CN114660145A - Rotary disk electrode device - Google Patents
Rotary disk electrode device Download PDFInfo
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- CN114660145A CN114660145A CN202210288421.3A CN202210288421A CN114660145A CN 114660145 A CN114660145 A CN 114660145A CN 202210288421 A CN202210288421 A CN 202210288421A CN 114660145 A CN114660145 A CN 114660145A
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- electrode assembly
- disk electrode
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- 239000007788 liquid Substances 0.000 claims abstract description 47
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 3
- 229920002530 polyetherether ketone Polymers 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 33
- 238000001069 Raman spectroscopy Methods 0.000 abstract description 10
- 238000012512 characterization method Methods 0.000 abstract description 9
- 238000009792 diffusion process Methods 0.000 abstract description 8
- 238000001819 mass spectrum Methods 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 6
- 230000005518 electrochemistry Effects 0.000 abstract 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- -1 potassium ferricyanide Chemical compound 0.000 description 2
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The utility model belongs to the technical field of electrochemistry electrode test equipment, a rotating disc electrode device is disclosed, including the last casing and the lower casing of detachable connection, form the cavity between the two, it is provided with inlet and liquid outlet to go up the casing, just the side of going up the casing is provided with the reference electrode, the casing is provided with the first mass flow body that is used for conducting disk electrode down, is used for conducting the second mass flow body of ring electrode and is used for conducting the third mass flow body of counter electrode, still includes externally utilize the pipeline set up in the inlet with peristaltic pump between the liquid outlet for driving liquid is in flow between the cavity. The rotary disc electrode device can reduce the thickness of a diffusion layer, improves the test stability, has larger working electrode area, can perform more subsequent characterizations, overcomes the defect that a certain species cannot be visually characterized by matching Raman, mass spectrum and liquid chromatogram, and improves the accuracy of a test result.
Description
Technical Field
The invention belongs to the technical field of electrochemical electrode testing equipment, and particularly relates to a rotary disk electrode device.
Background
In the field of electrochemical analysis, a rotating disk electrode is a common testing tool, and can effectively eliminate the influence of mass transfer and reduce the thickness of a diffusion layer by rotating at a certain angular speed in a solution, and particularly in an oxygen reduction test, the rotating disk electrode is required to be combined with a Koutecky-Levich equation to obtain the electron transfer number. However, the existing rotating disk electrode is easy to generate vortex in the rotating process, especially bubbles are generated on the surface of the electrode at a high rotating speed, and meanwhile, oxygen is simultaneously introduced into an electrolytic cell in an oxygen reduction test, so that a large amount of bubbles are generated, the active area of the surface of the electrode is reduced, and the accuracy of the test result is influenced; on the other hand, modern scientific research test instruments are continuously combined with each other in a cross mode so as to improve the accuracy of the test, for example: the mutual combination of the SEM-TOFSIMS characterization instruments can not only make up the defect that the SEM cannot deeply analyze element analysis, but also improve the accuracy of etching species of the TOFSIMS, but the existing rotating disk electrode cannot be combined with other instruments for characterization.
Disclosure of Invention
In order to solve the problems, the invention provides a rotary disk electrode device which can reduce the thickness of a diffusion layer and improve the test stability, has larger working electrode area, can perform more subsequent characterizations, overcomes the defect that a certain species cannot be visually characterized by matching Raman, mass spectrum and liquid chromatogram, and improves the accuracy of a test result.
The invention provides a rotary disc electrode device which comprises an upper shell and a lower shell which are detachably connected, wherein a cavity is formed between the upper shell and the lower shell, the upper shell is provided with a liquid inlet and a liquid outlet, the side surface of the upper shell is provided with a reference electrode, the lower shell is provided with a first current collector for conducting a disc electrode, a second current collector for conducting a ring electrode and a third current collector for conducting a counter electrode, and the rotary disc electrode device further comprises a peristaltic pump which is arranged between the liquid inlet and the liquid outlet by using a pipeline outside and is used for driving liquid to flow between the cavities.
