CN116377501A - Electrocatalytic hydrogen evolution material and preparation method and application thereof - Google Patents
Electrocatalytic hydrogen evolution material and preparation method and application thereof Download PDFInfo
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- CN116377501A CN116377501A CN202310376710.3A CN202310376710A CN116377501A CN 116377501 A CN116377501 A CN 116377501A CN 202310376710 A CN202310376710 A CN 202310376710A CN 116377501 A CN116377501 A CN 116377501A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000001257 hydrogen Substances 0.000 title claims abstract description 53
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 150
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 74
- 238000007747 plating Methods 0.000 claims abstract description 62
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical compound [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 239000002184 metal Substances 0.000 claims abstract description 34
- 238000009713 electroplating Methods 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 230000007704 transition Effects 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 22
- 150000002815 nickel Chemical class 0.000 claims description 14
- -1 nickel fluoroborate Chemical compound 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- DAPUDVOJPZKTSI-UHFFFAOYSA-L ammonium nickel sulfate Chemical compound [NH4+].[NH4+].[Ni+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DAPUDVOJPZKTSI-UHFFFAOYSA-L 0.000 claims description 6
- 229930182817 methionine Natural products 0.000 claims description 6
- 235000006109 methionine Nutrition 0.000 claims description 6
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 5
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 5
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 229940079864 sodium stannate Drugs 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 3
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims description 3
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 3
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 3
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 3
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 claims description 3
- ROHFNLRQFUQHCH-UHFFFAOYSA-N Leucine Natural products CC(C)CC(N)C(O)=O ROHFNLRQFUQHCH-UHFFFAOYSA-N 0.000 claims description 3
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims description 3
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012190 activator Substances 0.000 claims description 3
- 235000004279 alanine Nutrition 0.000 claims description 3
- 235000013922 glutamic acid Nutrition 0.000 claims description 3
- 239000004220 glutamic acid Substances 0.000 claims description 3
- 235000005772 leucine Nutrition 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 235000013930 proline Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 9
- 231100000572 poisoning Toxicity 0.000 abstract description 4
- 230000000607 poisoning effect Effects 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 17
- 238000005238 degreasing Methods 0.000 description 11
- 230000004913 activation Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000956 alloy Substances 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 238000011010 flushing procedure Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005488 sandblasting Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910003962 NiZn Inorganic materials 0.000 description 1
- 229910018502 Ni—H Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 238000005422 blasting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- 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
-
- 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
- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
- C25B11/053—Electrodes comprising one or more electrocatalytic coatings on a substrate characterised by multilayer electrocatalytic coatings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention provides an electrocatalytic hydrogen evolution material, a preparation method and application thereof, and relates to the technical field of electrode materials. The preparation method of the electrocatalytic hydrogen evolution material provided by the invention comprises the following steps: sequentially electroplating a nickel transition layer and a nickel-tin active plating layer on the surface of the metal substrate to obtain a metal substrate coated with an active composite plating layer; and aging the metal substrate coated with the active composite coating to obtain the electrocatalytic hydrogen evolution material. The electrocatalytic hydrogen evolution material prepared by the invention has high activity and high stability under high current density, and simultaneously has better reverse current resistance and poisoning resistance, and is suitable for industrial alkaline water electrolysis hydrogen production technology.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to an electrocatalytic hydrogen evolution material and a preparation method and application thereof.
Background
The combustion of fossil fuels generates a large amount of pollutants and greenhouse gases, with the consequent environmental protection problem. Hydrogen is used as a green and efficient renewable energy source, has high energy density and wide sources, and is the most potential clean energy source for replacing fossil fuel. The alkaline water electrolysis hydrogen production technology is the most mature and commercialized electrolytic hydrogen production technology at present, and MW level has realized large-scale assembly and commercialized application. At present, the hydrogen production technology by alkaline water electrolysis in China still has a certain gap with foreign countries in technical indexes such as current density, direct current power consumption and the like, and is based on the fact that the autonomous research and development level of key materials and core components of the electrolytic cell is low. The reduction of hydrogen evolution overpotential is one of key points for improving the comprehensive performance of an alkaline electrolytic tank, and the development of a high-performance non-noble metal alloy catalyst with abundant reserves and low price is an important research direction for electrocatalytic hydrogen production.
