spectroscopy cell, which comprises a window assembly 1, a counter electrode 2, a heating terminal 3, a reference electrode 4, an inner cavity 5, a heating furnace 6, a working electrode 7, an outer shell 8, a temperature measuring element (not shown), a temperature control box (not shown), a connecting pipe (not shown) and a peristaltic pump (not shown).
The inner cavity 5 is arranged inside the outer shell 8; the structure of the inner cavity 5 is designed into a complete three-electrode electrochemical reaction cell body, a counter electrode 2, a reference electrode 4 and a working electrode 7 are respectively connected into the inner cavity 5, the counter electrode 2 adopts a platinum wire electrode, and the reference electrode 4 adopts a silver chloride electrode; the inner cavity 5 is provided with a liquid inlet and a liquid outlet, the liquid inlet and the liquid outlet are respectively connected with an electrochemical workstation through connecting pipes, peristaltic pumps are arranged on the connecting pipes, electrolyte is introduced into and discharged from the inner cavity 5 through the liquid inlet and the liquid outlet for electrochemical performance test, and the circulating flow of the electrolyte can be realized when the reaction is carried out; the window assembly 1 is arranged on the inner cavity 5 and corresponds to the through hole on the outer shell 8, the condition of the working electrode 7 can be observed through the window assembly 1, and in-situ Raman characterization test can be carried out by combining various spectrum instruments such as a Raman spectrometer.
The heating furnace 6 is arranged in the outer shell 8 and contacts the outer part of the inner cavity 5, the heating binding post 3 is arranged on the heating furnace 6 and is connected with the temperature control box through a control wire, and the temperature measuring element is arranged on the inner cavity 5 and is in communication connection with the temperature control box; the temperature measuring element can monitor the temperature of the inner cavity 5 in real time and transmit the monitored data to the temperature control box in real time, and the temperature control box can accurately control the temperature of the heating furnace 6 according to the monitored data so as to realize the temperature regulation of the inner cavity 5; the temperature control range of the temperature control box is RT-100 ℃, and the control precision is 0.1 ℃; the temperature control box can be connected with a computer for testing to obtain a temperature control curve.
The heating furnace 6 is formed by winding a resistance wire around the periphery of the inner cavity 5, can directly conduct heat to the inner cavity 5, occupies small space, realizes the integration of a heating module in a limited space, and ensures that the heating temperature of a sample is more uniform and accurate by a heating mode of surrounding the periphery of the inner cavity 5; the temperature measuring element adopts a Pt100 temperature sensor or a K-type thermocouple.
The outer shell 8 comprises a lower shell and an upper cover, the inner cavity 5 is arranged in the lower shell and fixedly connected with the lower shell, and openings are formed in the tops of the lower shell and the inner cavity 5; the window component 1 covers the top opening of the inner cavity 5, and a sealing ring is arranged between the window component 1 and the inner cavity 5; the upper cover is pressed on the window assembly 1 and is fixedly connected to the top of the lower shell through screws, and a through hole is formed in the upper cover at a position corresponding to the window assembly 1; the working electrode 7 is arranged in the inner cavity 5 and is fixedly connected to the bottom of the inner cavity 5 through a screw; the counter electrode 2 and the reference electrode 4 pass through the lower shell and are connected with the inner cavity 5 in a threaded manner; the window assembly 1, the counter electrode 2, the reference electrode 4 and the working electrode 7 are convenient to disassemble, so that the operation of replacing, sample loading and the like on the working electrode 7 is convenient.
According to the different requirements of in-situ optical testing, the window assembly 1 with optical lenses made of different materials can be selected, for example, when infrared spectrum testing is performed, the optical lens on the window assembly 1 is CaF 2 The optical lens on the window assembly 1 is made of high-transmittance quartz material when carrying out Raman and optical imaging experiments.
The inner cavity 5 is made of polyether-ether-ketone (PEEK) material, and has the performances of high mechanical strength, high temperature resistance, chemical corrosion resistance, good insulation and the like; the internal volume of the inner cavity 5 can be designed according to the use requirement, so that the overall size of the heating electrochemical in-situ Raman spectrum cell is compact.
