CN113957456B - Nickel-based alkaline electrolyzed water catalyst co-doped with and combined with heterostructure and preparation method - Google Patents
Nickel-based alkaline electrolyzed water catalyst co-doped with and combined with heterostructure and preparation method Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 294
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 103
- 239000003054 catalyst Substances 0.000 title claims abstract description 100
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006260 foam Substances 0.000 claims abstract description 45
- 229910052742 iron Inorganic materials 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 36
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 29
- 239000012670 alkaline solution Substances 0.000 claims abstract description 7
- 238000002848 electrochemical method Methods 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 79
- 239000010949 copper Substances 0.000 claims description 65
- 239000000758 substrate Substances 0.000 claims description 26
- 238000006056 electrooxidation reaction Methods 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000004070 electrodeposition Methods 0.000 claims description 18
- 239000003792 electrolyte Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000002484 cyclic voltammetry Methods 0.000 claims description 12
- 239000007853 buffer solution Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000002082 metal nanoparticle Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 150000001879 copper Chemical class 0.000 claims description 8
- 150000002815 nickel Chemical class 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical group O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group 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 7
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000000872 buffer Substances 0.000 claims 2
- 125000005619 boric acid group Chemical group 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 18
- 239000001257 hydrogen Substances 0.000 abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 abstract description 18
- 239000001301 oxygen Substances 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000010276 construction Methods 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000010411 electrocatalyst Substances 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052956 cinnabar Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 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
- 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
- C25B11/04—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
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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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25D3/00—Electroplating: Baths therefor
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- C25D3/00—Electroplating: Baths therefor
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- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- 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
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Abstract
The invention belongs to the technical field of electrochemical catalytic materials, and discloses a co-doped nickel-based alkaline electrolyzed water catalyst combined with a heterostructure and a preparation method thereof, wherein the molecular formula of the catalyst is as follows: EO-Cu 3-Fe2-Ni50/NF. The catalyst is an alkaline electrolysis water catalyst loaded on foam nickel, and through Cu and Fe co-doping and Ni (OH) 2/Ni heterostructure construction, the oxidation state of active metal center Ni is regulated, and rich Ni (OH) 2/Ni heterogeneous interfaces are provided, so that the catalyst has excellent electrocatalytic hydrogen evolution activity, oxygen evolution activity and stability in alkaline solution, and has high-efficiency and stable electrocatalytic full water decomposition performance. The catalyst is prepared by adopting a two-step electrochemical method, the preparation process is simple, the raw materials are low in price and easy to obtain, and the prepared catalyst has excellent electrolysis water performance and can be applied to practical alkaline electrolysis water.
Description
Technical Field
The invention belongs to the technical field of electrochemical catalytic materials, and particularly relates to a co-doped nickel-based alkaline electrolyzed water catalyst combined with a heterostructure and a preparation method thereof.
Background
At present, a good environment is a basis for survival, and sufficient energy is a precondition for social development. The environmental pollution and energy shortage problems faced by today's society are key issues restricting survival and development. Therefore, development of clean renewable energy is urgently needed. The hydrogen energy is used as a new energy source with zero carbon emission, sustainability, reproducibility and high energy density, and is the most environment-friendly clean energy source. Therefore, how to produce hydrogen energy in a low cost, efficient, pollution-free manner has become a research hotspot.
The two half reactions of the electrolyzed water, the hydrogen evolution reaction of the cathode and the oxygen evolution reaction of the anode have the advantages of no carbon emission, sustainable development, high product purity and the like, and are widely paid attention to. The electrolysis of water requires the application of a certain voltage to drive the production of hydrogen and oxygen. In order to reduce the energy consumption and improve the energy conversion efficiency, the process needs a high-efficiency, low-cost and continuous stable catalyst to reduce the energy consumption, thereby realizing the practical application of hydrogen production by water electrolysis. At present, the high-activity catalyst is still a noble metal-based catalyst such as platinum, ruthenium, iridium, rhodium and the like. However, it is expensive and has poor stability, which limits its large-scale application. Therefore, the electrocatalyst with low development cost, high catalytic activity and good stability is a key for practical application of hydrogen production by water electrolysis.
