CN114150329A - Efficient nickel-based self-assembly oxygen evolution electrode - Google Patents
Efficient nickel-based self-assembly oxygen evolution electrode Download PDFInfo
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- CN114150329A CN114150329A CN202010830069.2A CN202010830069A CN114150329A CN 114150329 A CN114150329 A CN 114150329A CN 202010830069 A CN202010830069 A CN 202010830069A CN 114150329 A CN114150329 A CN 114150329A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 46
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000001301 oxygen Substances 0.000 title claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 20
- 238000001338 self-assembly Methods 0.000 title claims description 3
- 238000000034 method Methods 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000004070 electrodeposition Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract 4
- 230000000694 effects Effects 0.000 claims abstract 3
- OFBMZJXCFZLUJC-UHFFFAOYSA-M [OH-].[Ni+2].[O-2].[Fe+2] Chemical compound [OH-].[Ni+2].[O-2].[Fe+2] OFBMZJXCFZLUJC-UHFFFAOYSA-M 0.000 claims abstract 2
- 238000011065 in-situ storage Methods 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 4
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 1
- 230000008021 deposition Effects 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 235000014413 iron hydroxide Nutrition 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 239000013543 active substance Substances 0.000 abstract 1
- 238000006056 electrooxidation reaction Methods 0.000 abstract 1
- 229910000480 nickel oxide Inorganic materials 0.000 abstract 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 16
- 238000005868 electrolysis reaction Methods 0.000 description 11
- 239000003792 electrolyte Substances 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 11
- 238000011056 performance test Methods 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910021607 Silver chloride Inorganic materials 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 4
- 238000000527 sonication Methods 0.000 description 4
- 238000004832 voltammetry Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000004769 chrono-potentiometry Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 nickel metal oxide Chemical class 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229940010514 ammonium ferrous sulfate Drugs 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- DMTIXTXDJGWVCO-UHFFFAOYSA-N iron(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Fe++].[Ni++] DMTIXTXDJGWVCO-UHFFFAOYSA-N 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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
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- Chemical & Material Sciences (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
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Abstract
An efficient nickel-based self-assembled oxygen evolution electrode directly realizes in-situ oxidation on the surface of a nickel-based metal electrode by combining a simple hydrothermal oxidation method with electrochemical deposition to generate nickel oxide or hydroxide with better activity, then introduces iron element by electrochemical deposition to avoid the falling of surface active substances caused by the traditional preparation methods such as coating and spraying, and simultaneously the iron element generates iron oxide or hydroxide together due to the electrochemical oxidation effect, so that the generated nickel-iron oxide hydroxide has more complex structure, more catalytic sites and larger specific surface area, thereby effectively reducing the overpotential of the electrode and the energy consumption of electrolyzed water and improving the efficiency of electrolyzed water equipment.
Description
Technical Field
The invention belongs to the field of material science and disciplines and hydrogen production by alkaline water electrolysis, and particularly provides preparation of a nickel-based self-assembled oxygen evolution electrode for efficiently producing hydrogen by water electrolysis.
Background
With the continuous development of the industrial society, the environmental pollution is more serious. Hydrogen, a new clean energy source, is more important in the current society. Among various methods for producing hydrogen, the hydrogen production by electrolyzing water is a promising technology for obtaining high-purity hydrogen by electric energy. However, the slow kinetics of the four electrons of the oxygen evolution reaction and the high overpotential severely limit the efficiency of hydrogen production from water electrolysis. Traditional noble metal oxides such as iridium, ruthenium, platinum and the like are known as the most efficient oxygen evolution electrocatalysts, but the high price and low storage amount of the noble metals limit the wide application of the catalysts in water electrolysis oxygen production and the great development of water electrolysis hydrogen production processes. The search for efficient, stable, environmentally friendly and inexpensive electrocatalysts to replace precious metals is therefore the key to the development of electrolyzed water.
It has been shown that oxides and hydroxides of the first row transition metals (Mn, Fe, Co, Ni) exhibit good performance in alkaline and near neutral electrolytes, and in particular, hydroxides containing both nickel and iron are reported to have the lowest overpotential for oxygen evolution reactions under alkaline conditions (pH13 and pH14) and to be active at near neutral pH in borate buffers. The layered structure of bimetallic hydroxide of iron and nickel has larger active specific surface area, more active sites and lower overpotential in oxygen evolution reaction, and is the most promising material for replacing noble metals. Therefore, the nickel-iron bimetal oxide is constructed, so that the catalytic activity of the traditional electrolytic water electrode can be effectively improved, the whole electrolytic process is promoted, the overpotential is reduced, the cell voltage of an electrolytic cell is reduced, and the energy consumption of the electrolytic water is reduced.