The application flow of the heating electrochemical in-situ Raman spectrum pool is as follows: the upper cover of the outer shell 8 is detached from the lower shell, the working electrode 7 is taken out from the top opening of the inner cavity 5 after being detached, and after the working electrode 7 is loaded with a sample, the sample is loaded into the inner cavity 5 and fixedly connected with the inner cavity 5; then, a sealing ring is filled, the window assembly 1 is placed at the position of the top opening of the inner cavity 5, the upper cover is pressed on the window assembly 1 and fixedly connected to the top of the lower shell through a screw, and the upper cover presses the sealing ring through the window assembly 1 under the action of the screw to enable the inner cavity 5 to form a sealing environment; the liquid inlet and the liquid outlet are respectively connected with an electrochemical workstation through connecting pipes, and electrolyte is circularly pumped by a peristaltic pump, so that the electrochemical performance test can be performed; the heating binding post 3 is connected with the temperature control box through a control line, so that the temperature regulation and monitoring functions of the electrochemical in-situ detection process can be realized, the research experiment of electrochemical performance at different temperatures is completed, and limited in-situ Raman characterization data are obtained by matching with a Raman spectrometer.
The above embodiments are only for illustrating the technical solution of the present utility model, and are not limiting; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present utility model.
Claims (10)
1. A heated electrochemical in situ raman spectroscopy cell, characterized by: the device comprises a window component, a counter electrode, a heating binding post, a reference electrode, an inner cavity, a heating furnace, a working electrode, an outer shell, a temperature measuring element and a temperature control box; the inner cavity is arranged in the outer shell, and the counter electrode, the reference electrode and the working electrode are respectively connected into the inner cavity; the window component is arranged on the inner cavity and corresponds to the through hole on the outer shell; the heating furnace is arranged inside the outer shell and contacts the outside of the inner cavity; the heating terminal is arranged on the heating furnace, the temperature measuring element is arranged on the inner cavity, and the heating terminal and the temperature measuring element are both connected with the temperature control box.
2. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the heating electrochemical in-situ Raman spectrum pool further comprises a connecting pipe and a peristaltic pump, the inner cavity is provided with a liquid inlet and a liquid outlet, the liquid inlet and the liquid outlet are respectively connected with an electrochemical workstation through the connecting pipe, and the peristaltic pump is arranged on the connecting pipe.
3. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the outer shell comprises a lower shell and an upper cover, the inner cavity is arranged in the lower shell and fixedly connected with the lower shell, and openings are formed in the tops of the lower shell and the inner cavity; the window assembly covers the top opening of the inner cavity; the upper cover is pressed on the window assembly and is fixedly connected to the top of the lower shell through screws, and a through hole is formed in the upper cover at a position corresponding to the window assembly; the working electrode is arranged in the inner cavity and is fixedly connected to the bottom of the inner cavity through a screw.
4. A heated electrochemical in situ raman spectroscopy cell according to claim 3, wherein: and a sealing ring is arranged between the window assembly and the inner cavity.
5. A heated electrochemical in situ raman spectroscopy cell according to claim 3, wherein: the counter electrode and the reference electrode pass through the lower shell and are connected to the inner cavity in a threaded manner.
6. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the heating furnace is formed by winding a resistance wire around the periphery of the inner cavity.
7. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the temperature measuring element adopts a Pt100 temperature sensor or a K-type thermocouple.
8. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the optical lens on the window component adopts CaF 2 Or a quartz material.
9. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the inner cavity is made of polyether-ether-ketone.
10. A heated electrochemical in situ raman spectroscopy cell according to claim 1, wherein: the counter electrode adopts a platinum wire electrode, and the reference electrode adopts a silver chloride electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321366980.8U CN220154260U (en) | 2023-05-31 | 2023-05-31 | Heating electrochemical in-situ Raman spectrum pool |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321366980.8U CN220154260U (en) | 2023-05-31 | 2023-05-31 | Heating electrochemical in-situ Raman spectrum pool |
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| Publication Number | Publication Date |
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| CN220154260U true CN220154260U (en) | 2023-12-08 |
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| CN202321366980.8U Active CN220154260U (en) | 2023-05-31 | 2023-05-31 | Heating electrochemical in-situ Raman spectrum pool |
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| Country | Link |
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2023
- 2023-05-31 CN CN202321366980.8U patent/CN220154260U/en active Active
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