CN115219573A - Porous electrode and preparation method thereof - Google Patents
Porous electrode and preparation method thereof Download PDFInfo
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- CN115219573A CN115219573A CN202210837819.8A CN202210837819A CN115219573A CN 115219573 A CN115219573 A CN 115219573A CN 202210837819 A CN202210837819 A CN 202210837819A CN 115219573 A CN115219573 A CN 115219573A
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Abstract
The application discloses porous electrode, including silver post, silver chloride powder end layer and electrically conductive porous component, the surface of electrically conductive porous component sets up cylindrical counter bore, silver chloride powder end layer sets up the bottom of cylindrical counter bore, with electrically conductive porous component connects, the silver post sets up in the cylindrical counter bore, the silver post with the silver chloride powder end layer is connected, the silver post with electrically conductive porous component connects. The application also provides a method for preparing the porous electrode.
Description
Technical Field
The application relates to the field of electrochemical sensors, in particular to a porous electrode and a preparation method thereof.
Background
In the novel fields of ocean exploration, biosensing, intelligent detection and the like, the electrochemical sensor is widely applied. The porous electrode is a most popular reference electrode or signal acquisition electrode in various electrochemical sensors because of the advantages of small electrode impedance, low self-noise, high sensitivity, difficult polarization and the like.
In general, silver chloride is easily decomposed by light, and therefore, it is necessary to protect the porous electrode from light in the whole process. In addition, silver chloride and silver are usually mixed and prepared into a whole by means of sintering, electroplating and the like, the electrochemical generation place is generally limited on the contact surface of the silver chloride and the silver, and in the related use environment, silver chloride particles can be decomposed into silver nanoparticles after the silver chloride particles are exposed to light, so that the originally small reaction area is smaller, and the performance of the sensor is reduced or even loses efficacy. In general environmental applications, the electrodes must be in direct contact with the medium to be measured, and particularly, when the fluid is detected and measured, silver chloride and silver are continuously lost along with the fluid. Due to the above-mentioned problems occurring in the use of the porous electrode, the service life of the porous electrode is short.
In order to solve the problem that the service life of the porous electrode is short, the application provides the porous electrode.
Disclosure of Invention
In order to solve the problem of short service life of the porous electrode, the application provides a porous electrode, comprising: the silver-containing conductive porous element comprises a silver column, a silver chloride powder layer and a conductive porous element, wherein a cylindrical counter bore is formed in the surface of the conductive porous element, the silver chloride powder layer is arranged at the bottom of the cylindrical counter bore and connected with the conductive porous element, the silver column is arranged in the cylindrical counter bore and connected with the silver chloride powder layer, and the silver column is connected with the conductive porous element.
The porous electrode is applied to the field of electrochemical sensors and used for collecting electric signals or used as a reference electrode. The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the silver chloride can be prevented from being decomposed by visible light, the silver chloride loss caused by direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Optionally, the conductive porous element comprises one or more of metal wool, metal foam, an at least partially conductive porous polymer, an at least partially conductive porous ceramic, an at least partially conductive porous graphite, and an at least partially conductive activated carbon.
The conductive porous element is in contact with the silver column and the silver chloride to serve as a place for electrolytic reaction, and meanwhile, the phenomenon that the silver chloride is continuously lost along with fluid in the reaction process and decomposed under light is avoided, and the service life of the porous electrode is prolonged.
Optionally, the particle size of the powder of the silver chloride powder layer is 0.5-1um, and the mass of the silver chloride arranged in the cylindrical counter bore is 3-7mg.
Optionally, the diameter of the conductive porous element is greater than or equal to 4mm, the height of the conductive porous element is greater than or equal to 5mm, the height of the cylindrical counter bore is less than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore is less than or equal to the diameter of the conductive porous element.
The cylindrical holes arranged on the surface of the conductive porous element are used for arranging silver chloride and silver, the bottom surfaces and the side surfaces of the cylindrical holes are required to be made of conductive porous materials, and only the upper surfaces of the cylindrical holes are open, so that the height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element.
The application also protects a method for preparing the electrode, which is used for preparing the porous electrode and comprises the following steps:
arranging a cylindrical counter bore on the surface of the conductive porous element, and arranging a silver chloride powder layer in the cylindrical counter bore to form a silver chloride powder layer;
and arranging the silver columns in the cylindrical counter bores, wherein the silver columns are connected with the silver chloride powder layer, and the silver columns are connected with the conductive porous element to obtain the porous electrode.
