CN116180128A - Self-supporting non-noble metal electrocatalyst material, and preparation method and application thereof - Google Patents
Self-supporting non-noble metal electrocatalyst material, and preparation method and application thereof Download PDFInfo
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 87
- 239000000463 material Substances 0.000 title claims abstract description 76
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 168
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 85
- 239000006260 foam Substances 0.000 claims abstract description 79
- 239000000243 solution Substances 0.000 claims abstract description 54
- 239000011259 mixed solution Substances 0.000 claims abstract description 46
- 239000004094 surface-active agent Substances 0.000 claims abstract description 39
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 23
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 150000001868 cobalt Chemical class 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000009210 therapy by ultrasound Methods 0.000 claims description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 12
- -1 iron ions Chemical class 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical group C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 8
- 229940081974 saccharin Drugs 0.000 claims description 8
- 235000019204 saccharin Nutrition 0.000 claims description 8
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 8
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 3
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 3
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 claims description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 3
- VXWSFRMTBJZULV-UHFFFAOYSA-H iron(3+) sulfate hydrate Chemical compound O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VXWSFRMTBJZULV-UHFFFAOYSA-H 0.000 claims description 3
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000001965 increasing effect Effects 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000001291 vacuum drying Methods 0.000 description 11
- 150000002632 lipids Chemical class 0.000 description 10
- 238000010008 shearing Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 238000004502 linear sweep voltammetry Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- KGWWEXORQXHJJQ-UHFFFAOYSA-N [Fe].[Co].[Ni] Chemical compound [Fe].[Co].[Ni] KGWWEXORQXHJJQ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229940068911 chloride hexahydrate Drugs 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002091 nanocage Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
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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
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- 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
- 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
-
- 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
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
-
- 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
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
-
- 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 relates to the technical field of electrocatalytic materials, in particular to a self-supporting non-noble metal electrocatalytic material, and a preparation method and application thereof. The preparation method of the self-supporting non-noble metal electrocatalyst material comprises the following steps: obtaining a raw material solution: preparing a mixed solution from ferric salt and cobalt salt, soaking foam nickel in the mixed solution, and preparing a surfactant into a surfactant solution; hydrothermal reaction: mixing the mixed solution soaked with the foam nickel with the surfactant solution, and performing hydrothermal reaction after mixing. According to the invention, the NiCoFe-LDH ternary OER electrocatalyst with high activity and high current density can be synthesized in situ on the three-dimensional porous foam nickel by a simple one-step hydrothermal method, and the foam nickel can be used as a carrier of the electrocatalyst and can also provide a nickel source for synthesis, so that the close contact and conductivity between the electrocatalyst and the foam nickel are enhanced, the specific surface area of the electrocatalyst is increased, and more active sites are exposed.
Description
Technical Field
The invention relates to the technical field of electrocatalytic materials, in particular to a self-supporting non-noble metal electrocatalytic material, and a preparation method and application thereof.
Background
With the rapid development of society, the demand for global fossil fuels is increasing, and people inevitably raise concerns about energy shortage and environmental deterioration. To cope with the above problems, researchers have put a great deal of effort on renewable energy conversion and storage technologies, such as electrolyzed water and metal-air batteries.
Electrolytic water to produce hydrogen is considered an ideal, clean technique for producing high purity hydrogen. The electrolytic water is divided into two half reactions, cathodic Hydrogen Evolution (HER) and anodic Oxygen Evolution (OER), respectively. Among these, the complex four electron transfer process of OER and the large overpotential, slow kinetics are considered as bottlenecks for electrolysis of water, where intermediates such as OH and OOH are the main causes of energy and efficiency losses. Therefore, synthesizing an efficient OER electrocatalyst to reduce the overpotential required for electrolyzed water is very important for practical hydrogen production.
