CN117996094A - Ce-NiCo2O4C@Ni foam electrode and preparation method and application thereof - Google Patents
Ce-NiCo2O4C@Ni foam electrode and preparation method and application thereof Download PDFInfo
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- CN117996094A CN117996094A CN202410052804.XA CN202410052804A CN117996094A CN 117996094 A CN117996094 A CN 117996094A CN 202410052804 A CN202410052804 A CN 202410052804A CN 117996094 A CN117996094 A CN 117996094A
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- foam
- nico
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- polytetrafluoroethylene lining
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- 239000006260 foam Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910003266 NiCo Inorganic materials 0.000 claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- -1 polytetrafluoroethylene Polymers 0.000 claims description 20
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 20
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052684 Cerium Inorganic materials 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract description 2
- 239000000446 fuel Substances 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8605—Porous electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention provides a Ce-NiCo 2O4/C@Ni foam electrode and a preparation method and application thereof, and relates to the technical field of electrode materials. According to the invention, ce-Co 2Ni(OH)x/NF is obtained by hydrothermally doping Ce, co and the like on foam nickel; and then mixing the dimethyl imidazole solution with Ce-Co 2Ni(OH)x/NF, carrying out hydrothermal treatment, and roasting to obtain the Ce-NiCo 2O4/C@Ni foam. The Ce-NiCo 2O4/C@Ni foam electrode has the characteristics of large specific surface area and good electronic conductivity, can effectively improve the rapid permeation of electrolyte and the conduction of electrons, can promote the electroreduction reaction of H 2O2, and greatly improves the electroreduction performance and the utilization rate of H 2O2.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a Ce-NiCo 2O4/C@Ni foam electrode, and a preparation method and application thereof.
Background
Hydrogen peroxide (H 2O2) is an environment-friendly renewable oxidant and has wide application in the fields of environmental remediation, fine chemical industry, electronic industry and the like. The H 2O2 electroreduction is a two-electron process, has better electroreduction activity than the O 2 reduced four-electron process, can not cause catalyst poisoning, is liquid at normal temperature, is convenient to store and transport, and is more suitable for anaerobic environments such as space water. H 2O2 thus exhibits potential for use as a fuel cell oxidant in place of O 2. The self-decomposition problem of H 2O2 causes a decrease in fuel utilization, see equations (1) and (2), resulting in a decrease in long-term operation stability of the fuel cell.
H2O2+2e-→2OH- (1)
2H2O2→2H2O+O2 (2)
Disclosure of Invention
In view of this, the present invention provides a Ce-NiCo 2O4/C@Ni foam electrode and a method for preparing the same, which are used for improving the electrochemical performance of a fuel cell. According to the invention, ce-Co 2Ni(OH)x/NF is obtained by hydrothermally doping Ce, co and Ni on foam nickel; and then mixing the dimethyl imidazole solution with Ce-Co 2Ni(OH)x/NF, carrying out hydrothermal treatment, and roasting to obtain the Ce-NiCo 2O4/C@Ni foam,Ce-NiCo2O4/C@Ni foam. The Ce-NiCo 2O4/C@Ni foam electrode has the characteristics of large specific surface area and good electronic conductivity, can effectively improve the rapid permeation of electrolyte and the conduction of electrons, can promote the electroreduction reaction of H 2O2, and greatly improves the electroreduction performance and the utilization rate of H 2O2.
The invention is realized by adopting the following technical scheme:
The invention provides a preparation method of a Ce-NiCo 2O4/C@Ni foam electrode, which comprises the following steps:
(1) Dissolving cerium nitrate, cobalt nitrate, nickel nitrate, urea and ammonium fluoride in water to obtain electrolyte;
(2) Placing foam nickel into a polytetrafluoroethylene lining, transferring the electrolyte into the polytetrafluoroethylene lining in which the foam nickel is placed, then placing the polytetrafluoroethylene lining into a reaction kettle, carrying out hydrothermal treatment at 100-140 ℃ for 4-8 hours, naturally cooling to room temperature, taking out the hydrothermal foam nickel, washing the surface with deionized water and alcohol, and carrying out vacuum drying to obtain Ce-Co 2Ni(OH)x/NF;
(3) Dissolving dimethyl imidazole in a methanol solution to obtain a dimethyl imidazole solution, then placing the dried foam nickel in the step (2) in a polytetrafluoroethylene lining, transferring the dimethyl imidazole solution to the polytetrafluoroethylene lining in which the dried foam nickel is placed, placing the polytetrafluoroethylene lining in a reaction kettle, carrying out hydrothermal treatment at 80-120 ℃ for 4-6 h, naturally cooling to room temperature, taking out the foam nickel after secondary hydrothermal treatment, alternately flushing with alcohol and deionized water, and drying;
(4) And (3) placing the foam nickel dried in the step (3) into a muffle furnace, heating to 300-400 ℃, and preserving heat for 1-3 h to obtain the Ce-NiCo 2O4/C@Ni foam.