Optionally, the particle size of the silver chloride powder layer powder is 0.5-1um, and the mass of the silver chloride in the cylindrical counter bore formed in the surface of the conductive porous element is 3-7mg.
Optionally, the conductive porous element comprises one or more of metal wool, metal foam, at least partially conductive porous polymer, at least partially conductive porous ceramic, at least partially conductive porous graphite and at least partially conductive activated carbon; the diameter of the conductive porous element is larger than or equal to 4mm, the height of the conductive porous element is larger than or equal to 5mm, the height of the cylindrical counter bore is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore is smaller than or equal to the diameter of the conductive porous element.
Optionally, in the step of connecting the silver posts or the conductive porous element, a method for connecting the silver posts and the conductive porous element includes one or more of a colloid bonding method, a mechanical compression method, and a sintering method.
Optionally, the method for preparing the porous electrode further includes:
and (3) activating the porous electrode by using a solution containing chloride ions to obtain the activated porous electrode.
The utility model provides a novel porous electrode sets up a columniform hole in with electrically conductive porous material to place the electrode material of silver chloride and silver in the hole, in order to realize extension porous electrode life's purpose. The application also provides a method for preparing the porous electrode.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments are briefly described below, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic view of a porous electrode;
fig. 2 is a flow chart of a method of making a porous electrode.
Detailed Description
Reference will now be made in detail to embodiments, examples of which are illustrated in the accompanying drawings. The following description refers to the accompanying drawings in which the same numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following examples do not represent all embodiments consistent with the present application. But merely as exemplifications of systems and methods consistent with certain aspects of the application, as recited in the claims.
In the novel fields of ocean exploration, biosensing, intelligent detection and the like, the electrochemical sensor is widely applied. The porous electrode is a most popular reference electrode or signal acquisition electrode in various electrochemical sensors because of the advantages of small electrode impedance, small self-noise, high sensitivity, difficult polarization and the like.
Example 1:
the porous electrode has a structure shown in figure 1 and comprises a conductive porous material, a silver chloride powder layer and silver columns, wherein the powder particle size of the silver chloride powder layer is 0.5um; the conductive porous material is metal wool, and the diameter of the conductive porous element is 4mm, and the height of the conductive porous element is 5mm. A cylindrical counter bore is arranged on the surface of the conductive porous material, and the central axis of the counter bore is horizontal to the central axis of the conductive porous material. The height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element. The bottom of the counter bore is provided with a silver chloride powder layer, and the mass of the silver chloride powder is 3mg. The silver columns are arranged in the holes, and the silver chloride powder layer is arranged between the silver columns and the bottoms of the holes of the conductive porous material. The silver column and the conductive porous element are tightly connected by adopting a colloid bonding method.
The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the silver chloride can be prevented from being decomposed by visible light, the silver chloride loss caused by direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Example 2:
the porous electrode has a structure shown in figure 1, and comprises a conductive porous material, a silver chloride powder layer and a silver column, wherein the powder particle size of the silver chloride powder layer is 0.6um; the electrically conductive porous material is an at least partially electrically conductive porous polymer, said electrically conductive porous element having a diameter of 5mm and a height of 6mm. A cylindrical counter bore is arranged on the surface of the conductive porous material, and the central axis of the counter bore is horizontal to the central axis of the conductive porous material. The height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element. The bottom of the counter bore is provided with a silver chloride powder layer, and the mass of the silver chloride powder is 4mg. The silver columns are arranged in the holes, and the silver chloride powder layer is arranged between the silver columns and the bottoms of the holes of the conductive porous material. The silver column and the conductive porous element are tightly connected by adopting a mechanical compression method.
The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the visible light decomposition of the silver chloride can be avoided, the silver chloride loss caused by the direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Example 3:
the porous electrode has a structure shown in figure 1, and comprises a conductive porous material, a silver chloride powder layer and a silver column, wherein the powder particle size of the silver chloride powder layer is 0.5um; the electrically conductive porous material is an at least partially electrically conductive porous ceramic, said electrically conductive porous element having a diameter of 6mm and a height of 7mm. A cylindrical counter bore is arranged on the surface of the conductive porous material, and the central axis of the counter bore is horizontal to the central axis of the conductive porous material. The height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element. The bottom of the counter bore is provided with a silver chloride powder layer, and the mass of the silver chloride powder is 7mg. The silver columns are arranged in the holes, and the silver chloride powder layer is arranged between the silver columns and the bottoms of the holes of the conductive porous material. The silver column and the conductive porous element are tightly connected by adopting a sintering method.
