CN110438525A - A kind of porous electrode and its application producing gas for electrochemistry - Google Patents
A kind of porous electrode and its application producing gas for electrochemistry Download PDFInfo
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- CN110438525A CN110438525A CN201910732265.3A CN201910732265A CN110438525A CN 110438525 A CN110438525 A CN 110438525A CN 201910732265 A CN201910732265 A CN 201910732265A CN 110438525 A CN110438525 A CN 110438525A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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- 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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of porous electrode for producing gas for electrochemistry, the electrode is the porous metals network structure electrode of hole size distribution gradient.Herein described porous electrode is a kind of porous metals network structure electrode of hole gradient distribution, electrode structure is designed and is optimized for the different function of different location on electrode, the overpotential on electrode is significantly reduced, to improve electrolytic efficiency, cut operating costs;Preparation method multiplicity, the techniques such as 3D printing, stamping of powder, metal metallurgy smelting can realize the change of gradient in aperture by changing parameter or increasing and decreasing pore creating material;It has wide range of applications, gradient porous electrode is widely portable to the fields such as acid electrolysis water, alkali formula electrolytic water device, chlorine industry, electrochemical wastewater processing, and design principle is suitable for existing simultaneously other electrochemical reactions that solid-liquid, solid gas, solid-liquid-gas are catalyzed.
Description
Technical field
The present invention relates to electrochemistry and electrochemistry to produce gas technical field, especially a kind of porous electricity that gas is produced for electrochemistry
Pole.
Background technique
As environmental problem is more and more severeer, the development and use of renewable energy are had received widespread attention.However, to the greatest extent
Pipe renewable energy " inexhaustible, nexhaustible ", but limited by factors such as its timeliness and region, it can not
It is directly used in daily life well, it is necessary to first pass through the transport and storage of energy.Due to the receipts of renewable energy
Collection is mainly distributed on the lesser area of the density of population, therefore electric energy is very high by cost needed for long-range transmission of electricity.It will be by renewable
The energy obtains electric energy to be converted into easily stored chemical energy and be stored in fuel being very cost-effective mode.Pass through fuel
It is a kind of very efficient selection that electric energy is obtained fuel by way of electrolysis by battery.Fuel caused by being electrolysed can be detached from
The limitation of battery device itself, is individually stored and is transported.The application model of produced fuel can also be according to application simultaneously
Specific adjustment, therefore there is very big flexibility and reliability.
Hydrogen is one kind of fuel, is referred to as the green energy resource closest to future, its small, energy enthalpy with relative formula mass
Value is high, oxidation product only has the advantages that water is pollution-free.Meanwhile hydrogen is also one of industrial important source material, is widely applied
In synthesis ammonia, gasoline refining, fine welding and food industry.Have using renewable energy electrolysis producing hydrogen apparent
Realistic meaning.Therefore, efficient electrolysis water aerogenesis apparatus how is developed to have a very important significance, and electrode is produced as electrolysis
Core component in device of air is then even more the most important thing therein.
Currently, binding isotherm calculates and related experiment is as a result, commercial electrolyte aerogenesis apparatus electrode is guarantee stability and can
By property, mainly still use sheet metal or foam metal as electrode.For the catalytic performance and stabilization for further promoting electrode
Property, researchers are made that many work in terms of the material of electrode, and the preparation process of electrode is studied and explored.
However, there is no set the structure of electrode in terms of the research for producing pneumoelectric pole to electrolysis above is concentrated mainly on material modification
Meter and exploitation.In practical work process, the structure of electrode can generate apparent influence to the electrochemical over potential in electrolytic process.
When electrode cannot be discharged in time to empty electrochemical reaction active site in the gas that electrode surface generates, electrolytic cell will be will receive
The influence of apparent concentration polarization, generates larger overpotential, so that consumption electric energy increases, efficiency reduces.Therefore, if energy
Enough reasonable design electrode structures, can effectively reduce overpotential, improve the efficiency of electrolysis aerogenesis apparatus, reduce operation at
This.
Summary of the invention
Based on this, provided a kind of for electrochemistry it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place
Produce the porous electrode of gas.Herein described porous electrode is a kind of porous metals network structure electrode of hole gradient distribution, needle
The different function of different location on electrode is designed and is optimized to electrode structure, the overpotential on electrode is significantly reduced,
To improve electrolytic efficiency, cut operating costs.