Currently, many non-noble metal-based electrocatalysts, such as Fe, co, ni, mo-based electrocatalysts, have been developed that are excellent in performance, low in cost, and good in stability. In particular, ni-based catalysts have been widely studied because of their good conductivity, high catalytic activity, low cost, easy availability, environmental friendliness, etc., but the catalytic activity and stability of metallic nickel are not very good. Therefore, various strategies have been developed to improve the catalytic activity and stability of nickel, such as metal compound synthesis, alloying, doping with different elements, heterostructures construction, etc. However, most nickel-based catalysts exhibit only good electrocatalytic hydrogen or oxygen evolution properties and are less efficient in water electrolysis due to their different selectivity for catalytic reactions.
Therefore, in order to realize efficient electrolysis of water, it is necessary to develop a bifunctional electrocatalyst having both excellent hydrogen evolution reaction and oxygen evolution reaction.
Through the above analysis, the problems and defects existing in the prior art are as follows: the existing nickel-based catalyst has poor catalytic activity and stability and low water electrolysis efficiency.
The difficulty of solving the problems and the defects is as follows: how to synthesize the bifunctional catalyst with high catalytic activity and stable activity through the combination design of various strategies.
The meaning of solving the problems and the defects is as follows: the development of a dual-function electrocatalyst with excellent hydrogen evolution reaction and oxygen evolution reaction simultaneously can realize high-efficiency water electrolysis.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a co-doped nickel-based alkaline electrolyzed water catalyst combined with a heterostructure and a preparation method thereof.
The invention is realized in such a way that the co-doped nickel-based alkaline water electrolysis catalyst combined with the heterostructure is Cu and Fe co-doped Ni (OH) 2/Ni heterostructure alkaline water electrolysis catalyst with rich heterogeneous interfaces; physical properties: the method has rich heterogeneous interfaces; chemical characteristics: catalyzing alkaline electrolysis water reaction;
The molecular formula of the catalyst is as follows: EO-Cu 3-Fe2-Ni50/NF.
Another object of the present invention is to provide a method for preparing the co-doped heterostructure-combined nickel-based alkaline electrolyzed water catalyst, which includes:
And loading the Cu and Fe co-doped Ni (OH) 2/Ni heterostructure catalyst on the foam nickel substrate by a two-step electrochemical method.
Further, the preparation method of the co-doped and heterostructure-combined nickel-based alkaline electrolyzed water catalyst comprises the following steps of:
Step one, foam nickel treatment is carried out: soaking a certain area of foam nickel by using concentrated hydrochloric acid placed in a beaker, and performing ultrasonic treatment; cleaning the soaked and ultrasonically treated foam nickel by using deionized water and ethanol, and drying;
Step two, preparing Cu 3-Fe2-Ni50/NF by electrochemical deposition: loading Cu and Fe co-doped Ni on a foam nickel substrate of a working electrode by adopting a three-electrode system through an electrochemical deposition method to obtain Cu 3-Fe2-Ni50/NF;
Step three, synthesizing EO-Cu 3-Fe2-Ni50/NF by electrochemical oxidation: and carrying out electrochemical oxidation on the prepared Cu 3-Fe2-Ni50/NF by adopting a three-electrode system through a cyclic voltammetry to obtain the co-doped nickel-based alkaline electrolyzed water catalyst combined with the heterostructure.
Further, in the first step, the area of the foam nickel is 1×1cm 2; the ultrasonic treatment time is 10min; to remove the oxide layer on the surface of the foam nickel.
Further, in the second step, the three-electrode system includes: hg/Hg 2SO4 and a carbon rod are respectively used as a reference electrode and a counter electrode.