The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the visible light decomposition of the silver chloride can be avoided, the silver chloride loss caused by the direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Example 4:
the porous electrode has a structure shown in figure 1, and comprises a conductive porous material, a silver chloride powder layer and a silver column, wherein the particle size of the powder of the silver chloride powder layer is 1um; the outer layer of electrically conductive porous material is at least partially electrically conductive and the inner layer of porous graphite is a metal foam, said electrically conductive porous element having a diameter of 4mm and a height of 5mm. A cylindrical counter bore is arranged on the surface of the conductive porous material, and the central axis of the counter bore is horizontal to the central axis of the conductive porous material. The height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element. The bottom of the counter bore is provided with a silver chloride powder layer, and the mass of the silver chloride powder is 5mg. The silver columns are arranged in the holes, and the silver chloride powder layer is arranged between the silver columns and the bottoms of the holes of the conductive porous material. The silver column and the conductive porous element are tightly connected by adopting a colloid bonding method.
The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the visible light decomposition of the silver chloride can be avoided, the silver chloride loss caused by the direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Example 5:
the porous electrode has a structure shown in figure 1, and comprises a conductive porous material, a silver chloride powder layer and a silver column, wherein the particle size of the powder of the silver chloride powder layer is 0.5um; the outer layer of conductive porous material is an at least partially conductive inner layer of activated carbon, that is a metal wool, and the conductive porous element has a diameter of 4mm and a height of 5mm. A cylindrical counter bore is arranged on the surface of the conductive porous material, and the central axis of the counter bore is horizontal to the central axis of the conductive porous material. The height of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore arranged on the surface of the conductive porous element is smaller than or equal to the diameter of the conductive porous element. The bottom of the counter bore is provided with a silver chloride powder layer, and the mass of the silver chloride powder is 6mg. The silver columns are arranged in the holes, and the silver chloride powder layer is arranged between the silver columns and the bottoms of the holes of the conductive porous material. The silver column and the conductive porous element are tightly connected by adopting a colloid bonding method.
The silver chloride and the silver are used as electrochemical reactants, and the conductive porous element is in close contact with the silver chloride and is used for providing a reaction site for electrochemical reaction. The silver chloride is arranged in the cylindrical counter bore of the porous element, so that the silver chloride can be prevented from being decomposed by visible light, the silver chloride loss caused by direct contact of the silver chloride and a measured medium in the using process can be reduced, and the service life of the porous electrode is prolonged.
Example 6:
the preparation process of the porous electrode is shown in fig. 2. Arranging a cylindrical counter bore on the surface of the conductive porous element, wherein the central axis of the counter bore is horizontal to the central axis of the conductive porous element, and arranging silver chloride powder in the cylindrical counter bore arranged on the surface of the conductive porous element to form a silver chloride powder layer; arranging the silver column in the cylindrical counter bore, closely connecting the silver column with the silver chloride powder layer, and connecting the silver column with the conductive porous element to obtain a porous electrode; and (3) activating the porous electrode by using a solution containing chloride ions to obtain the activated porous electrode.
The particle size of the silver chloride powder is 0.5um, and the mass of the silver chloride arranged in the cylindrical counter bore arranged on the surface of the conductive porous element is 3mg. The conductive porous element is metal wool; the diameter of the conductive porous element is 4mm, the height of the conductive porous element is 5mm, the height of the cylindrical counter bore is smaller than or equal to the height of the conductive porous element, the diameter of the cylindrical counter bore is smaller than or equal to the diameter of the conductive porous element, and in the step of connecting the silver column or the silver column with the conductive porous element, the silver column and the conductive porous element are tightly connected through a colloid bonding method.
Example 7:
the preparation process of the porous electrode is shown in fig. 2. Arranging a cylindrical counter bore on the surface of the conductive porous element, wherein the height of the counter bore is equal to that of the conductive porous element, and arranging silver chloride powder in the cylindrical counter bore arranged on the surface of the conductive porous element to form a silver chloride powder layer; arranging the silver columns in the cylindrical counter bores, connecting the silver columns with the silver chloride powder layer, and connecting the silver columns with the conductive porous element to obtain a porous electrode; and (3) carrying out activation treatment on the porous electrode by using a solution containing chloride ions to obtain the activated porous electrode.
