CN106702419A - Ni-S-W-C hydrogen evolution electrode and preparation method thereof - Google Patents
Ni-S-W-C hydrogen evolution electrode and preparation method thereof Download PDFInfo
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- CN106702419A CN106702419A CN201710025671.7A CN201710025671A CN106702419A CN 106702419 A CN106702419 A CN 106702419A CN 201710025671 A CN201710025671 A CN 201710025671A CN 106702419 A CN106702419 A CN 106702419A
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- hydrogen
- preparation
- plating
- hydrogen evolution
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- 238000002360 preparation method Methods 0.000 title claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title abstract description 53
- 229910052739 hydrogen Inorganic materials 0.000 title abstract description 53
- 239000001257 hydrogen Substances 0.000 title abstract description 53
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- 238000009713 electroplating Methods 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 238000007747 plating Methods 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 20
- 238000000576 coating method Methods 0.000 claims description 20
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- 239000008139 complexing agent Substances 0.000 claims description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004472 Lysine Substances 0.000 claims description 9
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 8
- 229940081974 saccharin Drugs 0.000 claims description 8
- 235000019204 saccharin Nutrition 0.000 claims description 8
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 8
- 239000006258 conductive agent Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 150000003863 ammonium salts Chemical class 0.000 claims description 5
- 150000002815 nickel Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000011247 coating layer Substances 0.000 abstract description 7
- 239000007772 electrode material Substances 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000005868 electrolysis reaction Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000004070 electrodeposition Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910020350 Na2WO4 Inorganic materials 0.000 description 5
- 238000007605 air drying Methods 0.000 description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- YCPXWRQRBFJBPZ-UHFFFAOYSA-N 5-sulfosalicylic acid Chemical class OC(=O)C1=CC(S(O)(=O)=O)=CC=C1O YCPXWRQRBFJBPZ-UHFFFAOYSA-N 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910017112 Fe—C Inorganic materials 0.000 description 2
- 229910017263 Mo—C Inorganic materials 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical class [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- 229910000564 Raney nickel Inorganic materials 0.000 description 1
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Inorganic materials [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 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
- 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- 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
-
- 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)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention provides a Ni-S-W-C hydrogen evolution electrode comprising a nickel base body and a Ni-S-W-C coating layer deposited on the surface of the nickel base body. The Ni-S-W-C coating layer comprises, by weight, 50%-80% of Ni, 5%-20% of S, 0.1%-1.5% of W and the balance C. The W and C elements are added to a Ni-S coating layer to form the Ni-S-W-C coating layer. The Ni-S-W-C coating layer has low hydrogen evolution over potentiality, high hydrogen evolution catalytic activity and excellent stability and can be widely used as an alkaline water electrolysis hydrogen evolution electrode material. According to the embodiment, the Ni-S-W-C hydrogen evolution electrode provided by the invention has the hydrogen evolution over potentiality being 270mV, the apparent current density being 5.27x10<2> mA/cm<2>, and has higher hydrogen evolution catalytic activity.
Description
Technical field
The present invention relates to electrocatalytic hydrogen evolution technical field, more particularly to a kind of Ni-S-W-C hydrogen-precipitating electrodes and its preparation side
Method.
Background technology
Hydrogen Energy has the advantages that rich reserves, wide material sources, energy density be high, cleaning because of it, and is considered as a kind of excellent
Different energy carrier, has caused the extensive concern of countries in the world at present.On a large scale, at low cost hydrogen making using Hydrogen Energy
Precondition.In numerous hydrogen producing technologies, water electrolysis hydrogen producing has that simple to operate, hydrogen purity is high, energy efficiency it is high (>=
70%) the advantages of, raw material sources are extensive, is currently a kind of ripe Process of Hydrogen Production, and its hydrogen manufacturing amount accounts for total hydrogen manufacturing amount
4%.But the overpotential of hydrogen evolution of the method high energy consumption, wherein cathode material is the principal element for influenceing energy consumption.Your gold such as Pt, Pd
Although category is with relatively low overpotential of hydrogen evolution, but its reserves is limited, and price is higher, it is difficult to heavy industrialization application.Cause
This, researches and develops a kind of inexpensive, low overpotential of hydrogen evolution hydrogen-precipitating electrode and has important practical significance and practical value.