To achieve the above object, the technical solution used in the present invention are as follows: a kind of porous electrode that gas is produced for electrochemistry,
The electrode is the porous metals network structure electrode of hole size distribution gradient.Specifically refer to the hole inside porous electrode
It is in one-dimensional square by pore size distribution gradient.
The present invention is to be designed on the basis of traditional punch metal plate electrode to the structure of hole.Specifically by it
Hole makes it in the electrodes, improve gas on electrode according to specific gradient distribution with this by pore size, by special preparation technique
The mass-transfer efficiency of body, ion, to reduce the overpotential on electrode, improve electrolysis water efficiency.
Design principle of the invention is as follows: by taking the electrolysis water under alkaline condition as an example, when electrochemistry aerogenesis apparatus works,
Shown in electrochemical reaction formula such as following formula (1), (2) on electrode.
4OH-→2H2O+0.5O2+4e- (1)
2H2O+2e-→H2+2OH- (2)
As can be seen that producing one of the necessary condition of gas as electrochemistry, can there are ion and gas in reaction process simultaneously
Participation.This has higher requirement to the mass transfer exchange rate of the two.Under conditions of porosity is certain, aperture can make ion
Elongated with the diffusion free path of gas, i.e., mass transfer is apart from elongated.This is unfavorable to mass exchange rate is improved.However, electrode
On reaction be all to occur under the catalytic action of electrode surface, the catalytic action of this surface of solids can ratio table to electrode
Area has higher requirement.At this time, aperture can obtain bigger specific surface instead, to obtain higher catalysis effect
Rate.Therefore, electrochemistry, which produces gas, has the different of mutual antagonism to require at electrode.In general, electrolytic water device includes two blocks of electricity
Pole plate and the electrolyte (film) of centre.For the ion for participating in reaction, when reaction is from hydrogen-precipitating electrode to analysis oxygen electrode
Diffusion.That is, the main generation place of electrochemical reaction is in the side close to electrolyte.It therefore, can be according to this
Characteristic is designed and optimizes to the structure of electrode.
Therefore, we have proposed the gradient porous electrodes that gas is produced for electrochemistry.For device work characteristics, electricity will be close to
Solution matter side is prepared into the porous structure with small-bore, to increase specific surface, improves reaction efficiency;It will be far from electrode side to be prepared into
Porous structure with large aperture, to reduce the diffusion free path of ion and gas.By above-mentioned design, it can effectively improve
The performance of electrode when electrolysis reduces overpotential, improves electrolytic efficiency.
Preferably, described hole size is that continuous gradient changes or discontinuous gradient changes.
Preferably, described hole size is local continuous change of gradient or/and partial discontinuous change of gradient.
Preferably, described hole size increases in gradient;Or described hole size is reduced in gradient.The porous electrode
Hole configurations includes and is not limited to straight hole, circular hole, square hole, irregular hole.
Preferably, when described hole size is discontinuous variation, hole size includes at least three-level different size, in gradient
The composite structure of arrangement, with meet reactor at different location between pore size and specific surface mutual antagonism different demands.
Preferably, the porous electrode is that aperture (increasing active specific surface)-mesoporous (transitional region)-macropore (is improved and passed
Matter rate) composite construction, wherein the porous electrode is aperture gauge structure close to electrolyte side, and the porous electrode is remote
It is macropore gauge structure from electrode side.
Preferably, the electrode is chip or flat.
Preferably, the material of the porous electrode is the electrode material of commercial electrolyte water.Specifically include and be not limited to nickel,
Iron, molybdenum, platinum, rhodium, palladium and its alloy.
Preferably, the preparation method of the porous electrode be 3D printing, compression molding, metal metallurgy smelting, powder metallurgy, etc. it is quiet
Molded, loose sintering molding, powder rolling, powder extrusion molding, centrifugal deposition molding, injection moulding, laser fast shaping,
One of electron beam rapid shaping.
Meanwhile the porous electrode of the gas electrolysis water under external electrical energy drive is produced for electrochemistry the present invention also provides described
Application in the anode of device, cathode or symmetry electrode.