At present, noble metal oxide IrO 2 And RuO (Ruo) 2 Is widely regarded as a benchmark catalyst for OER, but its large-scale use is still significantly hampered by the scarcity of these metals and the associated high costs. For this reason, it is highly desirable to develop other elemental OER electrocatalysts that are cost effective and strong based on the abundance of earth elements. Among them, the two-dimensional LDH of the first row transition metal element (including Ni, co, and Fe) is a promising OER catalyst, which has advantages of simple synthesis process, low cost, high catalytic performance, and the like. However, LDHs themselves have poor conductivity and cannot sufficiently expose active sites, and generated bubbles adhere to the surface of the catalyst and are difficult to be exported in solution, thus degrading the performance and stability of the catalyst. Chinese patent document CN115386908A discloses an iron-cobalt-nickel double hydroxide nanocage electrocatalytic oxygen evolution material and a preparation method thereof, which can provide more exposed active sites and enhanced electron transport capability, but has very strict requirements on precursors and a more complex preparation method.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the existing preparation method of the NiCoFe-LDH-based electrocatalyst is harsh and complex in condition, so as to provide a self-supporting non-noble metal electrocatalyst material, and a preparation method and application thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method of preparing a self-supporting non-noble metal electrocatalyst material comprising:
obtaining a raw material solution: preparing a mixed solution from ferric salt and cobalt salt, soaking foam nickel in the mixed solution, and preparing a surfactant into a surfactant solution;
hydrothermal reaction: mixing the mixed solution soaked with the foam nickel with the surfactant solution, and performing hydrothermal reaction after mixing.
Preferably, the concentration of iron ions in the mixed solution is 0.2-0.34 mol/L, and the concentration of cobalt ions is 0.16-0.32 mol/L;
and/or the solvent used in the mixed solution is water or/and ethanol.
Preferably, the iron salt is ferric nitrate nonahydrate [ Fe (NO) 3 ) 3 ·9H 2 O]Ferric chloride hexahydrate (FeCl) 3 •6H 2 O), ferric sulfate hydrate [ Fe 2 (SO 4 ) 3 •xH 2 O]Preferably ferric nitrate nonahydrate;
and/or the cobalt salt is cobalt nitrate hexahydrate (Co (NO) 3 ) 2 ·6H 2 O]Cobalt chloride hexahydrate (CoCl) 2 •6H 2 O), cobalt sulphate heptahydrate (CoSO) 4 •7H 2 O), cobalt acetate tetrahydrate [ (CH) 3 COO) 2 Co•4H 2 O]Cobalt acetate [ (CH) 3 COO) 2 Co]Preferably cobalt nitrate hexahydrate.
Preferably, the surfactant is saccharin or/and cetyltrimethylammonium bromide;
and/or the concentration of the surfactant solution is 0.64 mol/L;
and/or the solvent of the surfactant solution is an organic solvent.
Preferably, the organic solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone and methanol, and preferably N, N-dimethylformamide.
Preferably, the volume ratio of the mixed solution to the surfactant solution is 3:20.
preferably, the foam nickel is also pretreated before soaking;
the pretreatment process comprises the following steps: firstly slicing the foam nickel, then immersing the foam nickel into hydrochloric acid, acetone and ethanol solution in sequence, respectively carrying out ultrasonic treatment, and finally carrying out drying treatment;
and/or the soaking time of the foam nickel in the mixed solution is 15-75 min, namely the soaking time of the foam nickel in the mixed solution can be 15min, 30 min, 60 min, 75 min, preferably 60 min;
and/or the duration of continuous soaking and magnetic stirring after mixing the surfactant solution and the mixed solution is 15-60 min, i.e. the duration of continuous soaking and magnetic stirring after mixing the surfactant solution and the mixed solution can be 15min, 30 min, 45 min, 60 min, preferably 30 min.
Preferably, the temperature of the hydrothermal reaction is 105-135 ℃ and the duration is 7-10 hours;
and/or, washing and drying are also carried out after the hydrothermal reaction.
The invention also provides a self-supporting non-noble metal electrocatalyst material, which is prepared by the preparation method of the self-supporting non-noble metal electrocatalyst material.