Preferably, in the above-described rotating disk electrode assembly, the upper case is detachably connected to the lower case by a first fixing screw provided on the upper case.
Preferably, in the above-described rotary disk electrode device, the upper casing and the lower casing are both polyetheretherketone casings.
Preferably, in the above-described rotating disc electrode assembly, the upper case is a quartz glass case.
Preferably, in the above rotating disk electrode device, the reference electrode is fixed on a side surface of the upper housing by using a second fixing screw and a first groove which are formed.
Preferably, in the above-mentioned rotating disk electrode device, the number of the liquid inlet and the liquid outlet is at least four.
Preferably, in the above-mentioned rotating disc electrode device, the liquid inlet and the liquid outlet are connected through a second groove inside the cavity.
Preferably, in the above-mentioned rotating disk electrode device, the bottom of the first current collector is provided with a third groove having a thread.
Preferably, in the above-described rotating disk electrode assembly, the bottom of the second current collector is provided with a fourth groove.
As can be seen from the above description, the above-mentioned rotating disk electrode device provided by the present invention includes the upper housing and the lower housing detachably connected, a cavity is formed between the upper housing and the lower housing, the upper housing is provided with the liquid inlet and the liquid outlet, and the side of the upper housing is provided with the reference electrode, the lower housing is provided with the first current collector for conducting the disk electrode, the second current collector for conducting the ring electrode, and the third current collector for conducting the counter electrode, and further includes the peristaltic pump externally disposed between the liquid inlet and the liquid outlet by using a pipeline for driving the liquid to flow between the cavities, so that the electrode in the device does not need to move, but allows the liquid to flow, thereby reducing the thickness of the diffusion layer, improving the test stability, and the working electrode area is larger, facilitating the replacement of the electrode and the replacement of the housing according to the actual needs, therefore, more subsequent characterizations can be carried out, the defect that a certain species cannot be visually characterized is overcome by matching Raman, mass spectrum and liquid chromatogram, and the accuracy of the test result is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a top view of an upper housing of an embodiment of a rotating disc electrode assembly according to the present invention;
FIG. 2 is a side view of an upper housing of an embodiment of a rotating disc electrode assembly provided by the present invention;
FIG. 3 is a top view of a lower housing of an embodiment of a rotating disc electrode assembly according to the present invention;
FIG. 4 is a side view of the lower housing of one embodiment of a rotary disk electrode assembly provided in accordance with the present invention;
FIG. 5 is a schematic diagram of the ultimate steady state current density for testing different flow rates of 1mM potassium ferricyanide and 1M potassium chloride solutions;
fig. 6 is a schematic diagram comparing the limit steady-state current density of the test of the rotating disk electrode device provided in this embodiment with that of the prior art device.
Detailed Description
The core of the invention is to provide a rotating disc electrode device, which can reduce the thickness of a diffusion layer and improve the test stability, has larger working electrode area, can perform more subsequent characterizations, overcomes the defect that a certain species cannot be intuitively characterized by matching Raman, mass spectrum and liquid chromatogram, and improves the accuracy of the test result.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1, fig. 2, fig. 3 and fig. 4 show an embodiment of a rotating disk electrode device provided by the present invention, fig. 1 is a top view of an upper housing of an embodiment of a rotating disk electrode device provided by the present invention, fig. 2 is a side view of an upper housing of an embodiment of a rotating disk electrode device provided by the present invention, fig. 3 is a top view of a lower housing of an embodiment of a rotating disk electrode device provided by the present invention, fig. 4 is a side view of a lower housing of an embodiment of a rotating disk electrode device provided by the present invention, the device comprises an upper housing 1 and a lower housing 2 detachably connected, a cavity is formed between the upper housing 1 and the lower housing, the upper housing 1 is provided with a liquid inlet 101 and a liquid outlet 102, the number of the liquid inlet and the liquid outlet can be but not limited to 4, which can be set according to the actual housing size, of course, the number of the liquid inlet and the liquid outlet is as large as the size allows, and a reference electrode (not shown in fig. 1) is disposed on a side surface of the upper housing 1, the lower housing 2 is provided with a first current collector 201 for conducting a disk electrode, a second current collector 202 for conducting a ring electrode, and a third current collector 203 for conducting a counter electrode, and further comprises a peristaltic pump (not shown in the figure) externally disposed between the liquid inlet 101 and the liquid outlet 102 by using a pipeline, for driving liquid to flow between the cavities.
