CN115078483B - Electrochemical reactor for microscope observation - Google Patents
Electrochemical reactor for microscope observation Download PDFInfo
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- CN115078483B CN115078483B CN202210730251.XA CN202210730251A CN115078483B CN 115078483 B CN115078483 B CN 115078483B CN 202210730251 A CN202210730251 A CN 202210730251A CN 115078483 B CN115078483 B CN 115078483B
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- microscope
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- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 13
- 239000011521 glass Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 7
- 238000003487 electrochemical reaction Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000007850 fluorescent dye Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006059 cover glass Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- DSLLHVISNOIYHR-UHFFFAOYSA-M ethyl 2-(6-methoxyquinolin-1-ium-1-yl)acetate;bromide Chemical compound [Br-].COC1=CC=C2[N+](CC(=O)OCC)=CC=CC2=C1 DSLLHVISNOIYHR-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- DPGAAOUOSQHIJH-UHFFFAOYSA-N ruthenium titanium Chemical compound [Ti].[Ru] DPGAAOUOSQHIJH-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000007794 visualization technique Methods 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The application discloses an electrochemical reactor for microscopic observation, comprising: the device comprises a container, an electrode to be observed and a counter electrode; the electrode to be observed is a lamellar electrode, and the electrode to be observed is placed in the container in the following manner: and the placement mode of the electrode to be observed in the container with the smallest vertical projection area. The reactor provided by the application can realize in-situ observation of electrode surface ions with spatial resolution of 0.104 mu m and time resolution of 0.47 s.
Description
Technical Field
The present disclosure relates to, but is not limited to, the field of electrochemical technology, to, but is not limited to, an electrochemical reactor for microscopic observation, and in particular, but not limited to, a method for in situ observation of dynamic changes in ion concentration at the electrode surface by a confocal microscope.
Background
At the electrode interface where the electrochemical reaction occurs, the electrolyte on the electrode surface may exhibit a completely different local microenvironment from the bulk electrolyte under the influence of factors such as generation/consumption, diffusion, electromigration, and convection of the reactive ions. The local microenvironment directly determines the activity and selectivity of the electrochemical reaction, so understanding the local microenvironment of the solid-liquid interface is key to understanding the heterogeneous catalytic mechanism.
In order to understand the nature of the local microenvironment, it is necessary to visualize the ion concentration of the microenvironment near the electrode during the reaction. However, the ion concentration in the microenvironment is dynamically changed and is below the mesoscale, so that it is difficult to measure by means of sampling points and the like. Therefore, it is important to develop an in-situ observation means for ion concentration that is easy to operate and traceable. And the closer the solution to the electrode surface, the more favorable it is to reveal the electrochemical catalytic mechanism, the more capable of determining the nature of the electrochemical reaction. Therefore, in addition to easy operation and traceability, higher requirements on the observation precision are required.
Disclosure of Invention
The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the claims.
The application provides a method for in-situ observation of dynamic change of ion concentration on the surface of an electrode by a confocal microscope.
The present application provides an electrochemical reactor for microscopic observation, comprising:
the device comprises a container, an electrode to be observed and a counter electrode;
the electrode to be observed is a lamellar electrode, and the placement mode of the electrode to be observed in the container is as follows: the direction perpendicular to the placement mode with the smallest perpendicular projection area of the electrode to be observed in the container and the direction observed by the microscope can be the same direction.
In one electrochemical reactor provided by the present application, the electrochemical reactor further comprises,
the electrode clamping groove to be observed is used for positioning the electrode to be observed;
and the electrode bolt to be observed is used for fixing the electrode to be observed and supplying power to the electrode to be observed.
In the electrochemical reactor provided by the application, the thickness of the electrode to be observed is 0.01mm to 0.1mm.
In one electrochemical reactor provided by the application, the thickness of the container is 0.1mm to 1mm;
the thickness of the container is the thickness of the container between the microscope and the electrode to be observed.
In one electrochemical reactor provided by the present application, the electrochemical reactor further comprises,
the counter electrode clamping groove is used for positioning the counter electrode;
and a counter electrode bolt for fixing the counter electrode and supplying power to the counter electrode.
In one electrochemical reactor provided by the present application, the electrochemical reactor further comprises,
a reference electrode,
a reference electrode clamping groove for positioning the reference electrode;
and the reference electrode bolt is used for fixing the reference electrode and supplying power to the reference electrode.
In the electrochemical reactor provided by the application, the objective lens used by the microscope is any one or more of a 40x objective lens and an objective lens with magnification less than 40 x.
In yet another aspect, the present application provides the use of the above-described electrochemical reactor for microscopic observation, for in situ real-time observation of dynamic changes in ion concentration at the electrode surface.