Further, in the second step, the electrochemical deposition for preparing Cu 3-Fe2-Ni50/NF comprises the following steps:
adding proper copper salt, ferric salt and nickel salt into the buffer solution, and stirring for a period of time by ultrasonic waves to obtain transparent electrolyte;
under a certain voltage, metal ions are electrodeposited from electrolyte to a foam nickel substrate in the form of nickel metal nano particles co-doped with copper and iron, the foam nickel substrate is taken out after standing for a period of time, and the foam nickel substrate is washed clean by deionized water, so that Cu 3-Fe2-Ni50/NF can be obtained.
Further, the buffer solution is boric acid solution, and the concentration of the buffer solution is 0.5M; the method has the effects of inhibiting the generation of hydroxide and improving the purity of the sample.
The nickel salt is nickel nitrate hexahydrate, and the concentration of the nickel salt is 0.5M; the function is to provide rich nickel ions.
The copper salt is copper nitrate trihydrate, and the concentration of the copper salt is 0.03M; acting to provide a copper dopant.
The ferric salt is ferric nitrate nonahydrate, and the concentration of the ferric salt is 0.02M; acting to provide an iron dopant.
The voltage was-2 vvs.hg/Hg 2SO4, which was operative to reduce and deposit metal ions in the form of copper, iron co-doped nickel metal nanoparticles from the electrolyte to the foam nickel substrate at negative voltage, the electrodeposition time was 600 seconds.
Further, in step three, the three-electrode system includes: cu 3-Fe2-Ni50/NF is used as a working electrode, and a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode.
Further, in the third step, the electrochemical oxidation synthesis of EO-Cu 3-Fe2-Ni50/NF comprises the following steps:
The prepared Cu 3-Fe2-Ni50/NF was immersed in an alkaline solution having a concentration of 1.0M by cyclic voltammetry, and 25 cycles were performed at a sweep rate of 100mV/s in a voltage range of-0.675 to 0Vvs. RHE. The function is to oxidize part of the metal to hydroxide, building up a heterostructure.
Another object of the present invention is to provide the use of the co-doped heterostructure-bound nickel-based alkaline electrolyzed water catalyst in alkaline electrolyzed water.
By combining all the technical schemes, the invention has the advantages and positive effects that: the catalyst is an alkaline electrolysis water catalyst loaded on foam nickel, and through Cu and Fe co-doping and Ni (OH) 2/Ni heterostructure construction, the oxidation state of active metal center Ni is regulated, and rich Ni (OH) 2/Ni heterogeneous interfaces are provided, so that the catalyst has excellent electrocatalytic hydrogen evolution activity, oxygen evolution activity and stability in alkaline solution, and has high-efficiency and stable electrocatalytic full water decomposition performance. The catalyst is prepared by adopting a two-step electrochemical method, the heterostructure catalyst is synthesized under the conditions of normal temperature and normal pressure, the preparation process is simple, the raw materials are low in price and easy to obtain, the prepared catalyst has excellent electrolysis water performance, and the practical application of alkaline electrolysis water can be realized.
The stability of the copper and iron co-doped nickel hydroxide is improved, the heterogeneous interface of the catalyst is stabilized, and the co-doping optimizes the electronic structure of the catalyst, so that the catalytic activity and stability of the electrocatalytic hydrogen evolution of the catalyst are improved. Meanwhile, the oxidation state of nickel in the center of the active metal is regulated through Cu and Fe co-doping, and the oxygen production efficiency and catalytic activity of electrocatalytic oxygen evolution are improved. The invention utilizes Cu and Fe co-doping to combine with the construction of Ni (OH) 2/Ni heterostructure, realizes the synthesis of the catalyst with excellent electrochemical hydrogen evolution and oxygen evolution catalytic activity and stability, and realizes the high-efficiency stable alkaline electrolyzed water application.
According to the invention, a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure electrocatalyst is synthesized by utilizing a dual strategy, and experimental results show that by improving the stability of copper and iron co-doped nickel hydroxide, the Ni (OH) 2/Ni heterostructure of the catalyst is stabilized, and the co-doping optimizes the electronic structure of the catalyst, so that the catalytic activity and stability of the catalyst for electrocatalytic hydrogen evolution are improved. In addition, cu and Fe co-doping regulates the oxidation state of nickel in the center of the active metal, and improves the oxygen production efficiency and catalytic activity of electrocatalytic oxygen evolution. In conclusion, the method utilizes a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure to deposit on foam nickel by a two-step electrochemical method to obtain the EO-Cu 3-Fe2-Ni50/NF electrocatalyst, and can realize high-efficiency and stable alkaline electrolyzed water.