In the prior art, Ni alloys have the advantages that catalysis activity is high, it is simple to make, low cost because of it, make it as weight
The catalytic hydrogen evolution material wanted and widely paid close attention to.However, the overpotential of hydrogen evolution still phase of current Ni alloy hydrogen-precipitating electrodes
To higher, such as HashiWto is disclosed and is introduced C element in Ni-Mo alloys, is conducive to refining grain size and is suppressed Mo units
The dissolution of element, enhances Ni-Mo-C hydrogen-precipitating electrodes catalytic activity for hydrogen evolution and anti-power-off performance, and overpotential of hydrogen evolution is in 100mA/cm2
When be only 200mV (referring to《Nanocrystalline electrodeposited Ni-Mo-C cathodes for
hydrogen production》,K HashiWto,T Sasaki,S Meguro,et al.,Materials Science
and Engineering A,2004,375-377:942-945)；Jiang etc. discloses one kind prepared by with lysine as carbon source
Ni-Fe-C hydrogen-precipitating electrodes method：After C element enters Ni-Fe alloys, the crystallite dimension of alloy is refined, increased alloy
The surface energy of particle, so that surface atom has activity higher, and then reduces overpotential of hydrogen evolution, and its overpotential of hydrogen evolution is
65mV (referring to《Study on Ni-Fe-C cathode for hydrogen evolution from seawater
electrolysis》,Nan Jiang,Hui-Min Meng,Li-Jun Song,et al.,International Journal
of Hydrogen Energy,2010,35:8056-8062)。
The content of the invention
In view of this, it is an object of the invention to provide a kind of Ni-S-W-C hydrogen-precipitating electrodes, the liberation of hydrogen of hydrogen-precipitating electrode is improved
Catalysis activity, reduces the overpotential of hydrogen evolution of hydrogen-precipitating electrode.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of Ni-S-W-C hydrogen-precipitating electrodes, including Ni substrate and the Ni-S-W-C coating for being deposited on the Ni substrate surface,
The Ni-S-W-C coating includes the component of following weight percentage：Ni：50~80%, S：5~20%, W：0.1~
1.5%, the C of surplus.
Preferably, described Ni-S-W-C coating includes the component of following weight percentage：Ni：60~70%, S：10
~15%, W：0.5~1%, the C of surplus.
Preferably, the thickness of described Ni-S-W-C coating is 20~50 μm.
Present invention also offers the preparation method of the Ni-S-W-C hydrogen-precipitating electrodes described in above-mentioned technical proposal, including following step
Suddenly：
(1) electroplating aqueous solution is provided, the electroplating aqueous solution includes the component of following concentration：80~160g/L of nickel source, sulphur
80~130g/L of urea, 10~45g/L of tungsten source, 1~5g/L of lysine, complexing agent 60~100g/L, H3BO320~60g/L, it is conductive
20~60g/L of agent, 0.5~5.0g/L of saccharin, 5~30g/L of sulfosalicylic acid；
(2) with Ni substrate as cathode and anode, distance between cathode and anode is 0.5~3.0cm, is obtained with the step (1)
Electroplating aqueous solution is electroplated, and obtains Ni-S-W-C hydrogen-precipitating electrodes.
Preferably, in the step (2) in electroplating process, the temperature of electroplating aqueous solution is 30~60 DEG C, the plating
Time is 30~90min.
Preferably, the current density of plating is 2~6A/dm in the step (2)2, the pulse frequency of the plating is 50
~250Hz, the dutycycle of the plating is 0.30~0.85.
Preferably, nickel source includes the mixture of one or more in water soluble nickel salt in the step (1).
Preferably, tungsten source includes the mixture of one or more in soluble tungstate salt in the step (1).
Preferably, step (1) complexing agent includes Na3C6H5O7And/or (NH4)3C6H5O7。
Preferably, conductive agent includes alkali metal inorganic salts and/or soluble ammonium salt in the step (1).
