CN111939939A - Method for synthesizing high-temperature-resistant and strong-alkali-resistant efficient NiFeS-OH oxygen evolution catalyst in one step - Google Patents
Method for synthesizing high-temperature-resistant and strong-alkali-resistant efficient NiFeS-OH oxygen evolution catalyst in one step Download PDFInfo
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- CN111939939A CN111939939A CN202010819758.3A CN202010819758A CN111939939A CN 111939939 A CN111939939 A CN 111939939A CN 202010819758 A CN202010819758 A CN 202010819758A CN 111939939 A CN111939939 A CN 111939939A
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000001301 oxygen Substances 0.000 title claims abstract description 44
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000003513 alkali Substances 0.000 title claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000243 solution Substances 0.000 claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 7
- HVENHVMWDAPFTH-UHFFFAOYSA-N iron(3+) trinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HVENHVMWDAPFTH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008096 xylene Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 5
- 239000012044 organic layer Substances 0.000 claims description 5
- 238000001308 synthesis method Methods 0.000 claims 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 1
- -1 iron ions Chemical class 0.000 abstract 1
- 239000006260 foam Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000010287 polarization Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/20—Sulfiding
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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 Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the field of electrocatalysis, and particularly relates to a method for synthesizing a high-temperature-resistant and strong-alkali-resistant high-efficiency NiFeS-OH oxygen evolution catalyst in one step. Soaking foamed nickel in dilute hydrochloric acid, ethanol and distilled water successively for ultrasonic pretreatment, dissolving 0.2-0.5 g of ferric nitrate hexahydrate in a mixed solution of 15mL of distilled water and 5mL of ethylene glycol, dissolving 0.02-0.08 g of sublimed sulfur in 30mL of toluene or xylene solution, mixing the two solutions to obtain a solution with layered interfaces, placing a foamed nickel sheet in the solution, calcining in a muffle furnace, cooling, and washing with distilled water. The method reacts at high temperature, hydroxyl is a coordination group, sublimed sulfur and iron ions grow on the foamed nickel in situ, so that the high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance is prepared, the production environment of high temperature resistance and strong alkali resistance in industrial production is met, the oxygen evolution overpotential is low, and the method has very important significance for environmental protection and resource utilization.
Description
Technical Field
The invention belongs to the field of electrocatalysis, and particularly relates to a method for synthesizing a NiFeS-OH oxygen evolution catalyst by utilizing foamed nickel in one step.
Background
Modern industrial development of all countries in the world is rapid, the demand for energy is continuously increased, the energy crisis is increasingly serious along with the depletion of fossil fuel, and people pay more attention to the development of renewable energy. Since the early 70 s of the last century, hydrogen has been regarded as an ideal clean energy source. The electrolyzed water can obtain hydrogen and oxygen which is necessary for human survival. However, the oxygen evolution half-reaction of electrolyzed water is a kinetic slow reaction due to the complex four-electron process, and the overpotential of the reaction is much higher than that of the hydrogen evolution reaction, which is a main factor limiting the water decomposition efficiency. In recent years, as a half reaction of the electrolytic water reaction, the hydrogen evolution reaction has progressed rapidly; in the oxygen evolution reaction, the catalyst with high-efficiency hydrogen evolution activity is usually a noble metal Ir or Ru-based material, and the preparation of hydrogen and oxygen by industrial electrolysis of water is generally carried out in a high-temperature strong alkali environment, so that the development of the oxygen evolution catalyst with high efficiency, easy obtainment, high temperature resistance and strong alkali resistance has important significance for the development of water electrolysis.
Disclosure of Invention
Aiming at the current situation that the common catalyst in the field of water electrolysis is poor in oxygen evolution catalytic effect in the prior art, the invention provides a method for synthesizing a NiFeS-OH oxygen evolution catalyst in one step.
In order to realize the purpose, the invention adopts the following technical scheme:
the method for synthesizing the NiFeS-OH oxygen evolution catalyst in one step comprises the following steps:
s1, soaking the foamed nickel in dilute hydrochloric acid, ethanol and distilled water in sequence, and performing ultrasonic treatment;
s2, dissolving ferric nitrate hexahydrate in a mixed solution of distilled water and ethylene glycol to obtain a solution A, dissolving sublimed sulfur in a toluene or xylene solution to obtain a solution B, and mixing the solution A and the solution B to obtain a solution with layered interfaces of an organic layer and a water layer;
s3, placing the foam nickel sheet into the solution prepared in the step S2, calcining the foam nickel sheet in a muffle furnace at 120-180 ℃ for 4-6 hours, cooling and washing the foam nickel sheet with distilled water.
In the above technical solution, the specification of the nickel foam sheet used in step S1 is 0.5cm × 0.5cm, 0.8cm × 0.8cm or 1cm × 1 cm.