Drawings
FIG. 1 is a flow chart of a method for preparing a nickel-based alkaline electrolyzed water catalyst with a co-doped and combined heterostructure according to an embodiment of the present invention.
FIG. 2 is an XRD pattern of a co-doped, heterostructure-bonded nickel-based alkaline electrolyzed water catalyst provided in accordance with an embodiment of the present invention.
FIG. 3 is a scanning electron microscope image of a nickel-based alkaline electrolyzed water catalyst co-doped with a heterostructure provided by an embodiment of the present invention.
FIG. 4 is a high power transmission electron microscope image of a nickel-based alkaline electrolyzed water catalyst co-doped and heterostructure provided by an embodiment of the present invention.
FIG. 5 is an X-ray photoelectron spectrum of a nickel-based alkaline electrolyzed water catalyst with a co-doped and combined heterostructure provided by an embodiment of the present invention.
FIG. 6 is a graph of electrocatalytic hydrogen evolution polarization of a co-doped, heterostructure-coupled nickel-based alkaline electrolyzed water catalyst provided by an embodiment of the present invention.
FIG. 7 is an electrocatalytic oxygen evolution cyclic voltammogram of a nickel-based alkaline electrolyzed water catalyst co-doped with a heterostructure provided by an embodiment of the present invention.
FIG. 8 is a graph of the polarization of alkaline electrolyzed water for a nickel-based alkaline electrolyzed water catalyst co-doped with a heterostructure provided by an embodiment of the present invention.
FIG. 9 is a graph of stability test i-t of alkaline electrolyzed water of a nickel-based alkaline electrolyzed water catalyst co-doped with a bonded heterostructure provided in accordance with an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Aiming at the problems existing in the prior art, the invention provides a co-doped nickel-based alkaline water electrolysis catalyst combined with a heterostructure and a preparation method thereof, and the invention is described in detail below with reference to the accompanying drawings.
The nickel-based alkaline electrolytic water catalyst co-doped with the combined heterostructure provided by the embodiment of the invention is a Ni (OH) 2/Ni heterostructure catalyst co-doped with Cu and Fe;
the molecular formula of the catalyst provided by the embodiment of the invention is as follows: EO-Cu 3-Fe2-Ni50/NF.
The preparation method of the nickel-based alkaline water electrolysis catalyst with the co-doped and combined heterostructure provided by the embodiment of the invention comprises the following steps:
And loading the Cu and Fe co-doped Ni (OH) 2/Ni heterostructure catalyst on the foam nickel substrate by a two-step electrochemical method.
As shown in fig. 1, the preparation method of the nickel-based alkaline water electrolysis catalyst with the co-doped and combined heterostructure provided by the embodiment of the invention comprises the following steps:
s101, performing foam nickel treatment: soaking foamed nickel of 1X 1cm 2 in concentrated hydrochloric acid in a beaker, and performing ultrasonic treatment for 10min; cleaning the soaked and ultrasonically treated foam nickel by using deionized water and ethanol, and drying;
S102, preparing Cu 3-Fe2-Ni50/NF by electrochemical deposition: the Hg/Hg 2SO4 and the carbon rod are respectively used as a reference electrode and a counter electrode, and Cu and Fe co-doped Ni metal nano particles are loaded on a foam nickel substrate of a working electrode by an electrochemical deposition method to obtain Cu 3-Fe2-Ni50/NF;
S103, synthesizing EO-Cu 3-Fe2-Ni50/NF by electrochemical oxidation: cu 3-Fe2-Ni50/NF is used as a working electrode, a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode, and the prepared Cu 3-Fe2-Ni50/NF is subjected to electrochemical oxidation by using a cyclic voltammetry to obtain the co-doped nickel-based alkaline electrolyzed water catalyst combined with the heterostructure.