The invention provides a kind of Ni-S-W-C hydrogen-precipitating electrodes, including Ni substrate and it is deposited on the Ni substrate surface
Ni-S-W-C coating, the Ni-S-W-C coating includes the component of following weight percentage：Ni：50~80%, S：5~
20%, W：0.1~1.5%, the C of surplus.The present invention is plated using formation Ni-S-W-C during W, C element are doped into Ni-S coating
Layer, Ni-S-W-C coating has relatively low overpotential of hydrogen evolution, catalytic activity for hydrogen evolution higher and excellent stability, can widely make
It is alkaline water electrolytic hydrogen evolution electrode material, the Ni-S-W-C hydrogen-precipitating electrode overpotential of hydrogen evolution provided from embodiment, the application
It is 270mV, apparent current density is 5.27 × 10-2mA/cm2, with catalytic activity for hydrogen evolution higher.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the surface topography and energy spectrum diagram of Ni-S-W-C hydrogen-precipitating electrodes obtained in the embodiment of the present invention 1；
Fig. 2 is Ni-S-W-C hydrogen-precipitating electrodes liberation of hydrogen linear scan curve obtained in the embodiment of the present invention.
Specific embodiment
The invention provides a kind of Ni-S-W-C hydrogen-precipitating electrodes, including Ni substrate and it is deposited on the Ni substrate surface
Ni-S-W-C coating, the Ni-S-W-C coating includes the component of following weight percentage：Ni：50~80%, S：5~
20%, W：0.1~1.5%, the C of surplus.
The Ni-S-W-C hydrogen-precipitating electrodes that the present invention is provided include Ni substrate electrode.The present invention does not have to the source of the Ni substrate
There is any special limitation, using commercial goods well known to those skilled in the art；Shape of the present invention to the Ni substrate
Shape does not have any special limitation, according to being selected the need for those skilled in the art；The Ni substrate is excellent in the present invention
Elect nickel foam, Raney's nickel and nickel plate as.
The Ni-S-W-C hydrogen-precipitating electrodes that the present invention is provided include being deposited on the Ni-S-W-C platings of the Ni substrate electrode surface
Layer, the Ni-S-W-C coating includes the Ni simple substance that weight/mass percentage composition is 50~80%, preferably 60~70%.
In the present invention, the Ni-S-W-C coating includes the S components that weight/mass percentage composition is 5~20%, preferably 10
~15%.
In the present invention, the Ni-S-W-C coating includes the W components that weight/mass percentage composition is 0.1~1.5%, preferably
0.5~1%.
In the present invention, the thickness of the Ni-S-W-C coating is preferably 20~50 μm, more preferably 25~35 μm.
Present invention also offers the preparation method of the Ni-S-W-C hydrogen-precipitating electrodes described in above-mentioned technical proposal, including following step
Suddenly：
(1) electroplating aqueous solution is provided, the electroplating aqueous solution includes the component of following concentration：80~160g/L of nickel source, sulphur
80~130g/L of urea, 10~45g/L of tungsten source, 1~5g/L of lysine, complexing agent 60~100g/L, H3BO320~60g/L, it is conductive
20~60g/L of agent, 0.5~5.0g/L of saccharin, 5~30g/L of sulfosalicylic acid；
(2) with Ni substrate as cathode and anode, distance between cathode and anode is 0.5~3.0cm, is obtained with the step (1)
Electroplating aqueous solution is electroplated, and obtains Ni-S-W-C hydrogen-precipitating electrodes.
The present invention provides electroplating aqueous solution, and the electroplating aqueous solution includes the component of following concentration：80~160g/L of nickel source,
80~130g/L of thiocarbamide, 10~45g/L of tungsten source, 1~5g/L of lysine, complexing agent 60~100g/L, H3BO320~60g/L, leads
Electric 20~60g/L of agent, 0.5~5.0g/L of saccharin, 5~30g/L of sulfosalicylic acid.
In the present invention, the pH value of the electroplating aqueous solution is preferably 3~5, more preferably 4.0~4.5.