In the application of the electrochemical reactor provided by the application in microscopic observation, the microscope uses any one or more of a 40x objective lens and an objective lens with magnification less than 40 x.
In the application of the electrochemical reactor in microscope observation, the objective lens of the microscope is tightly attached to the electrochemical reactor, and the electrochemical reactor is tightly attached to the electrode to be observed, so that the microscope can better observe the electrode to be observed.
In the application of the electrochemical reactor in microscopic observation, the in-situ dynamic observation of the ion concentration of the electrode micro-interface is realized through the reactor matched with the inverted confocal laser scanning microscope.
The application has the beneficial effects that:
the application provides a method for in-situ observation of dynamic change of ion concentration on the surface of an electrode by a confocal microscope, belonging to the field of electrochemistry. The ion concentration change of the micro-environment on the surface of the electrode plays an important role in understanding the electrode reaction, but no method for simply and conveniently observing the ion concentration change on the surface of the electrode exists at present. The implementation method of the application comprises the following steps: the in-situ observation of the ions on the electrode surface with spatial resolution of 0.104 μm and temporal resolution of 0.47s can be achieved by adding a fluorescent probe corresponding to the ions to be observed to the electrolyte and installing the reactor in an inverted confocal laser scanning microscope (as shown in fig. 6). By changing different fluorescent probes, the dynamic change of different ion concentrations on the electrode surface can be comprehensively known. The visualization method can be used as a bridge for connecting mesochemistry and industrial scale chemical engineering.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application. Other advantages of the application may be realized and attained by the structure particularly pointed out in the written description.
Drawings
The accompanying drawings are included to provide an understanding of the principles of the application, and are incorporated in and constitute a part of this specification, illustrate and, together with the description, serve to explain, without limitation, the principles of the application.
FIG. 1 is a schematic front view of a reactor used in an embodiment of the present application;
FIG. 2 is a schematic top view of a reactor used in an embodiment of the present application;
FIG. 3 is a schematic side view of a reactor used in an embodiment of the present application;
reference numerals: 1. an electrode to be observed; 2. a counter electrode; 3. a reference electrode; 4. a housing; 5. a glass bottom culture dish; 6. an electrode bolt to be observed; 7. a counter electrode bolt; 8. a reference electrode bolt.
FIG. 4 is a graph showing the control of chloride concentration and fluorescence intensity in the examples;
FIG. 5 is a graph of fluorescence taken at various times in the examples;
FIG. 6 is a schematic diagram of an inverted confocal laser scanning microscope, an electrochemical reactor for inverted microscopic observation, and an electrode to be observed in an embodiment;
FIG. 7 is a three-dimensional schematic of a reactor used in an embodiment of the present application.
Detailed Description
The following describes embodiments of the present application in detail for the purpose of making the objects, technical solutions and advantages of the present application more apparent. It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be arbitrarily combined with each other.
In an embodiment of the present application, there is provided an electrochemical reactor for microscopic observation, the electrochemical reactor comprising:
a container (housing 4 of a petri dish 5), an electrode to be observed 1 (anode, titanium ruthenium electrode) versus electrode 2 (cathode, titanium electrode) and a reference electrode 3 (silver wire).
Illustratively, the glass bottom culture dish 5 may be a glass bottom culture dish (model 802001) with a diameter of 20mm manufactured by tin-free resistant life technologies, inc.
Illustratively, the materials of the electrode to be observed 1, the counter electrode 2 and the reference electrode 3 may be determined to be suitable according to the experimental requirements.
Illustratively, the microscope is a confocal laser scanning microscope (Zeiss LSM980 Airyscan 2), and the matched objective lens is a Objective LD LCI Plan-Apochromat 40x/1.2Imm autocorr DIC M27 type objective lens.
As shown in fig. 1 to 3 and fig. 7, the electrode to be observed 1 is a sheet-like electrode, and the electrode to be observed 1 is placed in the container in the following manner: and the placement mode of the electrode to be observed with the smallest vertical projection area in the container is that the vertical direction is parallel to the direction of microscope observation.
Illustratively, the thickness of the container between the microscope and the electrode 1 to be observed may be 0.1mm to 1mm.
As shown in fig. 1 to 3 and 7, the housing 4 is used for fixing the cathode, the anode, the reference electrode, and connection studs and connection wires thereof.
Illustratively, as shown in fig. 1 to 3 and 7, a channel which is matched with the glass bottom culture dish 5 is arranged below the side wall of the shell 4, and the shell can be directly fixed on the glass bottom culture dish 5 through the channel (the side wall of the glass bottom culture dish 5 is inserted into the channel).
The material of the housing 4 may be methyl methacrylate, for example.
Illustratively, it is also possible to directly prepare a glass bottom culture dish (vessel) comprising said channels without using the housing 4.