However, the reported materials have the disadvantages of harsh preparation conditions, complex process and large energy consumption; the prepared catalyst is generally adhered to a substrate by methods such as spin coating, spray coating and coating, and the bonding method is not only weak, but also gaps can be generated at the bonding part, so that the resistance is increased, the catalyst falls off, and the service life of the electrode is seriously influenced.
In summary, it is still important to prepare an electrolytic water catalytic electrode of a nickel-iron compound by a simple, low-cost, and highly efficient and stable process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the electrode preparation method for self-assembling the nickel-iron compound on the nickel-based metal, and the method has the advantages of simple process, low cost and suitability for industrial production. The technical scheme is as follows:
firstly, directly controlling and synthesizing nickel metal oxide/hydroxide on the surface of nickel-based metal by utilizing a hydrothermal reaction under a milder alkaline condition, and then introducing an iron component by utilizing an electrodeposition method. The catalyst is a nickel metal oxide/hydroxide containing iron component. The method comprises the following specific steps:
1. pretreatment process of nickel-based metal: performing ultrasonic treatment in acetone and ethanol solution for 5-20 min respectively to remove surface oil layer; then ultrasonic treatment is carried out for 5 to 20 minutes in 0.5 to 6 mol per liter of hydrochloric acid to remove the oxide layer on the surface of the nickel-based metal.
2. Hydrothermal reaction: the solution of the hydrothermal reaction contains 0.1-2 mol/l of alkali, 5-500 micromol/l of hydrogen peroxide solution and 50 ml of deionized water. Putting the nickel-based metal subjected to pretreatment into a reaction solution, wherein the temperature of the hydrothermal reaction is 100-200 ℃, and the reaction time is 4-24 hours.
3. Electro-deposition: and (3) performing electrochemical deposition on the electrode obtained in the step (2) in a solution containing ferrous ions by using a chronopotentiometry, and introducing iron ions while oxidizing to form an electrode of nickel iron oxide or hydroxide.
Preferably, the nickel metal substrate is a nickel mesh or nickel foam.
Preferably, the base solution is a strongly alkaline solution, such as a potassium hydroxide or sodium hydroxide solution.
In the electrodeposition process, a two-electrode system is utilized, a nickel metal electrode obtained by hydrothermal reaction is used as a working electrode, hydrophilic carbon cloth is used as a counter electrode, a solution containing ferrous ions is used as an electrolyte, electrolysis is carried out under a certain current density by controlling the voltage of an electrolytic bath, and iron element enters the surface of nickel-based metal to generate an iron-nickel compound.
Preferably, the solution containing ferrous ions is a solution of ferrous chloride, ferrous sulfate, ferrous ammonium sulfate, or the like.
The invention has the advantages that: the introduction of iron element can be used as a high conductive layer to provide reliable electron transfer, overcome the defect of poor conductivity of simple nickel metal, reduce the energy barrier of intermediate products and promote catalytic reaction. Meanwhile, the layered structure of the bimetallic hydroxide of iron and nickel has larger active specific surface area, more active sites, lower overpotential in oxygen evolution reaction and quick release of gas products. The electrode material with the synergistic effect of the iron and the nickel elements has simple preparation process and easy scale-up production, and is an excellent choice for industrialized electrodes.
Drawings
FIG. 1 is a SEM photograph of the present invention.
FIG. 2 is a graph comparing the oxygen evolution performance of examples of the present invention with that of comparative examples.
FIG. 3 is a comparative graph of life tests of examples of the present invention and comparative examples.
Detailed Description
In order to better illustrate the technical features of the present invention, the following description is given with reference to specific examples, but the present invention is not limited thereto.
Example 1
The first step is as follows: respectively carrying out ultrasonic treatment on the nickel screen in ethanol and acetone solution for 10 minutes to remove a surface grease layer; then, the surface oxide layer was removed by sonication in a hydrochloric acid solution having a concentration of 3 mol/l for 10 minutes.
The second step is that: adding 0.16 g of sodium hydroxide, 1 ml of hydrogen peroxide and 50 ml of deionized water into a hydrothermal kettle with the volume of 100 ml, then putting the nickel mesh treated in the first step into the hydrothermal kettle together, carrying out hydrothermal reaction at 150 ℃ for 6 hours, and after the reaction is finished, cleaning and drying.