The preparation of Cu 3-Fe2-Ni50/NF by electrochemical deposition provided by the embodiment of the invention comprises the following steps:
Adding 0.5M nickel nitrate hexahydrate, 0.03M copper nitrate trihydrate and 0.02M ferric nitrate nonahydrate into a boric acid solution with the concentration of 0.5M, and stirring for a period of time by ultrasonic waves to obtain transparent electrolyte;
And electrodepositing metal ions from the electrolyte to a foam nickel substrate in the form of copper and iron co-doped nickel metal nano particles under the voltage of minus 2Vvs.
The electrodeposition time provided by the embodiment of the invention is 600 seconds.
The electrochemical oxidation synthesis of EO-Cu 3-Fe2-Ni50/NF provided by the embodiment of the invention comprises the following steps:
The prepared Cu 3-Fe2-Ni50/NF was immersed in an alkaline solution having a concentration of 1.0M by cyclic voltammetry, and 25 cycles were performed at a sweep rate of 100mV/s in a voltage range of-0.675 to 0Vvs. RHE.
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1:
The invention provides a co-doped nickel-based alkaline electrolytic water catalyst combined with a heterostructure, which is characterized in that a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure catalyst is loaded on treated foam nickel by a two-step electrochemical method.
The invention provides a preparation method of the catalyst, which comprises the following steps:
(1) Treating foam nickel: placing a certain area of foam nickel in a beaker, adding concentrated hydrochloric acid, soaking, performing ultrasonic treatment for a certain time, taking out, cleaning with a large amount of deionized water and ethanol, and drying.
(2) Electrochemical deposition of Cu 3-Fe2-Ni50/NF: and (3) taking Hg/Hg 2SO4 and a carbon rod as a reference electrode and a counter electrode respectively, and loading Cu and Fe co-doped Ni on the foam nickel substrate of the working electrode by an electrochemical deposition method. And under a certain voltage, metal ions are electrodeposited from the electrolyte into a foam nickel substrate in the form of copper and iron co-doped nickel metal nano particles by taking a certain concentration of buffer solution and a certain amount of copper salt, ferric salt and nickel salt as electrolyte, and then the foam nickel substrate is taken out after a period of time.
(3) Electrochemical Oxidation (EO) synthesis EO-Cu 3-Fe2-Ni50/NF: the electrochemical oxidation is carried out by a three-electrode system, the catalyst obtained in the step (2) is used as a working electrode, and a graphite electrode and Hg/HgO are used as a counter electrode and a reference electrode, respectively. The process uses cyclic voltammetry to carry out a certain number of cycles in alkaline solution with a certain concentration at a certain sweeping speed within a certain voltage range.
The certain area in the step (1) is 1 multiplied by 1cm 2, and the certain time is 10 minutes.
The buffer solution in the step (2) is boric acid solution with the concentration of 0.5M, the nickel salt is nickel nitrate hexahydrate with the concentration of 0.5M, the copper salt is copper nitrate trihydrate with the concentration of 0.03M, the ferric salt is ferric nitrate nonahydrate with the concentration of 0.02M, the voltage is-2 Vvs. Hg/Hg 2SO4, and the electrodeposition time is 600 seconds.
The alkaline solution in the step (3) is potassium hydroxide with the concentration of 1.0M, the voltage range is-0.675-0 Vvs. RHE, the sweeping speed is 100mV/s, and the number of circulation times is 25.
The invention discloses a nickel-based alkaline water electrolysis catalyst co-doped and combined with a heterostructure, which is applied to an electrochemical alkaline water electrolysis catalyst.
FIG. 2 is an XRD pattern of the catalyst prepared in example 2, from which it can be seen that there are only Ni and Ni (OH) 2 diffraction peaks and no Cu and Fe diffraction peaks, thus indicating successful synthesis of Cu and Fe co-doped Ni/Ni (OH) 2.