The electron arrangement of the transition metal nickel (Ni) is 3d 8 4s 2 The catalyst has unpaired 3d electrons, can be paired with a hydrogen atom 1s orbit in the electrocatalytic reaction of hydrogen evolution, forms a Ni-H adsorption bond with moderate strength, and is favorable for continuous implementation of the electrocatalytic hydrogen evolution reaction. Under the alkaline medium condition, the metallic nickel has better strong alkali corrosion resistance and rich reserves, and is the most widely used non-noble metal hydrogen evolution material in the current alkaline electrolytic bath application. Researches show that the alloy (namely nickel-based alloy) formed by nickel and other metals can effectively improve the catalytic activity and stability of the electrocatalytic material due to electronic structure optimization of alloy materials, synergistic effect among metal elements and the like. At present, research on binary nickel-based nonmetallic alloys mainly focuses on NiZn, niAl, niCo, niMo and the like, however, under working conditions, it is difficult to combine two key properties of catalytic activity and stability.
Disclosure of Invention
The invention aims to provide an electrocatalytic hydrogen evolution material, a preparation method and application thereof, and the electrocatalytic hydrogen evolution material prepared by the invention has high activity and high stability under high current density, and simultaneously has better reverse current resistance and poisoning resistance, and is suitable for industrial electrocatalytic hydrogen production technology.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an electrocatalytic hydrogen evolution material, which comprises the following steps:
sequentially electroplating a nickel transition layer and a nickel-tin active plating layer on the surface of the metal substrate to obtain a metal substrate coated with an active composite plating layer;
and aging the metal substrate coated with the active composite coating to obtain the electrocatalytic hydrogen evolution material.
Preferably, the nickel plating solution adopted by the nickel-plating transition layer comprises 50-500 g/L of nickel salt and 10-300 g/L of activating agent;
the nickel salt comprises one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate;
the activating agent comprises one or more of sodium chloride, potassium chloride, magnesium chloride and hydrochloric acid.
Preferably, the pH value of the nickel plating solution is 2-6.2.
Preferably, the electroplating temperature of the electroplated nickel transition layer is 40-60 ℃; the current density is 0.1-50A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is 1-30 min.
Preferably, the nickel-tin electroplating solution used for the nickel-tin electroplating active coating comprises 10-500 g/L of nickel salt, 0.1-200 g/L of tin salt and 50-500 g/L of additive;
the nickel salt comprises one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate;
the tin salt comprises one or more of stannous sulfate, stannous chloride, sodium stannate, tin sulfate and tin chloride;
the additive comprises one or more of sodium citrate, potassium pyrophosphate, sodium tripolyphosphate, alanine, glutamic acid, methionine, leucine, methionine, proline, tryptophan, serine, tyrosine and glycine.
Preferably, the pH value of the nickel-tin electroplating solution is 7-10.
Preferably, the electroplating temperature of the electroplated nickel-tin active coating is 30-90 ℃; the current density is 0.1-50A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is 1-60 min.
Preferably, the temperature of the aging treatment is 50-250 ℃, and the heat preservation time is 2-24 hours.
The invention provides the electrocatalytic hydrogen evolution material prepared by the preparation method of the technical scheme, which comprises a metal base material, and a nickel transition layer and a nickel-tin active plating layer which are sequentially laminated on the surface of the metal base material.
The invention provides application of the electrocatalytic hydrogen evolution material in hydrogen production by water electrolysis.
