CN115092968A - Preparation method, product and application of iron oxyhydroxide catalyst - Google Patents
Preparation method, product and application of iron oxyhydroxide catalyst Download PDFInfo
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- CN115092968A CN115092968A CN202210640318.0A CN202210640318A CN115092968A CN 115092968 A CN115092968 A CN 115092968A CN 202210640318 A CN202210640318 A CN 202210640318A CN 115092968 A CN115092968 A CN 115092968A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052742 iron Inorganic materials 0.000 claims abstract description 29
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 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 abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000002135 nanosheet Substances 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- 239000002086 nanomaterial Substances 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001301 oxygen Substances 0.000 abstract description 13
- -1 hydroxyl ferric oxide Chemical compound 0.000 abstract description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002362 energy-dispersive X-ray chemical map Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J37/12—Oxidising
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention belongs to the technical field of new materials, and relates to a preparation method, a product and application of a hydroxyl ferric oxide catalyst. The preparation method comprises the following steps: preparing an ammonium fluoride solution; soaking an iron source in an ammonium fluoride solution for standing reaction. The product is an F-FeOOH catalyst nano material with a nano-sheet structure. The application is the application of the iron oxyhydroxide catalyst product in the preparation of electrocatalytic materials, adsorption or nano devices. The invention discloses a method for mildly, concisely and quickly synthesizing an F-FeOOH catalyst with a nanosheet structure, wherein the used raw materials and solvent are cheap and easy to obtain, and the method is pollution-free and has important significance for preparing and applying an iron-based oxygen evolution catalytic material with low cost and high catalytic performance.
Description
Technical Field
The invention belongs to the technical field of new materials, and relates to a synthesis method of an FeOOH catalyst with a nanosheet structure, and a product and application thereof.
Background
Iron oxyhydroxide is a class of transition metal materials with high intrinsic oxygen evolution activity, which has great application potential in reducing noble metal usage. However, pure FeOOH is rarely used alone as an Oxygen Evolution Reaction (OER) catalyst due to its low conductivity, relatively weak oxygen evolution reactivity, and the like. Therefore, the intrinsic activity of FeOOH is greatly improved, which is beneficial to the utilization of rich iron resources in the future electrolytic water industrialization.
So far, the improvement of FeOOH performance mainly includes doping of metal or nonmetal elements, coupling with other oxygen evolution species, and the like. For example by means of electrical activation, at 10mA cm -2 The current density of (1) in situ oxidizing FeSe/IF to Se-doped FeOOH in a time period of 4 hours, although the OER activity is significantly improved, the preparation method is time-consuming and energy-consuming, and the devices required for preparation are complicated and expensive (reference: Journal of the American Chemical Society 141(2019) 7005-7013); although the coupling with metal Co and its oxyhydroxide can introduce new oxygen evolution reaction active site and improve the overall conductivity of the catalyst, the preparation of the required medicine needs to introduce foam nickel net, ammonium nitrate, zinc nitrate, ammonium oxalate, sodium chloride and other additives besides cobalt and iron salt, and the preparation cost is high and is difficult to realize commercial operation (refer to Angewandte Chemie International Edition 11(2016) 3694-. The disadvantages and shortcomings of these preparation or treatment methods described above limit the low cost and large scale preparation of FeOOH catalysts with great application prospects.
Therefore, how to synthesize the FeOOH catalyst with high activity in a room temperature environment, and the preparation method thereof is simple, efficient and green, which is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a mild, simple, green and rapid method for synthesizing an F-FeOOH catalyst with a nanosheet structure, and the method can reduce the preparation time and cost and realize the doping of an F element, so that the overall OER activity of the catalyst is greatly improved. The ammonium fluoride additive is added into the solution, so that fluorine ions are hydrolyzed on the surface of the iron net, a weak acid environment is provided for the growth of FeOOH while promoting the reaction of hydrogen ions and the foamed iron net and releasing Fe ions, the reaction condition is mild, the obtained catalyst has high oxygen precipitation reaction performance and uniform and controllable appearance, and can be produced in a large scale, so that the method has important significance for industrial production and application development of the iron-based high oxygen evolution active material.