The particle size of the silver chloride powder is 0.5-1um, and the mass of the silver chloride arranged in the cylindrical counter bore arranged on the surface of the conductive porous element is 6mg. The outer layer of the electrically conductive porous element is a metal foam and the inner layer is an at least partially electrically conductive porous polymer; the diameter of the conductive porous element is 6mm, the height of the conductive porous element is 8mm, the height of the cylindrical counter bore is smaller than or equal to the height of the conductive porous element, the diameter of the cylindrical counter bore is smaller than or equal to the diameter of the conductive porous element, and in the step of connecting the silver column with the conductive porous element, a method for tightly connecting the silver column with the conductive porous element is a colloid mechanical compression method.
Example 8:
the preparation process of the porous electrode is shown in fig. 2. Arranging a cylindrical counter bore on the surface of the conductive porous element, wherein the height of the counter bore is equal to that of the conductive porous element, and arranging silver chloride powder in the cylindrical counter bore arranged on the surface of the conductive porous element to form a silver chloride powder layer; arranging the silver column in the cylindrical counter bore, connecting the silver column with the silver chloride powder layer, and connecting the silver column with the conductive porous element to obtain a porous electrode; and (3) carrying out activation treatment on the porous electrode by using a solution containing chloride ions to obtain the activated porous electrode.
Wherein the particle diameter of silver chloride powder is 0.7um, the silver chloride quality of setting in the cylindrical counter bore that sets up electrically conductive porous component surface is 7mg. The outer layer of the electrically conductive porous element is an at least partially electrically conductive porous ceramic inner layer that is at least partially electrically conductive porous graphite and at least partially electrically conductive activated carbon; the diameter of the conductive porous element is 5mm, the height of the conductive porous element is 7mm, the height of the cylindrical counter bore is smaller than or equal to the height of the conductive porous element, the diameter of the cylindrical counter bore is smaller than or equal to the diameter of the conductive porous element, and in the step of connecting the silver column with the conductive porous element, the method for tightly connecting the silver column with the conductive porous element is a sintering method.
The embodiments provided in the present application are only a few examples of the general concept of the present application, and do not limit the scope of the present application. Any other embodiments extended according to the scheme of the present application without inventive efforts will be within the scope of protection of the present application for a person skilled in the art.
Claims (10)
1. A porous electrode, comprising: the silver column, the silver chloride powder layer and the conductive porous element; the conductive porous element is a cylinder, a cylindrical counter bore is arranged on the surface of the conductive porous element, the central axis of the cylindrical counter bore arranged on the surface of the conductive porous element is parallel to the central axis of the conductive porous element, the silver chloride powder end layer is arranged at the bottom of the cylindrical counter bore and connected with the conductive porous element, the silver column is arranged in the cylindrical counter bore and connected with the silver chloride powder end layer, and the silver column is connected with the conductive porous element.
2. The electrode of claim 1, wherein the electrically conductive porous element comprises one or more of metal wool, metal foam, an at least partially electrically conductive porous polymer, an at least partially electrically conductive porous ceramic, an at least partially electrically conductive porous graphite, and an at least partially electrically conductive activated carbon.
3. The electrode according to claim 1, wherein the powder of the silver chloride powder layer has a particle size of 0.5-1um.
4. The electrode of claim 1, wherein the mass of silver chloride disposed within the cylindrical counter bore is 3-7mg.
5. The electrode of claim 1, wherein the conductive porous element has a diameter greater than or equal to 4mm and a height greater than or equal to 5mm, wherein the cylindrical counter bore has a height less than or equal to the height of the conductive porous element, and wherein the diameter of the cylindrical counter bore is less than or equal to the diameter of the conductive porous element.
6. A method of preparing an electrode for preparing the porous electrode of claim 1, comprising:
arranging a cylindrical counter bore on the surface of the conductive porous element, and arranging silver chloride powder in the cylindrical counter bore to form a silver chloride powder layer;
and arranging the silver columns in the cylindrical counter bores, connecting the silver columns with the silver chloride powder layer, and connecting the silver columns with the conductive porous element to obtain the porous electrode.
7. The method according to claim 6, wherein the powder of the silver chloride powder layer has a particle size of 0.5-1um, and the mass of silver chloride disposed in the cylindrical counterbore is 3-7mg.