The invention provides a preparation method of an electrocatalytic hydrogen evolution material, which comprises the following steps: sequentially electroplating a nickel transition layer and a nickel-tin active plating layer on the surface of the metal substrate to obtain a metal substrate coated with an active composite plating layer; and aging the metal substrate coated with the active composite coating to obtain the electrocatalytic hydrogen evolution material. The invention adopts a composite electroplating process to construct an active composite plating layer with a multilayer structure on a metal substrate, a top layer material adopts a nickel-tin-based alloy, and a nickel-based material is adopted as a transition layer between the top layer and the metal substrate. The introduction of the transition layer can improve the binding force between the nickel-tin active plating layer and the metal substrate and increase the stability of the nickel-tin active plating layer. The electrocatalytic hydrogen evolution material prepared by the invention has high activity and high stability under high current density, and simultaneously has better reverse current resistance and poisoning resistance, and is suitable for industrial alkaline water electrolysis hydrogen production technology.
Detailed Description
The invention provides a preparation method of an electrocatalytic hydrogen evolution material, which comprises the following steps:
sequentially electroplating a nickel transition layer and a nickel-tin active plating layer on the surface of the metal substrate to obtain a metal substrate coated with an active composite plating layer;
and aging the metal substrate coated with the active composite coating to obtain the electrocatalytic hydrogen evolution material.
The invention sequentially electroplates a nickel transition layer and a nickel-tin active plating layer on the surface of a metal substrate to obtain the metal substrate coated with the active composite plating layer. In the present invention, the metal substrate is preferably a nickel mesh. In the present invention, the metal substrate is preferably pretreated before electroplating; the pretreatment preferably includes blasting, degreasing, and hydrochloric acid activation performed sequentially. In the invention, the degreasing preferably adopts an electrolytic degreasing process; the oil removal time is preferably 5 to 20 minutes, more preferably 10 to 15 minutes. The invention preferably carries out water washing after the degreasing. The invention removes the greasy dirt on the surface of the metal substrate by degreasing. In the present invention, the mass concentration of the hydrochloric acid solution used for the activation of hydrochloric acid is preferably 10 to 50%, more preferably 30 to 40%. The present invention preferably performs water washing after the hydrochloric acid activation. The hydrochloric acid activation of the invention has the function of improving the binding force between the plating layer and the metal substrate.
In the invention, the nickel plating solution adopted for the nickel-plating transition layer preferably comprises 50-500 g/L of nickel salt and 10-300 g/L of activating agent; more preferably, the catalyst comprises 100 to 200g/L of nickel salt and 30 to 90g/L of activator. In the present invention, the nickel salt preferably includes one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate. In the present invention, the activator preferably includes one or more of sodium chloride, potassium chloride, magnesium chloride and hydrochloric acid. In the present invention, the pH of the nickel plating solution is preferably 2 to 6.2, more preferably 4.5 to 5.5. In the present invention, the solvent of the nickel plating solution is preferably pure water.
In the invention, the electroplating temperature of the electroplated nickel transition layer is preferably 40-60 ℃; the current density is preferably 0.1 to 50A/dm 2 More preferably 1 to 20A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is preferably 1 to 30 minutes, more preferably 3 to 15 minutes. In the invention, the cathode of the electroplated nickel transition layer is preferably nickel screen; the anode is preferably a nickel plate; the distance between the cathode and the anode is preferably 50 to 100cm.
According to the invention, through designing the geometric structure and chemical components of the nickel transition layer, the electronic structure and micro morphology of the top nickel-tin active plating layer can be adjusted, so that the electrocatalytic hydrogen evolution material shows higher apparent activity under the working condition.
In the invention, the nickel-tin plating solution used for plating the nickel-tin active plating layer preferably comprises 10-500 g/L of nickel salt, 0.1-200 g/L of tin salt and 50-500 g/L of additive; more preferably, the nickel salt comprises 50-150 g/L, tin salt 30-90 g/L and additive 200-400 g/L. In the present invention, the nickel salt preferably includes one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate. In the present invention, the tin salt preferably includes one or more of stannous sulfate, stannous chloride, sodium stannate, tin sulfate and tin chloride. In the present invention, the additive preferably includes one or more of sodium citrate, potassium pyrophosphate, sodium tripolyphosphate, alanine, glutamic acid, methionine, leucine, methionine, proline, tryptophan, serine, tyrosine and glycine. In the present invention, the pH of the nickel tin plating solution is preferably 7 to 10, more preferably 7.5 to 9. In the present invention, the solvent of the nickel tin plating solution is preferably pure water.