FIG. 3 is a scanning electron micrograph of the catalyst prepared according to example 2, from which it can be seen that the catalyst is a nanoparticle having a diameter of about 300 nm.
FIG. 4 is a high power transmission electron micrograph of the catalyst prepared according to example 2; two lattice fringes can be seen from the figure, d=0.240 nm to Ni (OH) 2 (101) and d=0.21 nm to Ni (111). From this, successful synthesis of Ni (OH) 2/Ni was known, and a rich heterogeneous interface was seen.
FIG. 5 is an X-ray photoelectron spectrum of a catalyst prepared as in example 2; from the figure, it is clear that Ni is mainly divalent and exists in the form of Ni (OH) 2; cu is present in the catalyst mainly at zero and divalent and Fe is mainly at zero and trivalent, indicating successful doping of Cu and Fe.
FIG. 6 is an electrocatalytic hydrogen evolution polarization curve for a catalyst prepared as per example 2; as can be seen from the graph, the overpotential was 25mV at a current density of 10mA/cm 2. The comparison shows that the performance is superior to most of reported hydrogen evolution electrocatalysts. The method shows that the electrochemical oxidation is used for constructing the Ni (OH) 2/Ni heterogeneous interface, so that the hydrogen evolution performance is greatly improved, and meanwhile, the doping of Cu and Fe is beneficial to the further improvement of the performance by adjusting the electronic structure of the catalyst.
FIG. 7 is an electrocatalytic oxygen evolution cyclic voltammogram of a catalyst prepared as example 2. As can be seen, the overpotential was 202mV at a current density of 10mA/cm 2. The comparison shows that the performance is superior to that of most oxygen evolution electrocatalysts. And the oxidation potential of the catalyst can be known to rise along with the doping of Cu and Fe metal elements, which means that the oxidation state of the metal active center in the oxygen evolution reaction process is reduced along with the doping of Cu and Fe metal elements, so that the energy barrier of the oxygen evolution reaction is reduced, the oxygen production efficiency is improved, and the catalytic activity is improved.
FIG. 8 is an alkaline electrolyzed water polarization curve of a catalyst prepared according to example 2; it can be seen from the figure that the catalyst constructed by co-doping Cu and Fe with Ni (OH) 2/Ni heterostructures shows excellent alkaline electrolyzed water performance. At an operating current density of 10mA/cm 2, the voltage was only 1.439V.
FIG. 9 is a graph of stability test i-t for alkaline electrolyzed water of a catalyst prepared according to example 2; it can be seen from the graph that stable operation can be continued for at least 36 hours at a current density of 10mA/cm 2, indicating that the catalyst has excellent alkaline electrolyzed water stability.
The invention is characterized by XRD, XPS and HRTEM, and can know that an EO-Cu 3-Fe2-Ni50/NF sample consists of a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure, and Ni (OH) 2 grows from Ni through electrochemical oxidation. Electrochemical tests show that the catalyst has excellent and stable alkaline water electrolysis performance.
Example 2:
The preparation method of the nickel-based alkaline electrolysis water catalyst with the co-doped and combined heterostructure provided by the invention comprises the following steps: firstly, placing 1.0cm 2 of foam nickel into a beaker, adding concentrated hydrochloric acid, carrying out ultrasonic treatment for 10 minutes, taking out, cleaning with a large amount of deionized water and ethanol, and drying. And then Ni is loaded on a working electrode foam nickel substrate by an electrochemical deposition method, hg/Hg 2SO4 and a carbon rod are respectively used as a reference electrode and a counter electrode, 0.03M copper nitrate trihydrate, 0.005M ferric nitrate nonahydrate, 0.5M boric acid buffer solution and 0.5M nickel nitrate hexahydrate are used as electrolyte, cu, fe and Ni ions are electrodeposited from the electrolyte to the foam nickel substrate in the form of Cu and Fe co-doped Ni metal nano particles under the voltage of-2 Vvs. Hg/Hg 2SO4, and the foam nickel substrate is taken out after 600 seconds. And finally, carrying out electrochemical oxidation by using a three-electrode system, wherein the catalyst obtained above is used as a working electrode, and a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode. Electrochemical oxidation was carried out by cyclic voltammetry in a 1.0M potassium hydroxide solution at a voltage range of-0.675 to 0Vvs. RHE for 25 cycles at a sweep rate of 100 mV/s.