The invention also provides application of the self-supporting non-noble metal electrocatalyst material in electrocatalytic oxygen evolution.
In the invention, the specific process of pretreatment is as follows: firstly shearing foam nickel into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipids, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain the pretreated foam nickel.
In the invention, the specific steps of washing and drying after the hydrothermal reaction are as follows: washing with water and ethanol for 3 times, and vacuum drying at 80deg.C overnight.
The technical scheme of the invention has the following advantages:
1. a method of preparing a self-supporting non-noble metal electrocatalyst material comprising: obtaining a raw material solution: preparing a mixed solution from ferric salt and cobalt salt, soaking foam nickel in the mixed solution, and preparing a surfactant into a surfactant solution; hydrothermal reaction: mixing the mixed solution soaked with the foam nickel with the surfactant solution, and performing hydrothermal reaction after mixing. According to the invention, the NiCoFe-LDH ternary OER electrocatalyst with high activity and high current density can be synthesized in situ on the three-dimensional porous foam nickel by a simple one-step hydrothermal method, the foam nickel can be used as a carrier of the electrocatalyst, a nickel source can be provided for synthesis, the close contact and conductivity between the electrocatalyst and the foam nickel are enhanced, the specific surface area of the electrocatalyst is increased, more active sites are exposed, an adhesive is not needed to fix the electrocatalyst on the foam nickel, the electrocatalyst is prevented from falling off under high current, and finally, the electrocatalyst material has excellent OER performance.
2. The self-supporting non-noble metal electrocatalyst material has good hydrophilicity, and can enable electrolyte solution to be quickly immersed, thereby providing more OH capable of participating in reaction - In addition, the gas-permeable porous material also has stronger gas-permeable property, and can rapidly guide away bubbles generated in the OER process, and avoid the bubbles covering active sites, thereby enhancing mass transfer in the OER process.
3. The preparation method of the self-supporting non-noble metal electrocatalyst material has the advantages of wide sources of transition metals Ni, fe and Co in the synthetic raw materials, low cost and simple synthesis process, provides a new thought for designing the synthesis of the high-efficiency self-supporting non-noble metal OER electrocatalyst, and also provides a new thought for solving the problem of sustainable development of the current energy crisis (green hydrogen energy).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is an X-ray diffraction (XRD) spectrum of the electrocatalyst materials of examples 1-7 and comparative example 1 and blank nickel foam;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the electrocatalyst material prepared in comparative example 1;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the electrocatalyst material prepared in example 1, wherein (a) image, (b) image is a front scan of the electrocatalyst material, and (c) image is a cross-sectional view of the electrocatalyst material;
FIG. 4 is a Transmission Electron Microscope (TEM) image of the electrocatalyst material prepared in example 1;
FIG. 5 is an X-ray photoelectron spectrum (XPS) chart of the electrocatalyst material prepared in example 1, wherein (a) is a full spectrum, (b) is a Ni 2p spectrum, (c) is a Fe 2p spectrum, and (d) is a Co 2p spectrum;
FIG. 6 is a Linear Sweep Voltammetry (LSV) plot of the oxygen evolution reaction for the electrocatalyst materials prepared in example 1 and comparative example 1, comparative example 2 and blank nickel foam;
fig. 7 is a graph showing a Contact Angle (CA) test of the electrocatalyst material prepared in example 1, wherein (a) is a graph showing a contact angle image of the electrocatalyst material in air at 0 s, (b) is a graph showing a contact angle image of the electrocatalyst material in air at 50 ns, and (c) is a graph showing a contact angle image of the electrocatalyst material in 1M KOH;
FIG. 8 is a chart showing the chronopotentiometric measurements of the electrocatalyst material prepared in example 1 in 1M KOH.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.35 mmol of ferric nitrate nonahydrate and 0.35 mmol of cobalt nitrate hexahydrate were added to 1.5 mL of H 2 Preparing mixed solution in O;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL of N, N-dimethylformamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 60 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 30 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 2
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.48 mmol of ferric chloride hexahydrate and 0.48 mmol of cobalt chloride hexahydrate were added to 1.5 mL of H 2 Preparing mixed solution in O;
3) 6.4 mmol of cetyltrimethylammonium bromide was weighed and dissolved in 10 mL of N, N-dimethylacetamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 15min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 15min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 3