Preferably, the mass concentrations of cerium nitrate, cobalt nitrate, nickel nitrate, urea and ammonium fluoride in the electrolyte are 1g/L, 19.4g/L, 9.7g/L, 30g/L and 14.8g/L respectively.
Preferably, the nickel foam has dimensions of 2cm by 3cm.
Preferably, the mass concentration of the dimethylimidazole is 8g/L-12g/L, and the concentration of the methanol solution is 30% -70%.
Preferably, the drying temperature in the step (3) is 60-80 ℃ and the drying time is 8-14 h.
Preferably, the temperature rise rate is 2 ℃ min -1.
Preferably, the polytetrafluoroethylene lining has a specification of 50mL.
The Ce-NiCo 2O4/C@Ni foam catalyst is used as a working electrode, a carbon rod is used as a counter electrode, and Ag/AgCl is used as a reference electrode.
A Ce-NiCo 2O4/C@Ni foam electrode is prepared by the method.
The application of the Ce-NiCo 2O4/C@Ni foam electrode applies the Ce-NiCo 2O4/C@Ni foam electrode to a hydrogen peroxide electroreduction reaction, and comprises the following steps:
Mixing sodium hydroxide with the concentration of 1 mol.L -1-3mol·L-1 and hydrogen peroxide with the concentration of 0.3 mol.L -1-0.70mol·L-1, and dissolving the mixture in water to obtain hydrogen peroxide electrolyte; and placing the Ce-NiCo 2O4/C@Ni foam electrode serving as a working electrode in the hydrogen peroxide electrolyte, and performing electroreduction reaction under the voltage of-0.2 to-0.8 Vvs.
Compared with the prior art, the invention has the following beneficial effects:
1. The invention improves the conductivity through the doping of Ce, and the Ce has two oxidation states Ce 3+ and Ce 4+, can change the electronic structure in the transition metal oxide, is beneficial to breaking O-O bond in H 2O2, and further promotes the occurrence of electric reduction reaction.
2. According to the invention, the specific surface area of the electrode is increased by adding the organic ligand dimethyl imidazole, so that the electrode is contacted with electrolyte, the reaction rate is improved, meanwhile, a conductive carbon network is formed in the carbonization process of the organic ligand dimethyl imidazole, and a large number of active sites are exposed while the conductivity is increased.
Drawings
FIG. 1 is an SEM characterization of Ce-Co 2Ni(OH)x/NF;
FIG. 2 is an XRD pattern for Ce-NiCo 2O4/C@Ni foam;
FIG. 3 is an SEM characterization of Ce-NiCo 2O4/C@Ni foam;
FIG. 4 is a timing current test of Ce-NiCo 2O4/C@Ni foam electrode.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
A preparation method of a Ce-NiCo 2O4/C@Ni foam electrode comprises the following specific steps:
1. Weighing 0.03gCe(NO3)3·6H2O,0.582gCo(NO3)2·6H2O,0.291gNi(NO3)2·6H2O,0.9gCO(NH2)2,0.444gNH4F, dissolving in 30mL of deionized water, and fully stirring to obtain electrolyte;
2. Taking 2cm multiplied by 3cm of foam nickel, vertically inserting the foam nickel into 50mL of polytetrafluoroethylene lining, transferring electrolyte into the polytetrafluoroethylene lining inserted with the foam nickel, then placing the polytetrafluoroethylene lining into a reaction kettle, carrying out hydrothermal treatment at 120 ℃ for 6 hours, naturally cooling to room temperature, taking out the hydrothermal foam nickel, washing the surface with deionized water and alcohol, and then carrying out vacuum drying to obtain Ce-Co 2Ni(OH)x/NF, wherein the SEM representation of Ce-Co 2Ni(OH)x/NF is shown in FIG. 1;
3.1 g of dimethyl imidazole is weighed and dissolved in a methanol solution with the concentration of 50 percent, and the mixture is fully stirred; and (3) vertically inserting the foam nickel dried in the step (2) into 50mL of polytetrafluoroethylene lining, transferring the dimethyl imidazole solution into the polytetrafluoroethylene lining inserted with the dried foam nickel, putting the polytetrafluoroethylene lining into a reaction kettle, carrying out hydrothermal treatment at 100 ℃ for 5h, taking out the foam nickel after the secondary hydrothermal treatment after naturally cooling to room temperature, alternately flushing with alcohol and deionized water, and carrying out vacuum drying at 60 ℃ for 12h.
And (3) placing the foam nickel dried in the step (3) into a muffle furnace, and raising the temperature to 350 ℃ at a heating rate of 2 ℃/min for 2h, so as to obtain the Ce-NiCo 2O4/C@Ni foam, as shown by the XRD pattern of the Ce-NiCo 2O4/C@Ni foam in figure 2 and the SEM characterization of the Ce-NiCo 2O4/C@Ni foam in figure 3.