As shown in fig. 1 to 3 and fig. 7, the housing 4 further includes an electrode clamping groove to be observed, for positioning the electrode to be observed; the electrode bolt 6 to be observed is used for fixing the electrode 1 to be observed and supplying power to the electrode to be observed; a counter electrode clamping groove for positioning the counter electrode 2; a counter electrode bolt 7 for fixing the counter electrode 2 and supplying power to the counter electrode; a reference electrode clamping groove for positioning the reference electrode 3; a reference electrode bolt 8 for fixing the reference electrode 3 and supplying power to the reference electrode.
For example, the electrode clamping groove to be observed, the electrode bolt to be observed 6, the counter electrode clamping groove, the counter electrode bolt 7, the reference electrode clamping groove and the reference electrode bolt 8 can also be directly arranged in the glass bottom culture dish 5 (container).
Illustratively, as shown in fig. 1 to 3 and 7, the middle of the side wall of the housing 4 is provided with three holes for engaging with bolts.
The bolt can be used, for example, both to fix the electrode and as an electrically conductive terminal. The bolt may be copper.
Illustratively, the electrode surface chloride ion distribution is measured (example 1):
as shown in fig. 6, the confocal laser scanning microscope was inverted, and the electrochemical reactor for observation by the inverted microscope and the electrode to be observed were assembled well. The anode adopts a titanium ruthenium electrode, the cathode adopts a titanium electrode, the length of the cathode and the anode is 15mm, the width of the cathode and the anode is 10mm, the thickness of the cathode and the anode is 0.1mm (the thickness of a container between the microscope and the electrode to be observed is 0.17 mm), the reference electrode adopts silver wires, the diameter of the reference electrode is 1mm, the length of the reference electrode is 7mm (the length can also be 5mm to 9 mm), and the electrolyte contains 80mmol/L sodium chloride and 10mmol/L MQAE (N- (ethoxycarbonyl) methyl) -6-methoxyquinolinium bromide and chloride ion fluorescent probe). The constant current method is adopted to provide power, and the current density is 4mA/cm 2 . The model of the objective lens is Objective LD LCI Plan-Apochromat 40x/1.2Imm autocorr DIC M27, the shooting resolution is 512 x 512, the shooting interval is 0.47s, the excitation wavelength is 401nm, the absorption wavelength is 422nm, and the detection is carried outThe wavelength is 411-553nm. FIG. 4 is a graph of chloride concentration versus fluorescence intensity. Fig. 5 is a fluorescent image taken at different times, with the black lower portion being the non-fluorescing electrode and the gray upper portion being the solution containing the fluorescent dye. From the fluorescence signal of the solution, the chloride ion concentration of the solution can be deduced. At 0s, the chloride ion concentration is 80mmol/L; at 10s, the concentration of chloride ions is reduced to 39.3mmol/L because of participation in electrode interface reaction; the chloride ion concentration continues to drop to 20.6mmol/L at 20 s; at 40s, the chloride concentration did not change much from 20s, indicating that the interfacial chloride concentration had approached steady state. The application quantitatively observes the change of the chloride ion concentration on the surface of the electrode by using a 40x objective lens in real time.
The working distance using a 40x objective lens was 0.58mm, with 0.41mm remaining after subtracting the 0.17mm glass bottom thickness. Such a small working distance cannot be achieved in the prior art. The smaller the working distance, the less the solution is at the interval between the objective lens and the observed object, which is beneficial to reducing the interference of the solution to the incident light, and obtaining higher quality images.
Comparative example
As in the prior art documents: fuladdanjeh-Hojaghan B, elsutohy M, V Kabanov, et al, in-Operando Mapping of pH Distribution in Electrochemical Processes [ J ]. Angewandte Chemie International Edition,2019,58 (47) the objective lens used was 10x (HC PL APO CS2 10x/0.40 dry).
As can be seen from fig. 1 (b) of the prior art (prior art objective system), the objective lens photographs the obliquely placed electrode through the side, which is at a distance from the cover glass, whereas the 40x objective lens used in example 1 of the present application has a working distance of 0.58mm, such a side placement cannot guarantee a working distance of 0.58 mm.
As can be seen from fig. 3, 4 and 5 (observation effect diagrams) of the present application, the electrode is vertically placed above the glass bottom, the bottom of the electrode is tightly combined with the cover glass by self gravity, and the distance between the electrode and the objective lens is reduced.