Example 3:
The preparation method of the nickel-based alkaline electrolysis water catalyst with the co-doped and combined heterostructure provided by the invention comprises the following steps: firstly, placing 1.0cm 2 of foam nickel into a beaker, adding concentrated hydrochloric acid, carrying out ultrasonic treatment for 10 minutes, taking out, cleaning with a large amount of deionized water and ethanol, and drying. Then Ni is loaded on a working electrode foam nickel substrate by an electrochemical deposition method, hg/Hg 2SO4 and a carbon rod are respectively used as a reference electrode and a counter electrode, 0.03M copper nitrate trihydrate, 0.02M ferric nitrate nonahydrate, 0.5M boric acid buffer solution and 0.5M nickel nitrate hexahydrate are used as electrolyte, cu, fe and Ni ions are electrodeposited from the electrolyte to the foam nickel substrate in the form of Cu and Fe co-doped Ni metal nano particles under the voltage of-2.5 Vvs. Hg/Hg 2SO4, and the foam nickel substrate is taken out after 600 seconds. And finally, carrying out electrochemical oxidation by using a three-electrode system, wherein the catalyst obtained above is used as a working electrode, and a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode. Electrochemical oxidation was carried out by cyclic voltammetry in a 1.0M potassium hydroxide solution at a voltage range of-0.675 to 0Vvs. RHE for 25 cycles at a sweep rate of 100 mV/s.
Example 4:
The preparation method of the nickel-based alkaline electrolysis water catalyst with the co-doped and combined heterostructure provided by the invention comprises the following steps: firstly, placing 1.0cm 2 of foam nickel into a beaker, adding concentrated hydrochloric acid, carrying out ultrasonic treatment for 10 minutes, taking out, cleaning with a large amount of deionized water and ethanol, and drying. And then Ni is loaded on a working electrode foam nickel substrate by an electrochemical deposition method, hg/Hg 2SO4 and a carbon rod are respectively used as a reference electrode and a counter electrode, 0.03M copper nitrate trihydrate, 0.03M ferric nitrate nonahydrate, 0.5M boric acid buffer solution and 0.5M nickel nitrate hexahydrate are used as electrolyte, cu, fe and Ni ions are electrodeposited from the electrolyte to the foam nickel substrate in the form of Cu and Fe co-doped Ni metal nano particles under the voltage of-2 Vvs. Hg/Hg 2SO4, and the foam nickel substrate is taken out after 600 seconds. And finally, carrying out electrochemical oxidation by using a three-electrode system, wherein the catalyst obtained above is used as a working electrode, and a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode. Electrochemical oxidation was carried out by cyclic voltammetry in a 1.0M potassium hydroxide solution at a voltage range of-0.675 to 0Vvs. RHE for 30 cycles at a sweep rate of 50 mV/s.
In examples 1 to 4 of the present invention, the area of the catalyst working electrode was 1.0cm 2, and in order to make the data obtained by the electrochemical test comparable, the following examples were all subjected to the electrochemical test using the CHI660E electrochemical workstation of the Shanghai cinnabar instruments company. The test conditions were as follows: the graphite electrode is used as a counter electrode, the Hg/HgO electrode is used as a reference electrode, a three-electrode system is formed by the graphite electrode and the catalyst, and the electrolyte is 1.0MKOH aqueous solution.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (8)
1. The co-doped heterostructure-combined nickel-based alkaline electrolyzed water catalyst is characterized in that the co-doped heterostructure-combined nickel-based alkaline electrolyzed water catalyst is a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure catalyst;
The molecular formula of the catalyst is as follows: EO-Cu 3-Fe2-Ni50/NF.