The Ce-NiCo 2O4/C@Ni foam electrode prepared in example 1 is used as a working electrode, ag/AgCl is used as a reference electrode, a carbon rod is used as a counter electrode, and the counter electrode is placed in hydrogen peroxide electrolyte to prepare a three-electrode system, wherein the preparation method of the hydrogen peroxide electrolyte is as follows:
NaOH and H 2O2 were dissolved in water to give an H 2O2 electrolyte having a NaOH concentration of 3 mol.L -1 and an H 2O2 concentration of 0.70 mol.L -1.
The three electrode system is subjected to electroreduction reaction under the voltage of minus 0.6Vvs.Ag/AgCl, and the timing current density is 480 mA.cm -2, as shown in the timing current test of the Ce-NiCo 2O4/C@Ni foam electrode in FIG. 4.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the Ce-NiCo 2O4/C@Ni foam electrode is characterized by comprising the following steps of:
(1) Dissolving cerium nitrate, cobalt nitrate, nickel nitrate, urea and ammonium fluoride in water to obtain electrolyte;
(2) Placing foam nickel into a polytetrafluoroethylene lining, transferring the electrolyte into the polytetrafluoroethylene lining in which the foam nickel is placed, then placing the polytetrafluoroethylene lining into a reaction kettle, carrying out hydrothermal treatment at 100-140 ℃ for 4-8 hours, naturally cooling to room temperature, taking out the hydrothermal foam nickel, washing the surface with deionized water and alcohol, and carrying out vacuum drying to obtain Ce-Co 2Ni(OH)x/NF;
(3) Dissolving dimethyl imidazole in a methanol solution to obtain a dimethyl imidazole solution, then placing the dried foam nickel in the step (2) in a polytetrafluoroethylene lining, transferring the dimethyl imidazole solution to the polytetrafluoroethylene lining in which the dried foam nickel is placed, placing the polytetrafluoroethylene lining in a reaction kettle, carrying out hydrothermal treatment at 80-120 ℃ for 4-6 h, naturally cooling to room temperature, taking out the foam nickel after secondary hydrothermal treatment, alternately flushing with alcohol and deionized water, and drying;
(4) And (3) placing the foam nickel dried in the step (3) into a muffle furnace, heating to 300-400 ℃, and preserving heat for 1-3 h to obtain Ce-NiCo 2O4/C@Ni foam.
2. The method for preparing the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the mass concentrations of cerium nitrate, cobalt nitrate, nickel nitrate, urea and ammonium fluoride in the electrolyte are 1g/L, 19.4g/L, 9.7g/L, 30g/L and 14.8g/L respectively.
3. The method for producing a Ce-NiCo 2O4/c@ni foam electrode according to claim 1, wherein the size of the nickel foam is 2cm x 3cm.
4. The preparation method of the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the mass concentration of the dimethylimidazole is 8g/L-12g/L, and the concentration of the methanol solution is 30% -70%.
5. The method for preparing the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the drying temperature in the step (3) is 60-80 ℃ and the drying time is 8-14 h.
6. The method for preparing the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the heating rate is 2 ℃ min -1.
7. The method for preparing the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the specification of the polytetrafluoroethylene lining is 50mL.
8. The method for preparing the Ce-NiCo 2O4/C@Ni foam electrode according to claim 1, wherein the Ce-NiCo 2O4/C@Ni foam catalyst is a working electrode, a carbon rod is a counter electrode, and Ag/AgCl is a reference electrode.
9. A Ce-NiCo 2O4/c@ni foam electrode, characterized in that it is prepared by the method of any one of claims 1 to 8.
10. The use of a Ce-NiCo 2O4/c@ni foam electrode according to claim 9, wherein the Ce-NiCo 2O4/c@ni foam electrode is used in a hydrogen peroxide electroreduction reaction. The method comprises the following steps:
Mixing sodium hydroxide with the concentration of 1 mol.L -1-3mol·L-1 and hydrogen peroxide with the concentration of 0.3 mol.L -1-0.70mol·L-1, and dissolving the mixture in water to obtain hydrogen peroxide electrolyte; and placing the Ce-NiCo 2O4/C@Ni foam electrode serving as a working electrode in the hydrogen peroxide electrolyte, and performing electroreduction reaction under the voltage of-0.2 to-0.8 Vvs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410052804.XA CN117996094A (en) | 2024-01-12 | 2024-01-12 | Ce-NiCo2O4C@Ni foam electrode and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410052804.XA CN117996094A (en) | 2024-01-12 | 2024-01-12 | Ce-NiCo2O4C@Ni foam electrode and preparation method and application thereof |
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| CN117996094A true CN117996094A (en) | 2024-05-07 |
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| CN202410052804.XA Pending CN117996094A (en) | 2024-01-12 | 2024-01-12 | Ce-NiCo2O4C@Ni foam electrode and preparation method and application thereof |
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| CN (1) | CN117996094A (en) |
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- 2024-01-12 CN CN202410052804.XA patent/CN117996094A/en active Pending
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