In the above technical solution, further, in the step S2, the solution a is 0.2 to 0.5g of ferric nitrate hexahydrate dissolved in a mixed solution of 15mL of distilled water and 5mL of ethylene glycol; the solution B is 0.02-0.08 g of sublimed sulfur and is dissolved in 30mL of toluene or xylene solution.
In the above technical solution, further, in the step S3, the raw material is calcined in a muffle furnace at 150 ℃ for 5 hours.
In the above technical solution, further, in the step S1, the volume fraction of the dilute hydrochloric acid is 20%, the ethanol is analytically pure, and the respective ultrasonic treatment time is 15 to 20 minutes.
The invention also provides a high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance, which is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the high-efficiency NiFeS-OH oxygen evolution catalyst synthesized by in-situ growth has excellent performances of high temperature resistance and strong alkali resistance, and can be well applied to the industry.
The invention has simple design and convenient operation, and can realize industrialized mass production.
The NiFeS-OH oxygen evolution catalyst synthesized by the method has low oxygen evolution overpotential, and can improve the resource utilization rate and protect the environment.
Drawings
FIG. 1 shows the layered solution mixed in step 2 of example 1.
FIG. 2 is a LSV polarization curve measured in a 1MKOH solution at room temperature for the NiFeS-OH oxygen evolution catalyst prepared in example 1.
FIG. 3 is a LSV polarization curve measured in a 1MKOH solution at ambient temperature for the NiFeS-OH oxygen evolution catalyst prepared in example 2.
FIG. 4LSV polarization curves measured in 6MKOH solution at 60 ℃ for the NiFeS-OH oxygen evolution catalyst prepared in example 1.
FIG. 5 is a scanning electron micrograph at 200nm of a NiFeS-OH oxygen evolution catalyst material prepared in example 1.
FIG. 6 is a 3 μm scanning electron micrograph of the NiFeS-OH oxygen evolution catalyst material prepared in example 1.
FIG. 7 is a scanning electron micrograph at 10 μm of a NiFeS-OH oxygen evolution catalyst material prepared in example 2.
FIG. 8 is an XPS spectrum of the NiFeS-OH oxygen evolution catalyst material prepared in example 2.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
Example 1
The high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance is synthesized by a one-step method and prepared according to the following steps:
s1, cutting the foam nickel into foam nickel sheets with the specification of 0.5cm multiplied by 0.5cm, soaking the foam nickel sheets in dilute hydrochloric acid with the volume fraction of 20 percent and the concentration of analytically pure ethanol and distilled water respectively, and performing ultrasonic treatment for 15 minutes to remove the inert oxide film on the surface layer of the foam nickel sheets.
S2, weighing 0.5g of ferric nitrate hexahydrate to be dissolved in 15mL of mixed solution of distilled water and 5mL of ethylene glycol, weighing 0.03g of sublimed sulfur to be dissolved in 30mL of toluene solution, and mixing the two solutions to obtain an interface layered solution with an organic layer and an aqueous layer at the same time, wherein the organic layer is the sublimed sulfur solution, and the aqueous layer is the ferric nitrate solution.
S3, placing the foam nickel sheet into the prepared solution, burning the foam nickel sheet in a muffle furnace at 120 ℃ for 6 hours, cooling the foam nickel sheet, and washing the foam nickel sheet with distilled water to obtain the high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance.
The NiFeS-OH oxygen evolution catalyst prepared above is neutralized in 1MKOH solution at normal temperature and in 6MKOH solution at 60 ℃ for testing, and the results are shown in figure 2 and figure 4. As can be seen from the LSV polarization curve of FIG. 2, in 1MKOH solution at 25 ℃ at room temperature, example 1 has a current density of 10mAcm-2The overpotential of oxygen evolution is 135mV, and after 5000 circles of circulating CV curve of the catalyst are measured in 1MKOH solution at normal temperature, the current density is 10mAcm-2The overpotential for oxygen evolution is 132mV, and the stability is extremely high. Simulating the high-temperature strong-alkali environment under the industrial production condition, as can be seen from the LSV polarization curve in FIG. 4, the current density is 500mAcm in 6MKOH solution at 60 DEG C-2The oxygen evolution overpotential is 267mV, and the catalyst is tested in 6MKOH solution at 60 ℃ for 3000 circles of circulating CV curve, and then the current density is 500mAcm-2The oxygen evolution overpotential is 265mV, the stability is very high and is less than the industrial production standard potential.
Example 2
The high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance is synthesized by a one-step method and prepared according to the following steps:
s1, cutting the foam nickel into foam nickel sheets with the specification of 1cm multiplied by 1cm, sequentially using 20% of dilute hydrochloric acid by volume fraction, ethanol with analytical purity concentration and distilled water for soaking, respectively carrying out ultrasonic treatment for 15 minutes, and removing inert oxide films on the surface layers.