The invention firstly provides a preparation method of a hydroxyl ferric oxide catalyst, which comprises the following steps: preparing an ammonium fluoride solution; soaking an iron source in an ammonium fluoride solution for standing reaction.
Further, the iron source is a foam iron net.
Further, the standing reaction temperature is 15-40 ℃.
Further, the standing reaction temperature is 25 ℃.
Further, the standing reaction time is 6-20 hours.
Further, the standing reaction time is 12 hours.
Further, the ammonium fluoride solution is obtained by adding ammonium fluoride into deionized water and stirring vigorously; further comprising the step of drying the reaction product in a vacuum drying oven.
The invention also provides a ferric hydroxide catalyst product prepared by the method.
Further, the product is an F-FeOOH catalyst nano material with a nano-sheet structure.
In addition, the invention also provides application of the iron oxyhydroxide catalyst product in preparation of electrocatalytic materials, adsorption or nano devices.
The invention provides a mild, rapid, simple, convenient, green and efficient new synthesis method for improving the activity and stability of the FeOOH catalyst. Compared with the traditional method, the method has the following outstanding advantages: 1. the reagent used in the reaction is easy to obtain, cheap, green and pollution-free; 2. the reaction condition is simple, the reaction can be carried out quickly, and the energy and the time are saved; 3. the oxygen evolution activity and the stability of the product are greatly improved; 4. the defect that FeOOH species are difficult to prepare under the room temperature condition is overcome; 5. the method expands the synthesis method for preparing the transition metal FeOOH catalyst, and has important guiding significance for researching the formation mechanism of the iron-based oxygen evolution active site catalyst, industrial large-scale production and expanding the application of the iron-based oxygen evolution active site catalyst in the aspects of catalysis, adsorption, nano device preparation and the like.
Description of the drawings:
FIG. 1 is an XRD pattern of the F-FeOOH catalyst prepared in example 1.
FIG. 2 is an SEM picture of the F-FeOOH catalyst prepared in example 1.
FIG. 3 is an EDX map of the F-FeOOH catalyst prepared in example 1.
The specific implementation mode is as follows:
the technical features of the present invention will be described below with reference to specific experimental schemes and drawings, but the present invention is not limited thereto. The test methods described in the following examples are all conventional methods unless otherwise specified; the apparatus and materials are commercially available, unless otherwise specified.
The invention utilizes a foamed iron net to prepare the iron-based oxygen evolution catalyst with a nanosheet structure by simply soaking in an aqueous solution containing an ammonium fluoride additive in a mild room temperature environment, and specifically comprises the following steps:
(1) at room temperature, a certain amount of ammonium fluoride is added into a proper amount of deionized water to form a mixed solution.
(2) Soaking an iron source in an ammonium fluoride solution for standing reaction. The iron source is preferably a foamed iron net. The standing reaction temperature is 15-40 ℃, and preferably 25 ℃. The reaction time is 6 to 20 hours, preferably 12 hours.
In addition, the method can also comprise a step of drying the standing reaction product in a vacuum drying oven.
Example 1:
the synthesis method for rapidly constructing the F-FeOOH catalyst by soaking at room temperature comprises the following steps: adding a certain amount of ammonium fluoride into 100 ml of deionized water, violently stirring to uniformly mix the ammonium fluoride and the deionized water, and adding 1 piece of 1 multiplied by 1 cm of foamed iron net into the solution; at room temperatureStanding and reacting for 12 hours, and drying the prepared product in a vacuum drying oven to obtain the F-FeOOH catalyst. XRD characterization of the sample showed that FeOOH, Fe and Fe were present in the synthesized product as shown in FIG. 1 2 O 3 Characteristic peak of (1), wherein Fe 2 O 3 Possibly due to oxidation of the iron mesh in air at the time of characterization. SEM characterization is carried out on the foam iron net, and as shown in figure 2, a layer of cross-linked nanosheets are uniformly grown on the surface of the foam iron net. FIG. 3 is an X-ray energy spectral analysis (EDX) diagram of the F-FeOOH catalyst, and it can be seen that the elements Fe, O and F are uniformly distributed, indicating that fluorine may be present in the FeOOH catalyst in a doped state.