The preparation method of the co-doped and heterostructure-combined nickel-based alkaline electrolyzed water catalyst comprises the following steps:
Loading a Cu and Fe co-doped Ni (OH) 2/Ni heterostructure catalyst on a foam nickel substrate by a two-step electrochemical method;
The preparation method of the co-doped and heterostructure-combined nickel-based alkaline electrolyzed water catalyst comprises the following steps of:
Step one, foam nickel treatment is carried out: soaking a certain area of foam nickel by using concentrated hydrochloric acid placed in a beaker, and performing ultrasonic treatment; cleaning the soaked and ultrasonically treated foam nickel by using deionized water and ethanol, and drying;
Step two, preparing Cu 3-Fe2-Ni50/NF by electrochemical deposition: loading Cu and Fe co-doped Ni on a foam nickel substrate of a working electrode by adopting a three-electrode system through an electrochemical deposition method to obtain Cu 3-Fe2-Ni50/NF;
Step three, synthesizing EO-Cu 3-Fe2-Ni50/NF by electrochemical oxidation: and carrying out electrochemical oxidation on the prepared Cu 3-Fe2-Ni50/NF by adopting a three-electrode system through a cyclic voltammetry to obtain the co-doped nickel-based alkaline electrolyzed water catalyst combined with the heterostructure.
2. The co-doped, heterostructure-bonded nickel-based alkaline electrolysis water catalyst of claim 1, wherein in step one, the area of the foamed nickel is 1 x 1cm 2; the sonication time was 10 minutes.
3. The co-doped heterostructure-bonded nickel-based alkaline water electrolysis catalyst of claim 1, wherein in step two, the three electrode system comprises: hg/Hg 2SO4 and a carbon rod are respectively used as a reference electrode and a counter electrode.
4. The co-doped, heterostructure-bonded nickel-based alkaline electrolyzed water catalyst of claim 1, wherein in step two, the electrochemical deposition to produce Cu 3-Fe2-Ni50/NF comprises the steps of:
adding proper copper salt, ferric salt and nickel salt into the buffer solution, and stirring for a period of time by ultrasonic waves to obtain transparent electrolyte;
under a certain voltage, metal ions are electrodeposited from electrolyte to a foam nickel substrate in the form of nickel metal nano particles co-doped with copper and iron, the foam nickel substrate is taken out after standing for a period of time, and the foam nickel substrate is washed clean by deionized water, so that Cu 3-Fe2-Ni50/NF can be obtained.
5. The co-doped, heterostructure-bonded nickel-based alkaline electrolysis water catalyst of claim 4, wherein the buffer is a boric acid solution at a buffer concentration of 0.5M;
The nickel salt is nickel nitrate hexahydrate, and the concentration of the nickel salt is 0.5M;
the copper salt is copper nitrate trihydrate, and the concentration of the copper salt is 0.03M;
the ferric salt is ferric nitrate nonahydrate, and the concentration of the ferric salt is 0.02M;
The voltage was-2 v vs. Hg/Hg 2SO4 and the electrodeposition time was 600 seconds.
6. The co-doped heterostructure-bonded nickel-based alkaline water electrolysis catalyst of claim 1, wherein in step three, the three electrode system comprises: cu 3-Fe2-Ni50/NF is used as a working electrode, and a graphite electrode and Hg/HgO are respectively used as a counter electrode and a reference electrode.
7. The co-doped, heterostructure-bonded nickel-based alkaline electrolyzed water catalyst of claim 1, wherein in step three, the electrochemical oxidation synthesis of EO-Cu 3-Fe2-Ni50/NF comprises the steps of:
The prepared Cu 3-Fe2-Ni50/NF was immersed in an alkaline solution having a concentration of 1.0M by cyclic voltammetry, and 25 cycles were performed at a sweep rate of 100mV/s in a voltage range of-0.675 to 0Vvs. RHE.
8. A nickel-based alkaline electrolyzed water catalyst co-doped with a bound heterostructure according to claim 1 for use in alkaline electrolyzed water.
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