And testing the oxygen evolution performance and the service life performance of the electrode by using the Shanghai Chenghua CHI 660E electrochemical workstation. The performance test adopts a three-electrode system for testing, and water is used for testingThe nickel mesh electrode for heat treatment is a working electrode, the silver/silver chloride electrode is a reference electrode, the platinum mesh electrode is a counter electrode, the electrolyte is 1 mol per liter of potassium hydroxide solution, the scanning rate of linear voltammetry scanning is 5 millivolts per second, and the potential window is 0-1 volt. The test results are presented in FIG. 1, where J is the current density in mA cm-2Milliamps per square centimeter; e is the potential difference, and the unit V is volt; the life performance test was performed using a two-electrode system, the working electrode was the platinum mesh electrode, the counter electrode was a 1-mole per liter solution of potassium hydroxide, the constant current density was 100 milliamps per square centimeter, and the test time was 24 hours, as described in example 1. The test results are shown in FIG. 2, where Time is the electrolysis Time and the unit h is hour.
Example 2
The first step is as follows: respectively carrying out ultrasonic treatment on the foamed nickel in ethanol and acetone solution for 10 minutes to remove a surface grease layer; then, the surface oxide layer was removed by sonication in a hydrochloric acid solution having a concentration of 3 mol/l for 10 minutes.
The second step is that: adding 0.16 g of sodium hydroxide, 1 ml of hydrogen peroxide and 50 ml of deionized water into a hydrothermal kettle with the volume of 100 ml, then putting the foamed nickel treated in the first step into the hydrothermal kettle together, carrying out hydrothermal reaction at 150 ℃ for 6 hours, and after the reaction is finished, cleaning and drying.
And testing the oxygen evolution performance and the service life performance of the electrode by using the Shanghai Chenghua CHI 660E electrochemical workstation. The performance test adopts a three-electrode system to test, a foamed nickel electrode subjected to hydrothermal treatment is taken as a working electrode, a silver/silver chloride electrode is taken as a reference electrode, a platinum mesh electrode is taken as a counter electrode, an electrolyte is 1 mol per liter of potassium hydroxide solution, the scanning rate of linear voltammetry scanning is 5 millivolts per second, and the potential window is 0-1 volt. The test results are presented in FIG. 1, where J is the current density in mA cm-2Milliamps per square centimeter; e is the potential difference, and the unit V is volt; the life performance test was carried out using a two-electrode system, the working electrode was the platinum mesh electrode, the counter electrode was a 1 molar solution of potassium hydroxide per liter of electrolyte, the constant current density was 100 milliamps per square centimeter, and the test time was 24 hoursThen (c) is performed. The test results are shown in FIG. 2, where Time is the electrolysis Time and the unit h is hour.
Example 3
The first step is as follows: respectively carrying out ultrasonic treatment on the nickel screen in ethanol and acetone solution for 10 minutes to remove a surface grease layer; then, the surface oxide layer was removed by sonication in a hydrochloric acid solution having a concentration of 3 mol/l for 10 minutes.
The second step is that: adding 0.16 g of sodium hydroxide, 1 ml of hydrogen peroxide and 50 ml of deionized water into a hydrothermal kettle with the volume of 100 ml, then putting the nickel net treated in the first step into the hydrothermal kettle together, carrying out hydrothermal reaction at 150 ℃ for 6 hours, and cleaning and drying after the hydrothermal reaction is finished.
The third step: taking the electrode obtained in the last step as an anode and conductive hydrophilic carbon cloth as a cathode, and carrying out polarization treatment for 1 hour at a current density of 1.2 milliampere per square centimeter in 10 millimole per liter of ammonium ferrous sulfate solution by adopting a chronopotentiometry method; and repeatedly washing the treated electrode with distilled water, and drying to obtain the final electrode.
And testing the oxygen evolution performance and the service life performance of the electrode by using the Shanghai Chenghua CHI 660E electrochemical workstation. The performance test adopts a three-electrode system to test, the obtained final electrode is taken as a working electrode, a silver/silver chloride electrode is taken as a reference electrode, a platinum mesh electrode is taken as a counter electrode, the electrolyte is 1 mol per liter of potassium hydroxide solution, the scanning rate of linear voltammetry scanning is 5 millivolts per second, and the potential window is 0-1 volt. The test results are presented in FIG. 1, where J is the current density in mA cm-2Milliamps per square centimeter; e is the potential difference, and the unit V is volt; the service life performance test is carried out by adopting a two-electrode system, wherein a working electrode is a nickel mesh, a counter electrode is a platinum mesh electrode, electrolyte is 1 mol/L potassium hydroxide solution, the constant current density is 100 milliampere per square centimeter, and the test time is 24 hours. The test results are shown in FIG. 2, where Time is the electrolysis Time and the unit h is hour.
Example 4
The first step is as follows: respectively carrying out ultrasonic treatment on the foamed nickel in ethanol and acetone solution for 10 minutes to remove a surface grease layer; then, the surface oxide layer was removed by sonication in a hydrochloric acid solution having a concentration of 3 mol/l for 10 minutes.