It should be noted that, when the embodiment of the above-mentioned rotating disk electrode device is used for testing, it is not necessary to rotate each electrode, but only the peristaltic pump is used to drive the liquid in the cavity to flow, so as to achieve the purpose of reducing the thickness of the diffusion layer. In addition, the area of a disc electrode in the device is larger, so that mass spectrum and gas chromatography tests can be matched subsequently, and a rotating disc electrode in the prior art is small in size and less in sediment on the surface of the electrode, so that the rotating disc electrode is difficult to be matched with mass spectrum and gas chromatography and other instruments for use.
The upper shell 1 in the device can be preferably a quartz glass shell, the quartz material can ensure that no Raman peak exists during Raman testing, so that the test result cannot be interfered, and in this case, the device can be combined with Raman to perform in-situ testing, thereby greatly expanding the range of testable items.
As can be seen from the above description, in the embodiment of the above-mentioned rotating disk electrode device provided by the present invention, since the rotating disk electrode device includes the upper housing and the lower housing detachably connected, a cavity is formed between the upper housing and the lower housing, the upper housing is provided with the liquid inlet and the liquid outlet, and the side of the upper housing is provided with the reference electrode, the lower housing is provided with the first current collector for conducting the disk electrode, the second current collector for conducting the ring electrode, and the third current collector for conducting the counter electrode, and further includes the peristaltic pump externally disposed between the liquid inlet and the liquid outlet by using a pipeline, for driving the liquid to flow between the cavities, it can be seen that the electrode in the device does not need to move, but lets the liquid flow, thereby the thickness of the diffusion layer can be reduced, the test stability is improved, the working electrode area is larger, the electrode replacement and the housing replacement can be conveniently performed according to actual needs, thereby more subsequent characterizations can be performed, by matching with Raman, mass spectrum and liquid chromatogram, the defect that a certain species cannot be directly represented is overcome, and the accuracy of the test result is improved.
In one embodiment of the above-mentioned rotating disk electrode device, with reference to fig. 1, the upper casing 1 can be detachably connected to the lower casing 2 by using the first fixing screw 104 disposed thereon, the number of the first fixing screw 104 can be selected according to actual requirements, and is not limited herein, and the hole formed on the lower casing 2 also needs to correspond to the position of the first fixing screw 104, so as to ensure that the upper and lower casings are firmly fixed together, so that the overall stability is good enough, and when the casings made of different materials need to be replaced, the casings can be easily detached for replacement. Moreover, both the upper shell 1 and the lower shell 2 may be preferably polyetheretherketone shells, which are corrosion resistant, especially in organic systems, and have high mechanical strength and are not easy to deform.
In another embodiment of the above-mentioned rotating disk electrode assembly, with continued reference to fig. 1 and 2, the side surface of the upper housing 1 can be fixed with a reference electrode by using the second fixing screw 103 and the first groove 105, the reference electrode is used for calibrating the potential in the electrochemical test of the battery, and the connection mode also facilitates the installation and the removal of the reference electrode, further improving the convenience of the test.
In the above-mentioned rotating disk electrode device, with continued reference to fig. 2, the liquid inlet 101 and the liquid outlet 102 may be connected, but not limited to, by the second groove 106 inside the cavity, so as to ensure that no turbulence is generated when the liquid flows.
In one preferred embodiment of the above-described rotating disk electrode assembly, with continued reference to fig. 4, the bottom of the first current collector 201 may be provided with a third recess 204 having threads. Moreover, the bottom of the third current collector 203 may also be provided with a third groove 204 having a thread, and in addition, the bottom of the second current collector 202 may also be provided with a fourth groove 205. It should be noted that, these grooves have screw threads, which can play a role in fixing and conducting the current collector.