The spatial resolution of comparative example 1 was only 1.13 μm×1.13 μm; the spatial resolution of example 1 can reach 0.104 μm×0.104 μm, and the spatial resolution is increased by 10 times, so that the change of local microenvironment on the surface of the electrode can be observed more advantageously. The closer to the local microenvironment of the electrode surface, the greater the reaction impact on the electrode surface. Taking the chloride ion in example 1 as an example, the concentration of the chloride ion in a range closer to the electrode can be seen by means of a 40X objective lens, and the interference of a solution medium can be reduced, so that a higher-resolution image is obtained, and microscopic data is provided for the dynamics of the de-electrochemical reaction.
Claims (1)
1. An application of an electrochemical reactor in confocal microscope observation, wherein the electrochemical reactor is used for in-situ real-time observation of dynamic change of ion concentration on the surface of an electrode;
the electrochemical reactor includes: the device comprises a container, an electrode to be observed and a counter electrode;
the electrode to be observed is a lamellar electrode, and the electrode to be observed is placed in the container in the following manner: the placement mode of the electrode to be observed with the smallest vertical projection area in the container;
the electrode clamping groove to be observed is used for positioning the electrode to be observed;
the electrode bolt to be observed is used for fixing the electrode to be observed and supplying power to the electrode to be observed;
the counter electrode clamping groove is used for positioning the counter electrode;
a counter electrode bolt for fixing and supplying power to the counter electrode;
a reference electrode,
a reference electrode clamping groove for positioning the reference electrode;
a reference electrode bolt for fixing the reference electrode and supplying power to the reference electrode;
the thickness of the electrode to be observed is 0.01mm to 0.1mm;
the thickness of the container is 0.1mm to 1mm;
the thickness of the container is the thickness of the container between the microscope and the electrode to be observed;
the microscope uses any one or more of a 40x objective lens and an objective lens with magnification less than 40 x;
the objective lens of the microscope is tightly attached to the electrochemical reactor, and the electrochemical reactor is tightly attached to the electrode to be observed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210730251.XA CN115078483B (en) | 2022-06-24 | 2022-06-24 | Electrochemical reactor for microscope observation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210730251.XA CN115078483B (en) | 2022-06-24 | 2022-06-24 | Electrochemical reactor for microscope observation |
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| Publication Number | Publication Date |
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| CN115078483A CN115078483A (en) | 2022-09-20 |
| CN115078483B true CN115078483B (en) | 2023-10-31 |
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Citations (7)
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| CN107039694A (en) * | 2017-06-08 | 2017-08-11 | 合肥国轩高科动力能源有限公司 | Device and method for observing electrochemical reaction process of lithium ion battery pole piece |
| CN113189157A (en) * | 2021-04-09 | 2021-07-30 | 北京科技大学 | Electrochemical reaction tank device suitable for scanning probe microscope |
| JP2021161468A (en) * | 2020-03-31 | 2021-10-11 | 国立大学法人横浜国立大学 | Electrochemical unit cell |
| CN113533787A (en) * | 2021-06-23 | 2021-10-22 | 浙江大学 | Electrochemical reaction process in-situ monitoring device based on atomic force microscope and monitoring method thereof |
| CN214503439U (en) * | 2020-11-30 | 2021-10-26 | 北京中研环科科技有限公司 | Electrochemical in-situ microscopic testing device under stress action |
| CN215917463U (en) * | 2021-02-01 | 2022-03-01 | 北京诺植科技有限公司 | Electrode holder and electrochemical reaction cell device |
| CN114384142A (en) * | 2022-01-18 | 2022-04-22 | 西北工业大学 | In-situ multi-field analysis testing device, method and application of chip-based micro electrochemical cell |
-
2022
- 2022-06-24 CN CN202210730251.XA patent/CN115078483B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107039694A (en) * | 2017-06-08 | 2017-08-11 | 合肥国轩高科动力能源有限公司 | Device and method for observing electrochemical reaction process of lithium ion battery pole piece |
| JP2021161468A (en) * | 2020-03-31 | 2021-10-11 | 国立大学法人横浜国立大学 | Electrochemical unit cell |
| CN214503439U (en) * | 2020-11-30 | 2021-10-26 | 北京中研环科科技有限公司 | Electrochemical in-situ microscopic testing device under stress action |
| CN215917463U (en) * | 2021-02-01 | 2022-03-01 | 北京诺植科技有限公司 | Electrode holder and electrochemical reaction cell device |
| CN113189157A (en) * | 2021-04-09 | 2021-07-30 | 北京科技大学 | Electrochemical reaction tank device suitable for scanning probe microscope |
| CN113533787A (en) * | 2021-06-23 | 2021-10-22 | 浙江大学 | Electrochemical reaction process in-situ monitoring device based on atomic force microscope and monitoring method thereof |
| CN114384142A (en) * | 2022-01-18 | 2022-04-22 | 西北工业大学 | In-situ multi-field analysis testing device, method and application of chip-based micro electrochemical cell |
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