Compared with the existing technology, the invention has the benefit that
1, this patent carries out structure optimization from the traditional electrode that structure design angle produces gas to electrochemistry for the first time, not to electricity
Pole material effectively raises electrode performance in the case of being adjusted;
2, this patent proposes the preparation method multiplicity of porous gradient electrode, the techniques such as 3D printing, stamping of powder, metal metallurgy smelting
The change of gradient in aperture can be realized by changing parameter or increasing and decreasing pore creating material;
3, this patent has wide range of applications, and gradient porous electrode is widely portable to acid electrolysis water, alkali formula electrolysis water
The fields such as device, chlorine industry, electrochemical wastewater processing, design principle, which is suitable for existing simultaneously solid-liquid, solid gas, solid-liquid-gas, urges
The other electrochemical reactions changed.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of porous electrode of the present invention;
Fig. 2 is a kind of cross-sectional view of the structure (choosing two of them unit) of porous electrode described in embodiment 1;
Fig. 3 is a kind of cross-sectional view of the structure (choosing two of them unit) of porous electrode described in embodiment 2;
Fig. 4 is a kind of cross-sectional view of the structure (choosing two of them unit) of porous electrode described in embodiment 3;
Fig. 5 is the OER polarization curve of gradient porous nickel sheet 3D1 in embodiment 1;
Fig. 6 is the HER polarization curve of gradient porous nickel sheet 3D1 in embodiment 1;
Fig. 7 is the OER polarization curve of gradient porous nickel sheet 3D2 in embodiment 2;
Fig. 8 is the HER polarization curve of gradient porous nickel sheet 3D2 in embodiment 2;
Fig. 9 is the OER polarization curve of gradient porous nickel sheet 3D3 in embodiment 3;
Figure 10 is the HER polarization curve of gradient porous nickel sheet 3D3 in embodiment 3.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
Comparative example
High-purity punching nickel sheet sample as a comparison is selected, selected punching nickel sheet porosity is 35% (± 1%).Weigh 56g
KOH is dissolved in 1L deionized water, is configured to 1mol L-1KOH solution.Punching nickel sheet obtained is impregnated in KOH solution
For 24 hours, it is activated.After the completion of activation, using punching nickel sheet as working electrode, carbon-point as to electrode, Hg/HgO as
The electro-chemical test of reference electrode progress three-electrode system.
It is tested using alkali formula electrolysis water performance of the Princeton PAR4000 electrochemical workstation to punching nickel sheet.Choosing
Constant voltage range is -1.7~1.1V (vs.Hg/HgO), scanning speed is 10mV s-1Cyclic voltammetric is carried out to punching nickel sheet to sweep
It retouches.Take pole of the curve for just sweeping direction as punching nickel sheet oxygen evolution reaction (Oxygen Evolution Reaction, OER)
Change curve, the negative curve for sweeping direction is as punching nickel sheet Hydrogen evolving reaction (Hydrogen Evolution Reaction, HER)
Polarization curve.With current density 10mA cm-2When corresponding analysis oxygen (hydrogen) current potential as overpotential, measure punching nickel sheet OER mistake
Current potential is 332mV, and HER overpotential is 266mV.Meanwhile using the polarization curve of punching nickel sheet as reference curve, it is shown in pair
In the OER/HER curve answered (Fig. 5~10), indicated with black hyphen dotted line.
Embodiment 1
The overall structure of porous electrode described in the present embodiment is as shown in Figure 1, Fig. 2 is the section for choosing two of them unit
Figure, it can be seen that the electrode is the porous metals network structure electrode of three-level hole size distribution gradient, specifically by three-level
The conical hole of different pore size forms, and secondary level-one is tangent compared with the edge of roundlet taper hole and the edge of the larger conical bore of upper level:
Construct 3D model and model progress dough sheet reparation and slicing treatment with the export of STL format, by derived STL format
And the parameter for editing laser printing is imported in 3D printing special-purpose software, finally import Germany EOS metal 3D printing equipment EOSM290
In, using high-purity nickel powder as raw material, carry out printing manufacture.Prepared gradient pore nickel sheet porosity is 35% (± 1%).Weigh 56g
KOH is dissolved in 1L deionized water, is configured to 1mol L-1KOH solution.Gradient pore nickel sheet obtained is impregnated in KOH solution
For 24 hours, it is activated.After the completion of activation, using gradient pore nickel sheet as working electrode, carbon-point as to electrode, Hg/HgO work
The electro-chemical test of three-electrode system is carried out for reference electrode.
It is tested using alkali formula electrolysis water performance of the Princeton PAR4000 electrochemical workstation to gradient pore nickel sheet.