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.15 mmol of ferric sulfate hydrate and 0.3 mmol of cobalt sulfate heptahydrate are added to 1.5 mL of H 2 Preparing mixed solution in O;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL of N-methylpyrrolidone to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 75 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 45 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 4
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.5 mmol of ferric nitrate nonahydrate and 0.25 mmol of cobalt acetate tetrahydrate are added to 1.5 mL of H 2 Preparing mixed solution in O;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL methanol to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 30 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 60 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 5
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.35 mmol of ferric nitrate nonahydrate and 0.35 mmol of cobalt acetate were added to 0.75 mL of H 2 Preparing mixed solution from O and 0.75 mL ethanol;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL of N, N-dimethylformamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 60 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 30 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 6
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.35 mmol of ferric nitrate nonahydrate and 0.35 mmol of cobalt nitrate hexahydrate were added to 1.5 mL of H 2 Preparing mixed solution in O;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL of N, N-dimethylformamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 60 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 30 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 105 ℃ for 10 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Example 7
A preparation method of a self-supporting non-noble metal electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.35 mmol of ferric nitrate nonahydrate and 0.35 mmol of cobalt nitrate hexahydrate were added to 1.5 mL of H 2 Preparing mixed solution in O;
3) 6.4 mmol of cetyltrimethylammonium bromide was weighed and dissolved in 10 mL of N, N-dimethylformamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the mixed solution of the step 2) for 60 min, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature, continuously immersing for 30 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 135 ℃ for 7 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and drying in vacuum at 80 ℃ overnight to obtain the NiCoFe-LDH electrocatalyst material.
Comparative example 1
A method for preparing a NiCo-LDH electrocatalyst material comprising the steps of:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing in 3 mol/L hydrochloric acid solution for ultrasonic treatment for 15min to remove surface oxides, immersing in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing in ethanol for ultrasonic treatment for 5min, and finally vacuum drying in an oven at 60 ℃ for 4h to obtain pretreated foam nickel;
2) 0.35 mmol of Co (NO 3 ) 2 ·6H 2 O was added to 1.5 mL H 2 Preparing cobalt salt solution in O;
3) Weighing 6.4 mmol of saccharin, and dissolving in 10 mL of N, N-dimethylformamide to prepare a surfactant solution;
4) Immersing the foam nickel pretreated in the step 1) into the cobalt salt solution in the step 2) to soak 1 h, adding the surfactant solution prepared in the step 3), magnetically stirring at room temperature and continuously soaking for 30 min, transferring the mixed solution and the foam nickel into a polytetrafluoroethylene reaction kettle of 25 mL, carrying out hydrothermal reaction at 125 ℃ for 8 h, finally cooling to room temperature, taking out the reacted foam nickel, washing with ethanol and deionized water for 3 times respectively, and vacuum drying at 80 ℃ for overnight to obtain the NiCo-LDH electrocatalyst material.
Comparative example 2
RuO (Ruo) device 2 The preparation method of the NF electrocatalyst material comprises the following steps:
1) Firstly shearing foam nickel with the thickness of 1.0 mm into 1.5 cm multiplied by 3 cm, immersing the foam nickel in a hydrochloric acid solution with the concentration of 3 mol/L for ultrasonic treatment for 15min to remove surface oxides, immersing the foam nickel in acetone for ultrasonic treatment for 10 min to remove surface lipid, immersing the foam nickel in ethanol for ultrasonic treatment for 5min, and finally drying the foam nickel in an oven with the temperature of 60 ℃ for 4h in vacuum to obtain pretreated foam nickel;
2) Weighing 4.5 mg RuO respectively 2 And 436.5 mu L of isopropanol, 450 mu L of deionized water and 13.5 mu L Nafion solution, and carrying out ultrasonic treatment for 60 min after mixing to prepare a uniform suspension;
3) Weighing 450mL of the suspension prepared in the step 2), dividing into 4 parts, namely 135 mu L, 135 mu L and 45 mu L, sequentially dripping the parts onto the foam nickel pretreated in the step 1), drying for 45 min after each dripping, and adding RuO 2 The mass loading of the catalyst on the nickel foam was controlled at about 0.5 mg cm -2 To obtain RuO 2 An NF electrocatalyst material.