The second step is that: adding 0.16 g of sodium hydroxide, 1 ml of hydrogen peroxide and 50 ml of deionized water into a hydrothermal kettle with the volume of 100 ml, then putting the foamed nickel treated in the first step into the hydrothermal kettle together, carrying out hydrothermal reaction at 150 ℃ for 6 hours, and cleaning and drying after the hydrothermal reaction is finished.
The third step: taking the electrode obtained in the last step as an anode and conductive hydrophilic carbon cloth as a cathode, and carrying out polarization treatment for 1 hour at a current density of 1.2 milliampere per square centimeter in 10 millimole per liter of ammonium ferrous sulfate solution by adopting a chronopotentiometry method; and repeatedly washing the treated electrode with distilled water, and drying to obtain the final electrode.
And testing the oxygen evolution performance and the service life performance of the electrode by using the Shanghai Chenghua CHI 660E electrochemical workstation. The performance test adopts a three-electrode system to test, the prepared foamed nickel electrode is taken as a working electrode, a silver/silver chloride electrode is taken as a reference electrode, a platinum mesh electrode is taken as a counter electrode, electrolyte is 1 mol per liter of potassium hydroxide solution, the scanning rate of linear voltammetry scanning is 5 millivolts per second, and the potential window is 0-1 volt. The test results are presented in FIG. 1, where J is the current density in mA cm-2Milliamps per square centimeter; e is the potential difference, and the unit V is volt; the service life performance test is carried out by adopting a two-electrode system, the working electrode is a prepared foamed nickel electrode, the counter electrode is a platinum mesh electrode, the electrolyte is 1 mol/L potassium hydroxide solution, the constant current density is 100 milliampere/square centimeter, and the test time is 24 hours. The test results are shown in FIG. 2, where Time is the electrolysis Time and the unit h is hour.
Comparative example
And directly carrying out electrochemical test on the electrode after the surface treatment step of the metal nickel screen is finished.
And testing the oxygen evolution performance and the service life performance of the electrode by using the Shanghai Chenghua CHI 660E electrochemical workstation. The performance test adopts a three-electrode system to test, a nickel screen is taken as a working electrode, a silver/silver chloride electrode is taken as a reference electrode, a platinum screen electrode is taken as a counter electrode, and the electrolyte is 1 mol per literThe sweep rate of the linear voltammetric sweep was 5 millivolts per second and the potential window was 0-1 volts. The test results are presented in FIG. 1, where J is the current density in mA cm-2Milliamps per square centimeter; e is the potential difference, and the unit V is volt; the service life performance test is carried out by adopting a two-electrode system, wherein a working electrode is a nickel mesh, a counter electrode is a platinum mesh electrode, electrolyte is 1 mol/L potassium hydroxide solution, the constant current density is 100 milliampere per square centimeter, and the test time is 24 hours. The test results are shown in FIG. 2, where Time is the electrolysis Time and the unit h is hour.
Claims (5)
1. A high-efficiency nickel-based self-assembly oxygen evolution electrode directly realizes in-situ oxidation on the surface of a nickel-based metal electrode by combining a simple hydrothermal oxidation method with an electrochemical deposition mode to generate an oxide or hydroxide of nickel with better activity, and then introduces an iron element by electrochemical deposition.
2. A high-efficiency nickel-based self-assembled oxygen evolution electrode is characterized in that the structure of the generated nickel-iron oxide hydroxide is more complex, more catalytic sites are provided, and the specific surface area is larger.
3. The method as claimed in claim 1, wherein the nickel-based metal is pre-treated by performing ultrasonic treatment in acetone, ethanol and hydrochloric acid with concentration of 0.5-5 mol/L for 5-20 min.
4. The method for preparing the high-efficiency nickel-based self-assembled oxygen evolution electrode as claimed in claim 1, wherein the hydrothermal method comprises the steps of using sodium hydroxide and hydrogen peroxide solution with different concentrations as reaction solutions, wherein the reaction temperature is 80-200 ℃ and the reaction time is 5-24 hours.
5. The method for preparing a high-efficiency nickel-based self-assembled oxygen evolution electrode as claimed in claim 1, wherein the electrochemical deposition method is to use a salt solution containing ferrous ions as the deposition solution, and the parameters are that the current density is 10-50 milliampere per square centimeter and the time of electrodeposition is 0.5-5 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116426951A (en) * | 2023-03-17 | 2023-07-14 | 湘南学院 | Leaf-like array amorphous phase nickel oxide/nickel foam electrode and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116426951A (en) * | 2023-03-17 | 2023-07-14 | 湘南学院 | Leaf-like array amorphous phase nickel oxide/nickel foam electrode and preparation method and application thereof |
| CN116426951B (en) * | 2023-03-17 | 2023-10-27 | 湘南学院 | Leaf-like array amorphous phase nickel oxide/nickel foam electrode and preparation method and application thereof |
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