Selected voltage range is -1.7~1.1V (vs.Hg/HgO), scanning speed is 10mV s-1Cyclic voltammetric is carried out to gradient pore nickel sheet
Scanning.Take the curve for just sweeping direction as gradient pore nickel sheet oxygen evolution reaction (Oxygen Evolution Reaction, OER)
Polarization curve, the negative curve for sweeping direction is as gradient pore nickel sheet Hydrogen evolving reaction (Hydrogen Evolution
Reaction, HER) polarization curve.With current density 10mA cm-2When corresponding analysis oxygen (hydrogen) current potential as overpotential.It will be electric
The data of test chemical are plotted in Fig. 5, Fig. 6.
The OER overpotential of gradient pore nickel sheet is 288mV, HER overpotential 252mV it can be seen from Fig. 5, Fig. 6, and the two is equal
Less than the OER overpotential (332mV) and HER overpotential (266mV) of punching nickel sheet.Since the material of Different electrodes is identical, hole
Rate is identical, therefore the difference of overpotential directly depends on influence of the hole configurations to catalytic performance, i.e., is substantially hole configurations
Influence to gas, ion mass transfer rate.The gradient pore nickel sheet in the present embodiment has smaller overpotential as a result, i.e., higher
Gas, ion mass transfer rate.Therefore the gradient porous electrode that the present embodiment is proposed has apparent superiority.
Embodiment 2
The overall structure of porous electrode described in the present embodiment is as shown in Figure 1, Fig. 3 is the section for choosing two of them unit
Figure, it can be seen that the electrode is the porous metals network structure electrode of three-level hole size distribution gradient, specifically by three-level
The rectangle hole of different pore size forms, and the edge at the edge and the larger rectangular opening of upper level of the secondary smaller rectangular opening of level-one is tangent.
3D model is constructed with shown drawing and is exported with STL format, and the model of derived STL format is subjected to dough sheet reparation
With slicing treatment and import in 3D printing special-purpose software edit laser printing parameter, finally import Germany's EOS metal 3D printing
In equipment EOSM290, using high-purity nickel powder as raw material, printing manufacture is carried out.Prepared gradient pore nickel sheet porosity be 35% (±
1%).It weighs 56g KOH to be dissolved in 1L deionized water, is configured to 1mol L-1KOH solution.Gradient pore nickel sheet obtained is existed
It is impregnated in KOH solution for 24 hours, it is activated.After the completion of activation, using gradient pore nickel sheet as working electrode, carbon-point as pair
Electrode, Hg/HgO carry out the electro-chemical test of three-electrode system as reference electrode.
It is tested using alkali formula electrolysis water performance of the Princeton PAR4000 electrochemical workstation to gradient pore nickel sheet.
Selected voltage range is -1.7~1.1V (vs.Hg/HgO), scanning speed is 10mV s-1Cyclic voltammetric is carried out to gradient pore nickel sheet
Scanning.Take the curve for just sweeping direction as gradient pore nickel sheet oxygen evolution reaction (Oxygen Evolution Reaction, OER)
Polarization curve, the negative curve for sweeping direction is as gradient pore nickel sheet Hydrogen evolving reaction (Hydrogen Evolution
Reaction, HER) polarization curve.With current density 10mA cm-2When corresponding analysis oxygen (hydrogen) current potential as overpotential.It will be electric
The data of test chemical are plotted in Fig. 7, Fig. 8.
The OER overpotential of gradient pore nickel sheet is 285mV, HER overpotential 227mV it can be seen from Fig. 7, Fig. 8, and the two is equal
Less than the OER overpotential (332mV) and HER overpotential (266mV) of punching nickel sheet.Since the material of Different electrodes is identical, hole
Rate is identical, therefore the difference of overpotential directly depends on influence of the hole configurations to catalytic performance, i.e., is substantially hole configurations
Influence to gas, ion mass transfer rate.The gradient pore nickel sheet in the present embodiment has smaller overpotential as a result, i.e., higher
Gas, ion mass transfer rate.Therefore the gradient porous electrode that the present embodiment is proposed has apparent superiority.
Embodiment 3
The overall structure of porous electrode described in the present embodiment such as Fig. 1, Fig. 4 are the sectional view for choosing two of them unit, can
To find out, the electrode is the porous metals network structure electrode of three-level hole size distribution gradient, specifically by three-level difference
The circular hole in aperture forms, and the edge at the edge and upper level large round hole in secondary level-one smaller round hole is tangent.
