CN115142083A - Preparation method of iron-cobalt-nickel-copper alloy composite oxide - Google Patents
Preparation method of iron-cobalt-nickel-copper alloy composite oxide Download PDFInfo
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- CN115142083A CN115142083A CN202210970772.2A CN202210970772A CN115142083A CN 115142083 A CN115142083 A CN 115142083A CN 202210970772 A CN202210970772 A CN 202210970772A CN 115142083 A CN115142083 A CN 115142083A
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 10
- ZHDZZQCPMPRKFO-UHFFFAOYSA-N [Fe].[Ni].[Cu].[Co] Chemical compound [Fe].[Ni].[Cu].[Co] ZHDZZQCPMPRKFO-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 239000002131 composite material Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 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
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910018054 Ni-Cu Inorganic materials 0.000 description 1
- 229910018481 Ni—Cu Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of an iron-cobalt-nickel-copper alloy composite oxide, which comprises the steps of solution preparation, drying, thermal reaction and the like.
Description
Technical Field
The invention relates to an electrocatalyst, in particular to a preparation method of an iron-cobalt-nickel-copper alloy composite oxide.
Technical Field
With the development of science and technology, how to obtain green sustainable energy efficiently becomes a focus of people. Among them, the generation of hydrogen and oxygen by electrolysis of water is an important means for obtaining hydrogen energy, which is a green sustainable energy source. The process of electrolyzing water is divided into two half-reactions, a hydrogen evolution reaction and an oxygen evolution reaction. Since the oxygen evolution process involves more reaction steps and is more difficult to occur than the hydrogen evolution process, it is important how to improve the oxygen evolution process of the electrolyzed water.
The oxygen evolution electrocatalyst can well promote the oxygen evolution process, thereby improving the catalytic efficiency of the catalyst. Therefore, the design and discovery of the novel oxygen evolution electrocatalyst have important significance. Currently, iridium, ruthenium and oxides thereof have good catalytic oxygen evolution effects, but the price of iridium, ruthenium and oxides thereof is very expensive, and other transition metals such as iron, cobalt and nickel have great potential to replace oxygen evolution catalysts of noble metals. However, the currently reported ferrocobalnickel and its compounds still have the problems of few kinds of active sites, high overpotential and high tafel slope, and the oxygen evolution catalytic activity needs to be further improved to meet the requirements of industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of an iron-cobalt-nickel-copper alloy composite oxide with low overpotential.
The preparation method of the iron-cobalt-nickel-copper alloy composite oxide provided by the invention comprises the following steps: weighing 1 g of paper towel, tearing the paper towel into fragments, and putting the fragments into a beaker; adding 0.25 g of ferric acetate, 0.25 g of cobalt acetate tetrahydrate, 0.25 g of nickel acetate and 0.25 g of copper acetate monohydrate into a beaker, adding 10 ml of deionized water, and stirring by using a magnetic stirrer at room temperature until the mixture is dissolved; completely soaking the paper towel into the solution in the beaker; removing excessive water by using a freeze dryer; selecting a proper alumina crucible, putting the paper towel after freeze drying into the crucible, and placing the crucible in the middle of a tube furnace; carrying out three times of gas washing operation on the tubular furnace by using argon to prevent the tubular furnace from being influenced by residual gas in the tubular furnace; flowing argon is introduced into the tube furnace, the temperature rising speed is set to be 5 ℃ per minute, the tube furnace is gradually heated to 700 ℃ from the room temperature after 140 minutes, the temperature is kept for 4 hours at the temperature, and then the tube furnace is cooled to the room temperature along with the furnace; taking out a sample in the crucible, placing the sample in a mortar, grinding the sample into powder, pouring the powder into a blue-covered bottle, uniformly mixing sulfuric acid with the total amount of 20 milliliters and the concentration of 0.1 mol per liter, putting the mixture into an ultrasonic cleaner, and performing ultrasonic treatment at room temperature for 8 hours; diluting the mixed solution ten times by using deionized water after ultrasonic treatment, filling the diluted mixed solution into a centrifugal tube, symmetrically putting the centrifugal tube into a centrifugal machine, setting the rotating speed to be 1000 revolutions per minute and the time to be 10 minutes, pouring out the upper layer liquid after centrifugation, adding the deionized water, repeating the centrifugal cleaning steps, then carrying out one-time centrifugal cleaning operation by using alcohol, and drying the mixed solution at 70 ℃ by using a constant-temperature air-blast drying box.
The Fe-Co-Ni-Cu alloy composite oxide provided by the invention is used for electrocatalytic oxygen evolution reaction under alkaline condition, and the exchange current density is 10 mA/cm 2 And the overpotential is 283 mV, which is obviously superior to the common Fe, co, ni and their compounds.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the examples will be briefly described below.
FIG. 1 is an X-ray powder diffraction spectrum of a sample prepared by the method of example.
FIG. 2 is an electrocatalytic oxygen evolution overpotential diagram of a sample prepared by the method of the example.
Detailed Description
The following describes the implementation of the present invention in detail with reference to specific embodiments.