S2, weighing 0.2g of ferric nitrate hexahydrate to be dissolved in 15mL of mixed solution of distilled water and 5mL of ethylene glycol, weighing 0.06g of sublimed sulfur to be dissolved in 30mL of xylene solution, and mixing the two solutions to obtain an interface layered solution with an organic layer and a water layer at the same time.
S3, placing the foam nickel sheet into the prepared solution, burning the foam nickel sheet in a muffle furnace at 180 ℃ for 4 hours, cooling the foam nickel sheet, and washing the foam nickel sheet with distilled water to obtain the high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance.
The NiFeS-OH oxygen evolution catalyst prepared above is tested in 1MKOH solution at normal temperature, and as can be seen from figure 3, in 1MKOH solution at normal temperature and 25 ℃, the current density is 10mAcm-2The overpotential of oxygen evolution is 133mV, and after 5000 circles of circulating CV curve of the catalyst are measured in 1MKOH solution at normal temperature, the current density is 10mAcm-2The oxygen evolution overpotential is 134mV, and the stability is extremely high.
As can be seen from FIGS. 5, 6 and 7, the NiFeS-OH oxygen evolution catalyst material synthesized by the method of the invention has uniform surface distribution and the morphology can provide a large number of active adsorption sites for OH-to attach and react gradually to generate O2And (4) releasing. It can be seen from FIG. 8 that the catalyst prepared by the present invention mainly contains Fe, Ni, O and S elements.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (6)
1. The method for synthesizing the NiFeS-OH oxygen evolution catalyst in one step is characterized by comprising the following steps of: the method comprises the following steps:
s1, soaking the foamed nickel in dilute hydrochloric acid, ethanol and distilled water successively for ultrasonic treatment;
s2, dissolving ferric nitrate hexahydrate in a mixed solution of distilled water and ethylene glycol to obtain a solution A, dissolving sublimed sulfur in toluene or xylene to obtain a solution B, and mixing the solution A and the solution B to obtain a solution with layered interfaces of an organic layer and a water layer;
s3, placing the foamed nickel sheet into the solution prepared in the step S2, calcining for 4-6 hours at 120-180 ℃, cooling, and then washing with distilled water to obtain the product.
2. The one-step synthesis method of the NiFeS-OH oxygen evolution catalyst according to claim 1, characterized in that: the specification of the foamed nickel sheet used in the step S1 is 0.5cm × 0.5cm, 0.8cm × 0.8cm or 1cm × 1 cm.
3. The one-step synthesis method of the NiFeS-OH oxygen evolution catalyst according to claim 1, characterized in that: in the step S2, the solution A is 0.2-0.5 g of ferric nitrate hexahydrate dissolved in a mixed solution of 15mL of distilled water and 5mL of glycol; the solution B is 0.02-0.08 g of sublimed sulfur and is dissolved in 30mL of toluene or xylene solution.
4. The one-step synthesis method of the NiFeS-OH oxygen evolution catalyst according to claim 1, characterized in that: in step S3, the mixture is calcined in a muffle furnace at 150 ℃ for 5 hours.
5. The one-step synthesis method of the NiFeS-OH oxygen evolution catalyst according to claim 1, characterized in that: in the step S1, the volume fraction of the dilute hydrochloric acid is 20%, the ethanol is analytically pure, and the ultrasonic treatment time is 15-20 minutes respectively.
6. A high-efficiency NiFeS-OH oxygen evolution catalyst with high temperature resistance and strong alkali resistance is characterized in that: the catalyst is prepared by the method of any one of claims 1 to 5.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018015891A1 (en) * | 2016-07-21 | 2018-01-25 | Ecole Polytechnique Federale De Lausanne (Epfl) | Nickel iron diselenide compound, process for the preparation thereof and its use as a catalyst for oxygen evolution reaction |
| CN108283926A (en) * | 2018-01-10 | 2018-07-17 | 青岛大学 | A kind of growth in situ ferronickel double-metal hydroxide preparation method with laminated structure in nickel foam |
| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN110227496A (en) * | 2019-06-17 | 2019-09-13 | 安徽师范大学 | A kind of microspheroidal Fe the doping three nickel nano structural material of curing, preparation method and application of nanometer sheet composition |
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Patent Citations (4)
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|---|---|---|---|---|
| WO2018015891A1 (en) * | 2016-07-21 | 2018-01-25 | Ecole Polytechnique Federale De Lausanne (Epfl) | Nickel iron diselenide compound, process for the preparation thereof and its use as a catalyst for oxygen evolution reaction |
| CN108283926A (en) * | 2018-01-10 | 2018-07-17 | 青岛大学 | A kind of growth in situ ferronickel double-metal hydroxide preparation method with laminated structure in nickel foam |
| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN110227496A (en) * | 2019-06-17 | 2019-09-13 | 安徽师范大学 | A kind of microspheroidal Fe the doping three nickel nano structural material of curing, preparation method and application of nanometer sheet composition |
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| Title |
|---|
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