8. The method of claim 6, wherein the electrically conductive porous element comprises one or more of metal wool, metal foam, an at least partially electrically conductive porous polymer, an at least partially electrically conductive porous ceramic, an at least partially electrically conductive porous graphite, and an at least partially electrically conductive activated carbon; the diameter of the conductive porous element is larger than or equal to 4mm, the height of the conductive porous element is larger than or equal to 5mm, the height of the cylindrical counter bore is smaller than or equal to the height of the conductive porous element, and the diameter of the cylindrical counter bore is smaller than or equal to the diameter of the conductive porous element.
9. The method according to claim 6, wherein in the step of connecting the silver pillar to the conductive porous member, the connection between the silver pillar and the conductive porous member includes one or more of a colloid bonding method, a mechanical compression method, and a sintering method.
10. The method of claim 6, further comprising:
and (3) activating the porous electrode by using a solution containing chloride ions to obtain the activated porous electrode.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210837819.8A CN115219573A (en) | 2022-07-15 | 2022-07-15 | Porous electrode and preparation method thereof |
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| CN202210837819.8A CN115219573A (en) | 2022-07-15 | 2022-07-15 | Porous electrode and preparation method thereof |
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Citations (10)
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| GB802650A (en) * | 1943-11-01 | 1958-10-08 | Francis Herbert Mohun Vaughan | Improvements in and relating to electrode elements |
| JPH0387643A (en) * | 1989-05-24 | 1991-04-12 | Hitachi Ltd | Electrochemical electrode and electrochemical cell using this electrode |
| JPH0720081A (en) * | 1993-07-02 | 1995-01-24 | Nakabootec:Kk | Silver/silver chloride reference electrode and its manufacture |
| JPH102876A (en) * | 1996-06-14 | 1998-01-06 | Hitachi Ltd | Chloride ion sensor |
| RU2002119679A (en) * | 2002-07-24 | 2004-01-20 | Научно-исследовательский институт интроскопии при Томском политехническом университете | Electrode device |
| WO2012057606A1 (en) * | 2010-10-29 | 2012-05-03 | Mimos Berhad | Silver and silver chloride reference electrode |
| CN204241414U (en) * | 2014-12-03 | 2015-04-01 | 上海仪电科学仪器股份有限公司 | A kind of Novel silver silver chloride reference system |
| CN107102362A (en) * | 2017-05-09 | 2017-08-29 | 中国地质大学（武汉） | A kind of Ag/AgCl solid nonpolarizing electrodes and preparation method thereof |
| CN109310355A (en) * | 2016-06-30 | 2019-02-05 | 拓自达电线株式会社 | Electrode material |
| CN110989008A (en) * | 2019-12-26 | 2020-04-10 | 吉林大学 | Nano Ag-AgCl solid nonpolarized electrode and preparation method thereof |
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2022
- 2022-07-15 CN CN202210837819.8A patent/CN115219573A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB802650A (en) * | 1943-11-01 | 1958-10-08 | Francis Herbert Mohun Vaughan | Improvements in and relating to electrode elements |
| JPH0387643A (en) * | 1989-05-24 | 1991-04-12 | Hitachi Ltd | Electrochemical electrode and electrochemical cell using this electrode |
| JPH0720081A (en) * | 1993-07-02 | 1995-01-24 | Nakabootec:Kk | Silver/silver chloride reference electrode and its manufacture |
| JPH102876A (en) * | 1996-06-14 | 1998-01-06 | Hitachi Ltd | Chloride ion sensor |
| RU2002119679A (en) * | 2002-07-24 | 2004-01-20 | Научно-исследовательский институт интроскопии при Томском политехническом университете | Electrode device |
| WO2012057606A1 (en) * | 2010-10-29 | 2012-05-03 | Mimos Berhad | Silver and silver chloride reference electrode |
| CN204241414U (en) * | 2014-12-03 | 2015-04-01 | 上海仪电科学仪器股份有限公司 | A kind of Novel silver silver chloride reference system |
| CN109310355A (en) * | 2016-06-30 | 2019-02-05 | 拓自达电线株式会社 | Electrode material |
| CN107102362A (en) * | 2017-05-09 | 2017-08-29 | 中国地质大学（武汉） | A kind of Ag/AgCl solid nonpolarizing electrodes and preparation method thereof |
| CN110989008A (en) * | 2019-12-26 | 2020-04-10 | 吉林大学 | Nano Ag-AgCl solid nonpolarized electrode and preparation method thereof |
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