3D model is constructed with shown drawing and is exported with STL format, and the model of derived STL format is subjected to dough sheet reparation
With slicing treatment and import in 3D printing special-purpose software edit laser printing parameter, finally import Germany's EOS metal 3D printing
In equipment EOSM290, using high-purity nickel powder as raw material, printing manufacture is carried out.Prepared gradient pore nickel sheet porosity be 35% (±
1%).It weighs 56g KOH to be dissolved in 1L deionized water, is configured to 1mol L-1KOH solution.Gradient pore nickel sheet obtained is existed
It is impregnated in KOH solution for 24 hours, it is activated.After the completion of activation, using gradient pore nickel sheet as working electrode, carbon-point as pair
Electrode, Hg/HgO carry out the electro-chemical test of three-electrode system as reference electrode.
It is tested using alkali formula electrolysis water performance of the Princeton PAR4000 electrochemical workstation to gradient pore nickel sheet.
Selected voltage range is -1.7~1.1V (vs.Hg/HgO), scanning speed is 10mV s-1Cyclic voltammetric is carried out to gradient pore nickel sheet
Scanning.Take the curve for just sweeping direction as gradient pore nickel sheet oxygen evolution reaction (Oxygen Evolution Reaction, OER)
Polarization curve, the negative curve for sweeping direction is as gradient pore nickel sheet Hydrogen evolving reaction (Hydrogen Evolution
Reaction, HER) polarization curve.With current density 10mA cm-2When corresponding analysis oxygen (hydrogen) current potential as overpotential.It will be electric
The data of test chemical are plotted in Fig. 9, Tu10Zhong.
The OER overpotential of gradient pore nickel sheet is 287mV, HER overpotential 243mV it can be seen from Fig. 9, Figure 10, and the two is equal
Less than the OER overpotential (332mV) and HER overpotential (266mV) of punching nickel sheet.Since the material of Different electrodes is identical, hole
Rate is identical, therefore the difference of overpotential directly depends on influence of the hole configurations to catalytic performance, i.e., is substantially hole configurations
Influence to gas, ion mass transfer rate.The gradient pore nickel sheet in the present embodiment has smaller overpotential as a result, i.e., higher
Gas, ion mass transfer rate.Therefore the gradient porous electrode that the present embodiment is proposed has apparent superiority.
In other embodiments, the hole of porous electrode of the present invention can be local continuous change of gradient or/and office
The variation of portion's discontinuous gradient, described hole size increase in gradient;Or described hole size is reduced in gradient;It can realize this
Particular technique effect in application, repeats no more in this.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of porous electrode for producing gas for electrochemistry, which is characterized in that the electrode is hole size distribution gradient
Porous metals network structure electrode.
2. the porous electrode of gas is produced for electrochemistry as described in claim 1, which is characterized in that described hole size is continuous
Change of gradient or discontinuous gradient variation.
3. the porous electrode of gas is produced for electrochemistry as claimed in claim 2, which is characterized in that described hole size is part
Continuous gradient variation or/and partial discontinuous change of gradient.
4. the porous electrode of gas is produced for electrochemistry as described in claim 1, which is characterized in that described hole size is in gradient
Increase;Or described hole size is reduced in gradient.
5. the porous electrode of gas is produced for electrochemistry as claimed in claim 2, which is characterized in that described hole size is not connect
When continuous variation, hole size is including at least three-level different size, the composite structure arranged in gradient.
6. the porous electrode of gas is produced for electrochemistry as claimed in claim 5, which is characterized in that the porous electrode is small
Hole-mesoporous-macropore composite construction.
7. the porous electrode as described in any one of claims 1 to 6 for producing gas for electrochemistry, which is characterized in that the electrode
For chip or flat.
8. the porous electrode as described in any one of claims 1 to 6 for producing gas for electrochemistry, which is characterized in that described porous
The material of electrode is the electrode material of commercial electrolyte water.
9. the porous electrode as described in any one of claims 1 to 6 for producing gas for electrochemistry, which is characterized in that described porous
The preparation method of electrode is 3D printing, compression molding, metal metallurgy smelting, powder metallurgy, isostatic pressing, loose sintering molding, powder
Last rolling, powder extrusion molding, centrifugal deposition molding, injection moulding, laser fast shaping, one in electron beam rapid shaping
Kind.
10. the porous electrode as described in any one of claims 1 to 9 for producing gas for electrochemistry is electrolysed under external electrical energy drive
Application in the anodes of water installations, cathode or symmetry electrode.
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