Test case
The 1 mol/L KOH solution used at present is used as electrolyte, an electrochemical workstation (Shanghai Chenhua CHI 660E) is adopted, under a three-electrode system, the electrocatalyst materials prepared in the example 1 and the comparative example 2 and blank foam nickel are respectively used as working electrodes (the size is 1.5 cm multiplied by 0.5 cm, and the effective exposure area is 0.5 cm 2 ) The platinum sheet is used as an auxiliary electrode, hg/HgO is used as a reference electrode, the (linear sweep voltammetry) LSV test (the scanning range is 0-1V, the quick sweep is firstly carried out for 25 circles at 50 mV/s for activation, then the LSV slow sweep is carried out for 5 mV/s at 1-0V) is carried out at normal temperature, the data are compensated by adopting 90% iR, the test result is shown in figure 6, wherein, the overpotential=E RHE -1.23; the stability of the electrocatalyst material prepared in example 1 was tested using the chronoamometry test method in an electrochemical workstation, the test results being shown in fig. 8;
as can be seen from FIG. 6, compared with NiCo-LDH, NF, ruO 2 for/NF, the OER performance of the NiCoFe-LDH electrocatalyst material prepared according to the invention is optimal when the current density is 10 mA cm -2 At the time, the NiCoFe-LDH electrocatalyst material had an overpotential of 192 mV and a current density of 100 mA cm -2 At the time of overpotential 261 mV, current density was 200 mA cm -2 When the over potential is 280 mV, the current density is 900 mA cm -2 At the time, the overpotential was 343 mV; as can be seen from FIG. 8, the NiCoFe-LDH electrocatalyst material prepared according to the invention was prepared at 200 mA cm -2 Can stably work 200 and h and has good stability.
Fig. 1 shows X-ray diffraction (XRD) spectra of the electrocatalyst materials of examples 1 to 7 and comparative example 1 and blank nickel foam, and as can be seen from fig. 1, the electrocatalyst materials prepared in comparative example 1 and example 1 to example 7 all have characteristic peaks of metallic Ni at 2θ=44.5 °, 2θ=51.8 °, and 2θ=76.4 °, whereas the NiCoFe-LDH electrocatalyst materials prepared in examples 1 to 7 have characteristic peaks at 2θ=11.4 ° corresponding to the (003) lattice in the LDH material, which proves that the present invention synthesizes the NiCoFe-LDH electrocatalyst material.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the NiCo-LDH electrocatalyst material prepared in comparative example 1, and it is understood from fig. 2 that the nano-sheets in the NiCo-LDH electrocatalyst material prepared in comparative example 1 are thicker, and the large size results in less exposure of active sites, so that the electrocatalytic activity of the NiCo-LDH electrocatalyst material is low.
FIG. 3 is a Scanning Electron Microscope (SEM) image of the NiCoFe-LDH electrocatalyst material prepared in example 1, and from FIGS. 3 (a) and (b), it can be seen that the nano-sheets in the NiCoFe-LDH electrocatalyst material have small size and form nanoflower, can expose more active sites, and have high electrocatalytic activity; from fig. 3 (c), it can be seen that the NiCoFe-LDH electrocatalyst is tightly bound to the support Nickel Foam (NF), thereby enhancing the electrical conductivity of the catalyst and reducing the shedding of the electrocatalyst during OER.