In conclusion, the invention quickly synthesizes the F-FeOOH oxidation-precipitation material with the nano-sheet structure by utilizing a room-temperature soaking mode, and the X-ray diffraction analysis proves that the synthesized material is FeOOH; the size and the morphology of the nanosheets are characterized by a scanning electron microscope; the uniform distribution of Fe, O and F elements was analyzed by X-ray spectroscopy. The method is simple, mild, efficient and green, provides effective guidance for industrial production of the iron-based oxygen evolution material, and has important value for expanding the application of the iron-based compound in the fields of catalysis, adsorption, photoelectric magnetic materials and the like.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of an iron oxyhydroxide catalyst is characterized by comprising the following steps:
preparing an ammonium fluoride solution;
soaking an iron source in an ammonium fluoride solution for standing reaction.
2. The method of claim 1, wherein: the iron source is a foam iron net.
3. The production method according to claim 1, characterized in that: the standing reaction temperature is 15-40 ℃.
4. The method of claim 1, wherein: the standing reaction temperature is 25 ℃.
5. The method of claim 1, wherein: the standing reaction time is 6-20 hours.
6. The method of claim 1, wherein: the standing reaction time is 12 hours.
7. The production method according to claim 1, characterized in that:
the ammonium fluoride solution is obtained by adding ammonium fluoride into deionized water and stirring violently;
further comprising the step of drying the reaction product in a vacuum drying oven.
8. An iron oxyhydroxide catalyst product prepared by the process of any one of claims 1 to 7.
9. The iron oxyhydroxide catalyst product of claim 8 wherein: the product is an F-FeOOH catalyst nano material with a nano-sheet structure.
10. Use of the iron oxyhydroxide catalyst product of claim 8 or 9 in the preparation of an electrocatalytic material, adsorption, or nanodevice.
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| CN202210640318.0A CN115092968A (en) | 2022-06-08 | 2022-06-08 | Preparation method, product and application of iron oxyhydroxide catalyst |
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| CN202210640318.0A CN115092968A (en) | 2022-06-08 | 2022-06-08 | Preparation method, product and application of iron oxyhydroxide catalyst |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008044826A (en) * | 2006-08-18 | 2008-02-28 | Kobe Univ | Nanoparticle and method for producing the same |
| CN104918698A (en) * | 2013-07-18 | 2015-09-16 | 中国石油大学(北京) | Iron-based hydrogenation catalyst and applications thereof |
| CN108217751A (en) * | 2018-02-09 | 2018-06-29 | 青岛大学 | A kind of preparation method of hexa-prism alpha-FeOOH nano-rod |
| CN108704649A (en) * | 2018-06-21 | 2018-10-26 | 厦门大学 | A kind of base metal base electrolysis water oxygen evolution reaction elctro-catalyst and preparation method thereof |
| CN110656488A (en) * | 2019-10-15 | 2020-01-07 | 陕西科技大学 | Method for loading hydroxyl iron oxide nano particle composite structural color on carbon fiber woven cloth and obtained carbon fiber woven cloth |
-
2022
- 2022-06-08 CN CN202210640318.0A patent/CN115092968A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008044826A (en) * | 2006-08-18 | 2008-02-28 | Kobe Univ | Nanoparticle and method for producing the same |
| CN104918698A (en) * | 2013-07-18 | 2015-09-16 | 中国石油大学(北京) | Iron-based hydrogenation catalyst and applications thereof |
| CN108217751A (en) * | 2018-02-09 | 2018-06-29 | 青岛大学 | A kind of preparation method of hexa-prism alpha-FeOOH nano-rod |
| CN108704649A (en) * | 2018-06-21 | 2018-10-26 | 厦门大学 | A kind of base metal base electrolysis water oxygen evolution reaction elctro-catalyst and preparation method thereof |
| CN110656488A (en) * | 2019-10-15 | 2020-01-07 | 陕西科技大学 | Method for loading hydroxyl iron oxide nano particle composite structural color on carbon fiber woven cloth and obtained carbon fiber woven cloth |
Non-Patent Citations (1)
| Title |
|---|
| XIN-YU ZHANG ET AL.: "F,P double-doped Fe3O4 with abundant defect sites for efficient hydrogen evolution at high current density", 《JOURNAL OF MATERIALS CHEMISTRY A》, pages 15836 - 15845 * |
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