In the invention, the plating temperature of the nickel-tin electroplated active coating is preferably 30-90 ℃, more preferably 40-65 ℃; the current density is preferably 0.1 to 50A/dm 2 More preferably 1 to 20A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is preferably 1 to 60 minutes, more preferably 10 to 50 minutes. In the invention, the cathode of the electroplated nickel-tin active coating is preferably nickel screen; the anode is preferably a nickel plate; the distance between the cathode and the anode is preferably 50 to 100cm.
In the invention, after the nickel-tin active plating layer is electroplated, the obtained sample is dried in the air to obtain the metal substrate coated with the active composite plating layer.
After the metal base material covered with the active composite coating is obtained, the metal base material covered with the active composite coating is aged to obtain the electrocatalytic hydrogen evolution material. In the present invention, the temperature of the aging treatment is preferably 50 to 250 ℃, more preferably 50 to 150 ℃; the holding time is preferably 2 to 24 hours, more preferably 4 to 15 hours. In the present invention, the atmosphere of the aging treatment preferably includes one or more of argon, nitrogen, hydrogen and oxygen. The aging treatment of the invention has the effect of promoting the material to slowly change from amorphous to amorphous/crystalline structure, thus obtaining higher stability.
In the invention, the reverse current resistance, impurity poisoning resistance and electrochemical stability of the electrocatalytic hydrogen evolution material can be further improved by adjusting the parameters of nickel-tin active plating and aging treatment, and the comprehensive electrochemical performance reaches the international advanced level.
The invention provides the electrocatalytic hydrogen evolution material prepared by the preparation method of the technical scheme, which comprises a metal base material, and a nickel transition layer and a nickel-tin active plating layer which are sequentially laminated on the surface of the metal base material.
The invention provides application of the electrocatalytic hydrogen evolution material in hydrogen production by water electrolysis. In the present invention, the application preferably includes: in a three-electrode system, a counter electrode is a platinum net, a reference electrode is an Hg/HgO electrode, a working electrode is the electrocatalytic hydrogen evolution material, electrolyte is alkaline electrolyte of 1mol/L, and the reference electrode is contacted with the alkaline electrolyte through a salt bridge at the temperature of 75-80 ℃ to perform hydrogen evolution reaction.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
1. Surface pretreatment: the nickel screen is first surface pretreated by sand blasting.
2. Deoiling: removing the greasy dirt on the surface of the nickel screen by adopting an electrolytic degreasing process, wherein the degreasing time is 10min, taking out the degreased test piece, and flushing the greasy dirt attached to the surface by using clear water.
3. Activation of hydrochloric acid: immersing the deoiled test piece into a tank body containing hydrochloric acid solution, wherein the mass concentration of the hydrochloric acid solution is 30%, taking out the activated test piece after activation, and flushing the hydrochloric acid solution attached to the surface of the test piece with clear water.
4. And (3) composite electroplating: the active composite coating on the nickel net is prepared by adopting a two-step cathode plating method, and the plating solution formula and the technological parameters are as follows:
(1) Electroplating a nickel transition layer: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode at 50cm; the nickel plating solution is 110g/L nickel chloride, 50g/L hydrochloric acid and 40g/L sodium chloride, the pH value of the nickel plating solution is 4.5, the temperature of the nickel plating solution is 40 ℃, and the current density is 10A/dm 2 The deposition time was 10min.
(2) Electroplating nickel-tin active plating: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode at 50cm; the nickel-tin electroplating solution comprises 80g/L nickel chloride, 40g/L sodium stannate, 250g/L potassium pyrophosphate and 50g/L sodium citrate; the pH value of the nickel-tin electroplating solution is 8.0, the temperature of the nickel-tin electroplating solution is 50 ℃, and the current density is 4A/dm 2 The deposition time was 30min.