In addition, with continued reference to fig. 3 and 4, insulators 206 may also be preferably disposed between the first current collector 201 and the second current collector 202, and between the second current collector 202 and the third current collector 203, to better avoid the disk electrode, the ring electrode, and the counter electrode from contacting each other.
Before the rotating disc electrode device provided by the embodiment is used for testing, a disc electrode (working electrode) and a counter electrode are respectively fixed on a first current collector and a third current collector, and an AgCl/Ag reference electrode is fixed at a second fixed screw. The liquid outlet of the peristaltic pump is communicated with the liquid inlet of the rotary disc electrode device, the peristaltic pump is opened during testing, the pump speed is adjusted, and the third groove with threads is respectively connected with a disc electrode (working electrode) and a counter electrode of the electrochemical workstation.
The results obtained by adjusting the pump speed are shown in fig. 5, fig. 5 is a graph showing the ultimate steady state current densities for different flow rates of 1mM potassium ferricyanide and 1M potassium chloride solutions. Wherein A, B, C, D, E, F, G and H correspond to pump speeds of 10mL/min, 20mL/min, 30mL/min, 40mL/min, 50mL/min, 100mL/min, 200mL/min, and 400mL/min, respectively. With the increase of the flow velocity, the thickness of the diffusion layer on the surface of the electrode is continuously reduced, and a comparison of current density with the prior art is obtained by combining formulas (a) and (b) as shown in fig. 6, fig. 6 is a schematic diagram for comparing the limit steady-state current density of the test of the rotating disk electrode device provided by the embodiment with the prior art, wherein a line formed by connecting five stars is a theoretical value obtained by the test of the prior art, and a square represents an actual test value obtained by using the device provided by the embodiment.
i＝nFA(D0/δ0)C0 (b)
After the electrochemical reaction by using the working electrode with large area, the subsequent characterization, such as mass spectrum, gas chromatography and the like, can be carried out. In addition, for the test of in-situ raman characterization, the upper shell needs to be replaced by quartz glass to meet the requirements of raman test, and the device provided by the embodiment is more convenient for replacing the shell.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The utility model provides a rotatory disc electrode assembly, its characterized in that, includes the last casing and the lower casing of detachable connection, forms the cavity between the two, it is provided with inlet and liquid outlet to go up the casing, just the side of going up the casing is provided with the reference electrode, the casing is provided with the first mass flow body that is used for switching on the disc electrode down, is used for switching on the second mass flow body of ring electrode and is used for switching on the third mass flow body of counter electrode, still includes externally utilize the pipeline set up in the inlet with peristaltic pump between the liquid outlet for drive liquid is in flow between the cavity.
2. The rotary disc electrode assembly of claim 1, wherein the upper housing is removably connected to the lower housing by a first retaining screw disposed thereon.
3. The rotating disk electrode assembly of claim 1 wherein the upper housing and the lower housing are both polyetheretherketone housings.
4. The rotating disk electrode assembly of claim 1 wherein the upper housing is a quartz glass housing.
5. The rotating disk electrode assembly as set forth in claim 1, wherein said reference electrode is fixed to a side surface of said upper housing by means of a second fixing screw and a first groove.
6. The rotary disk electrode assembly as defined in claim 1 wherein each of said inlet ports and said outlet ports is at least four in number.
7. The rotating disk electrode assembly as defined in claim 1, wherein said inlet port and said outlet port are connected by a second groove inside said cavity.
8. The rotating disk electrode assembly as claimed in claim 1, wherein the bottom of the first current collector is provided with a third recess having threads.
9. The rotating disk electrode assembly of claim 1 wherein the bottom of the second current collector is provided with a fourth recess.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210288421.3A CN114660145A (en) | 2022-03-23 | 2022-03-23 | Rotary disk electrode device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210288421.3A CN114660145A (en) | 2022-03-23 | 2022-03-23 | Rotary disk electrode device |
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| CN114660145A true CN114660145A (en) | 2022-06-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210288421.3A Pending CN114660145A (en) | 2022-03-23 | 2022-03-23 | Rotary disk electrode device |
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Application publication date: 20220624 |