Fig. 4 is a Transmission Electron Microscope (TEM) image of the NiCoFe-LDH electrocatalyst material prepared in example 1, and it can be seen from fig. 4 that the crystalline phase and the amorphous phase of the NiCoFe-LDH electrocatalyst material prepared in the invention are combined, and the crystalline phase has high conductivity, and abundant unsaturated sites exist in the amorphous phase, so that the design further promotes the improvement of the OER performance of the electrocatalyst.
FIG. 5 is an X-ray photoelectron spectrum (XPS) of the NiCoFe-LDH electrocatalyst material prepared in example 1, wherein the main non-noble metal elements in the NiCoFe-LDH electrocatalyst material are Ni, fe and Co, and the valence states of the Ni, fe and Co elements are +2.
Fig. 7 is a graph of Contact Angle (CA) measurements of the NiCoFe-LDH electrocatalyst material prepared in example 1, where in fig. 7 (a) and (b) it is known that the NiCoFe-LDH electrocatalyst material has a contact angle of 88.5 ° at 0 s in air, and at 50 ns, the NiCoFe-LDH electrocatalyst material is fully wetted, exhibiting good hydrophilicity, favoring adequate wetting of the electrolyte, and in fig. 7 (c) it is known that the NiCoFe-LDH electrocatalyst material has a contact angle of 159.1 ° in 1M KOH, exhibits superhydrophobicity, favoring the generated gas to rapidly leave the electrocatalyst material, avoiding aggregation of bubbles, and improving mass transfer during OER.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A method of preparing a self-supporting non-noble metal electrocatalyst material comprising:
obtaining a raw material solution: preparing a mixed solution from ferric salt and cobalt salt, soaking foam nickel in the mixed solution, and preparing a surfactant into a surfactant solution;
hydrothermal reaction: mixing the mixed solution soaked with the foam nickel with the surfactant solution, and performing hydrothermal reaction after mixing.
2. The preparation method according to claim 1, wherein the concentration of iron ions in the mixed solution is 0.2-0.34 mol/L, and the concentration of cobalt ions is 0.16-0.32 mol/L;
and/or the solvent used in the mixed solution is water or/and ethanol.
3. The preparation method according to claim 1 or 2, wherein the iron salt is at least one of ferric nitrate nonahydrate, ferric chloride hexahydrate, ferric sulfate hydrate;
and/or the cobalt salt is at least one of cobalt nitrate hexahydrate, cobalt chloride hexahydrate, cobalt sulfate heptahydrate, cobalt acetate tetrahydrate and cobalt acetate.
4. The preparation method according to claim 1 or 2, wherein the surfactant is saccharin or/and cetyltrimethylammonium bromide;
and/or the concentration of the surfactant solution is 0.64 mol/L;
and/or the solvent of the surfactant solution is an organic solvent.
5. The method according to claim 4, wherein the organic solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, and methanol.
6. The preparation method according to claim 1 or 2, wherein the volume ratio of the mixed solution to the surfactant solution is 3:20.
7. the method of claim 1 or 2, wherein the nickel foam is further pretreated prior to soaking;
the pretreatment process comprises the following steps: firstly slicing the foam nickel, then immersing the foam nickel into hydrochloric acid, acetone and ethanol solution in sequence, respectively carrying out ultrasonic treatment, and finally carrying out drying treatment;
and/or the soaking time of the foam nickel in the mixed solution is 15-75 min;
and/or mixing the surfactant solution and the mixed solution, and then continuously soaking and magnetically stirring for 15-60 min.
8. The preparation method according to claim 1 or 2, wherein the hydrothermal reaction is carried out at a temperature of 105-135 ℃ for 7-10 hours;
and/or, washing and drying are also carried out after the hydrothermal reaction.
9. A self-supporting non-noble metal electrocatalyst material, characterized in that it is prepared by a method for preparing a self-supporting non-noble metal electrocatalyst material according to any one of claims 1 to 8.
10. Use of the self-supporting non-noble metal electrocatalyst material according to claim 9 for electrocatalytic oxygen evolution.
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