5. Aging: the volume ratio of nitrogen to oxygen is 4:1, drying the mixture gas at 60 ℃ for 12 hours to obtain the electrocatalytic hydrogen evolution material.
Electrochemical testing: in a three-electrode system (a counter electrode is a platinum net, a reference electrode is an Hg/HgO electrode, a working electrode is an electrocatalytic hydrogen evolution material), the electrolyte is 1mol/L alkaline electrolyte, the reference electrode is contacted with the electrolyte through a salt bridge at 80 ℃, and the electrocatalytic hydrogen evolution material prepared by testing is 0.5A/cm 2 The electrochemical performance was compared with that of commercial nickel screen under the same conditions. The test results showed that the flow rate was 0.5A/cm 2 At current density, HER performance was improved by 270mV compared to nickel mesh, oer performance was improved by 30mV compared to nickel mesh, and activity decay was less at 500h of run time.
Example 2
1. Surface pretreatment: the nickel screen is first surface pretreated by sand blasting.
2. Deoiling: removing the greasy dirt on the surface of the nickel screen by adopting an electrolytic degreasing process, wherein the degreasing time is 15min, taking out the degreased test piece, and flushing the greasy dirt attached to the surface by using clear water.
3. Activation of hydrochloric acid: immersing the deoiled test piece into a tank body containing hydrochloric acid solution, wherein the mass concentration of the hydrochloric acid solution is 40%, taking out the activated test piece after activation, and flushing the hydrochloric acid solution attached to the surface of the test piece with clear water.
4. And (3) composite electroplating: the active composite coating on the nickel net is prepared by adopting a two-step cathode plating method, and the plating solution formula and the technological parameters are as follows:
(1) Electroplating a nickel transition layer: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode at 80cm; 150g/L nickel sulfate, 70g/L hydrochloric acid and 60g/L potassium chloride, the pH value of the nickel plating solution is 5, the temperature of the nickel plating solution is 50 ℃, and the current density is 5A/dm 2 The deposition time was 5min.
(2) Electroplating nickel-tin active plating: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode at 80cm; the nickel-tin electroplating solution comprises 100g/L nickel pyrophosphate, 60g/L stannous sulfate, 300g/L potassium pyrophosphate and 60g/L glycine; the pH value of the nickel-tin electroplating solution is 8.5, the temperature of the nickel-tin electroplating solution is 55 ℃, and the current density is 5A/dm 2 The deposition time was 25min.
5. Aging: the volume ratio of nitrogen to hydrogen is 4: and 1, drying the mixture gas at 80 ℃ for 6 hours to obtain the electrocatalytic hydrogen evolution material.
The electrochemical test method of example 1 was used at 0.5A/cm 2 At current density, HER performance was increased by 250mV compared to nickel mesh and oer performance was increased by 50mV compared to nickel mesh with minimal activity decay at 500h of run time.
Example 3
1. Surface pretreatment: the nickel screen is first surface pretreated by sand blasting.
2. Deoiling: removing the greasy dirt on the surface of the nickel screen by adopting an electrolytic degreasing process, wherein the degreasing time is 15min, taking out the degreased test piece, and flushing the greasy dirt attached to the surface by using clear water.
3. Activation of hydrochloric acid: immersing the deoiled test piece into a tank body containing hydrochloric acid solution, wherein the mass concentration of the hydrochloric acid solution is 40%, taking out the activated test piece after activation, and flushing the hydrochloric acid solution attached to the surface of the test piece with clear water.
4. And (3) composite electroplating: the active composite coating on the nickel net is prepared by adopting a two-step cathode plating method, and the plating solution formula and the technological parameters are as follows:
(1) Electroplating a nickel transition layer: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode as 100cm; the nickel plating solution is 180g/L nickel sulfate, 70g/L hydrochloric acid and 60g/L sodium chloride, the pH value of the nickel plating solution is 4.5, the temperature of the nickel plating solution is 40 ℃, and the current density is 1.5A/dm 2 The deposition time was 3min.