The specific steps of this example are as follows: weighing 1 g of paper towel, tearing the paper towel into pieces, and putting the pieces into a beaker; adding 0.25 g of ferric acetate, 0.25 g of cobalt acetate tetrahydrate, 0.25 g of nickel acetate and 0.25 g of copper acetate monohydrate into a beaker, adding 10 ml of deionized water, and stirring by using a magnetic stirrer at room temperature until the mixture is dissolved; completely soaking the paper towel into the solution in the beaker; removing excessive water by using a freeze dryer; selecting a proper alumina crucible, putting the paper towel after freeze drying into the crucible, and placing the crucible in the middle of a tube furnace; carrying out three times of gas washing operation on the tubular furnace by using argon to prevent the tubular furnace from being influenced by residual gas in the tubular furnace; flowing argon is introduced into the tube furnace, the temperature rising speed is set to be 5 ℃ per minute, the tube furnace is gradually heated to 700 ℃ from the room temperature after 140 minutes, the temperature is kept for 4 hours at the temperature, and then the tube furnace is cooled to the room temperature along with the furnace; taking out a sample in the crucible, placing the sample in a mortar, grinding the sample into powder, pouring the powder into a blue-covered bottle, uniformly mixing sulfuric acid with the total amount of 20 milliliters and the concentration of 0.1 mol per liter, putting the mixture into an ultrasonic cleaner, and performing ultrasonic treatment at room temperature for 8 hours; diluting the mixed solution ten times with deionized water after ultrasonic treatment, filling the diluted mixed solution into a centrifugal tube, symmetrically putting the centrifugal tube into a centrifugal machine, setting the rotation speed to be 1000 revolutions per minute and the time to be 10 minutes, pouring out the upper-layer liquid after centrifugation, adding the deionized water, repeating the centrifugal cleaning steps, then carrying out one-time centrifugal cleaning operation by using alcohol, and drying the mixed solution at 70 ℃ by using a constant-temperature air blast drying box.
The invention is further illustrated by the following examples in conjunction with the accompanying drawings.
FIG. 1 is an X-ray powder diffraction pattern of a sample prepared according to the example, showing that the sample prepared according to the example is indeed an iron-cobalt-nickel-copper alloy and its corresponding oxides. The XRD diffraction patterns of the iron, cobalt, nickel and copper simple substances are similar, only the diffraction peak of copper is shown in figure 1, the prepared sample has good corresponding relation with the diffraction peak of copper, and the diffraction peak is widened and shifted, which indicates that the iron-cobalt-nickel-copper alloy is indeed formed. FIG. 2 is a diagram of the overpotential of electrocatalytic oxygen evolution under alkaline conditions for a sample prepared by the method of example, at an exchange current density of 10 mA/cm 2 The overpotential was 283 mV.
It should be noted that the above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations, which may be directly derived or suggested to one skilled in the art without departing from the basic concept of the invention, are to be considered as included within the scope of the invention.
Claims (2)
1. The preparation method of the iron-cobalt-nickel-copper alloy composite oxide is characterized by comprising the following steps of: weighing 1 g of paper towel, tearing the paper towel into pieces, and putting the pieces into a beaker; adding 0.25 g of ferric acetate, 0.25 g of cobalt acetate tetrahydrate, 0.25 g of nickel acetate and 0.25 g of copper acetate monohydrate into a beaker, adding 10 ml of deionized water, and stirring by using a magnetic stirrer at room temperature until the materials are dissolved; completely soaking the paper towel into the solution in the beaker; removing excessive water by using a freeze dryer; selecting a proper alumina crucible, putting the paper towel after freeze drying into the crucible, and placing the crucible in the middle of a tube furnace; carrying out three times of gas washing operation on the tubular furnace by using argon to prevent the tubular furnace from being influenced by residual gas in the tubular furnace; flowing argon is introduced into the tubular furnace, the temperature rising speed is set to be 5 ℃ per minute, the temperature of the tubular furnace is gradually raised to 700 ℃ from the room temperature after 140 minutes, the temperature is kept for 4 hours at the temperature, and then the tubular furnace is cooled to the room temperature along with the furnace; taking out a sample in the crucible, placing the sample in a mortar, grinding the sample into powder, pouring the powder into a blue-covered bottle, uniformly mixing sulfuric acid with the total amount of 20 milliliters and the concentration of 0.1 mol per liter, putting the mixture into an ultrasonic cleaner, and performing ultrasonic treatment at room temperature for 8 hours; diluting the mixed solution ten times by using deionized water after ultrasonic treatment, filling the diluted mixed solution into a centrifugal tube, symmetrically putting the centrifugal tube into a centrifugal machine, setting the rotating speed to be 1000 revolutions per minute and the time to be 10 minutes, pouring out the upper layer liquid after centrifugation, adding the deionized water, repeating the centrifugal cleaning steps, then carrying out one-time centrifugal cleaning operation by using alcohol, and drying the mixed solution at 70 ℃ by using a constant-temperature air-blast drying box.
2. The iron-cobalt-nickel-copper alloy composite oxide according to claim 1, which is used in the field of electrocatalytic oxygen evolution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210970772.2A CN115142083A (en) | 2022-08-13 | 2022-08-13 | Preparation method of iron-cobalt-nickel-copper alloy composite oxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210970772.2A CN115142083A (en) | 2022-08-13 | 2022-08-13 | Preparation method of iron-cobalt-nickel-copper alloy composite oxide |
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| CN202210970772.2A Pending CN115142083A (en) | 2022-08-13 | 2022-08-13 | Preparation method of iron-cobalt-nickel-copper alloy composite oxide |
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| CN111185188A (en) * | 2019-12-27 | 2020-05-22 | 江南大学 | Iron-cobalt-nickel-copper-based high-entropy alloy electrolytic water catalytic material and preparation method thereof |
| CN112619649A (en) * | 2019-09-24 | 2021-04-09 | 中国石油大学(华东) | Nickel-cobalt-iron ternary oxide electrolytic water composite material and preparation method and application thereof |
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2022
- 2022-08-13 CN CN202210970772.2A patent/CN115142083A/en active Pending
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| CN110171822A (en) * | 2019-05-27 | 2019-08-27 | 北京科技大学 | A kind of porous hollow bowl-type graphite material and preparation method thereof |
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| Title |
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Application publication date: 20221004 |