(2) Electroplating nickel-tin active plating: taking a nickel screen as a cathode, taking a nickel plate as an anode, and keeping the distance between the cathode and the anode as 100cm; the nickel-tin electroplating solution comprises 100g/L of nickel chloride, 60g/L of stannous sulfate, 300g/L of sodium pyrophosphate and 70g/L of sodium tripolyphosphate; the pH value of the nickel-tin electroplating solution is 8.5, the temperature of the nickel-tin electroplating solution is 55 ℃, and the current density is 8A/dm 2 The deposition time was 15min.
5. Aging: the volume ratio of nitrogen, oxygen and hydrogen is 5:1: and 1, drying the mixture gas at 180 ℃ for 4 hours to obtain the electrocatalytic hydrogen evolution material.
The electrochemical test method of example 1 was used at 0.5A/cm 2 At current density, HER performance was improved by 230mV compared to nickel mesh and oer performance was improved by 10mV compared to nickel mesh with minimal activity decay at 500h of run time.
Comparative example
The preparation process was substantially the same as that of example 3, except that the nickel transition layer was not electroplated.
The electrochemical test method of example 1 was used at 0.5A/cm 2 Under the current density, HER performance is improved by 210mV compared with the nickel screen, OER performance is improved by 10mV compared with the nickel screen, the slag drop phenomenon of the test piece is serious, and the performance attenuation is serious under the running time of 500 h.
As can be seen from the test results of the examples and the comparative examples, the invention adopts the composite electroplating process of the nickel transition layer and the nickel tin active plating layer, and can improve the activity and stability of the electrocatalytic hydrogen evolution material.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the electrocatalytic hydrogen evolution material comprises the following steps:
sequentially electroplating a nickel transition layer and a nickel-tin active plating layer on the surface of the metal substrate to obtain a metal substrate coated with an active composite plating layer;
and aging the metal substrate coated with the active composite coating to obtain the electrocatalytic hydrogen evolution material.
2. The preparation method of claim 1, wherein the nickel plating solution used for the nickel-plating transition layer comprises 50-500 g/L nickel salt and 10-300 g/L activator;
the nickel salt comprises one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate;
the activating agent comprises one or more of sodium chloride, potassium chloride, magnesium chloride and hydrochloric acid.
3. The method according to claim 2, wherein the pH of the nickel plating solution is 2 to 6.2.
4. The method according to claim 1 or 2, wherein the electroplating temperature of the electroplated nickel transition layer is 40-60 ℃; the current density is 0.1-50A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is 1-30 min.
5. The preparation method of claim 1, wherein the nickel-tin plating solution used for the nickel-tin plating comprises 10-500 g/L nickel salt, 0.1-200 g/L tin salt and 50-500 g/L additive;
the nickel salt comprises one or more of nickel chloride, nickel sulfate, nickel fluoroborate, nickel sulfamate, nickel pyrophosphate and nickel ammonium sulfate;
the tin salt comprises one or more of stannous sulfate, stannous chloride, sodium stannate, tin sulfate and tin chloride;
the additive comprises one or more of sodium citrate, potassium pyrophosphate, sodium tripolyphosphate, alanine, glutamic acid, methionine, leucine, methionine, proline, tryptophan, serine, tyrosine and glycine.
6. The method according to claim 5, wherein the pH of the nickel-tin plating solution is 7 to 10.
7. The method according to claim 1 or 5, wherein the plating temperature of the nickel-tin plating active layer is 30 to 90 ℃; the current density is 0.1-50A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The deposition time is 1-60 min.
8. The preparation method according to claim 1, wherein the aging treatment is carried out at a temperature of 50-250 ℃ for a holding time of 2-24 hours.
9. The electrocatalytic hydrogen evolution material prepared by the preparation method of any one of claims 1 to 8, which comprises a metal substrate, and a nickel transition layer and a nickel-tin active plating layer which are sequentially laminated on the surface of the metal substrate.
10. The use of the electrocatalytic hydrogen evolution material of claim 9 in the production of hydrogen by electrolysis of water.
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