In the present invention, nickel source of the electroplating aqueous solution including 80~160g/L, more preferably 100~150g/L, most
Preferably 120~140g/L.In the present invention, the nickel source includes the mixture of one or more in water soluble nickel salt, institute
State water soluble nickel salt and preferably include NiSO4·6H2O、Ni(NO3)2·6H2O and NiCl2·6H2O, when the nickel source includes two kinds
During material, preferably NiSO4·6H2O and Ni (NO3)2·6H2The mixture of O, the present invention is to each water-soluble nickel in the mixture
The quality of salt does not have any special limitation, and those skilled in the art can according to actual needs select the water solubility of any mass ratio
The mixture of nickel salt；NiSO in embodiments of the present invention4·6H2O and Ni (NO3)2·6H2The mass ratio of O is preferably 1~3：1, more
Preferably 1.5~2：1.
In the present invention, the electroplating aqueous solution includes the thiocarbamide of 80~130g/L, more preferably 100~120g/L.
In the present invention, tungsten source of the electroplating aqueous solution including 10~45g/L, more preferably 5~25g/L, most preferably
It is 15~20g/L.In the present invention, the tungsten source include soluble tungstate salt in the mixture of one or more, it is described can
Dissolubility tungstates preferably includes Na2WO4·2H2O and (NH4)2WO4·2H2O, when the tungsten source includes two kinds of materials, preferably
Na2WO4·2H2O and (NH4)2WO4·2H2The mixture of O, the present invention does not have to the quality in each water-soluble tungsten source in the mixture
There is any special limitation, those skilled in the art can according to actual needs select the mixing of the water-soluble tungsten salt of any mass ratio
Thing；Na in embodiments of the present invention2WO4·2H2O and (NH4)2WO4·2H2The mass ratio of O is preferably 1~4:1, more preferably 2
~3:1.
In the present invention, the electroplating aqueous solution includes the lysine of 1~5g/L, more preferably 2~3g/L.
In the present invention, the electroplating aqueous solution includes the complexing agent of 60~100g/L, more preferably 70~80g/L.
In the present invention, the complexing agent preferably includes Na3C6H5O7·2H2O and/or (NH4)3C6H5O7·2H2O, when the complexing agent bag
When including the mixture of two kinds of materials, the present invention does not have any special limitation to the quality of each complexing agent in the mixture, this
Art personnel can according to actual needs select the mixture of the complexing agent of any mass ratio；In embodiments of the present invention
Na3C6H5O7·2H2O and (NH4)3C6H5O7·2H2The mass ratio of O is preferably 1~4:1, more preferably 2~3:1.
In the present invention, the electroplating aqueous solution includes the H of 20~60g/L3BO3, more preferably 25~40g/L, most preferably
It is 30~35g/L.
In the present invention, the electroplating aqueous solution includes the conductive agent of 20~60g/L, and more preferably 30~50g/L is optimal
Elect 35~45g/L as.In the present invention, the conductive agent includes alkali metal inorganic salts and/or soluble ammonium salt, the alkali metal
Inorganic salts preferably include NaCl, KCl, NaNO3And KNO3, the soluble ammonium salt preferably includes NH4Cl and NH4NO3, led when described
When electric agent includes the mixture of two kinds in alkali metal inorganic salts and soluble ammonium salt, preferably NaCl and NH4The mixture of Cl,
The present invention does not have any special limitation to the quality of each conductive agent in the mixture, and those skilled in the art can be according to reality
The mixture of the conductive agent for needing to select any mass ratio；NH in embodiments of the present invention4Cl and NH4NO3Mass ratio be preferably
1~3：1, more preferably 2~2.5：1.
In the present invention, the electroplating aqueous solution includes the saccharin of 0.5~5.0g/L, more preferably 1~1.5g/L.
In the present invention, the electroplating aqueous solution includes the sulfosalicylic acid of 5~30g/L, more preferably 10~15g/L.
The present invention does not have any special restriction to the preparation method of the electroplating aqueous solution, using those skilled in the art
Conventional meanses.In embodiments of the present invention, after preferably each component in electroplating aqueous solution is well mixed, water is added
Obtain electroplating aqueous solution.
The present invention originates without any restriction to each raw material, using commercially available business well known to those skilled in the art
Product.
After obtaining electroplating aqueous solution, with Ni substrate as cathode and anode, the distance between cathode and anode is 0.5~3cm to the present invention, is used
The electroplating aqueous solution is electroplated, and obtains Ni-S-W-C hydrogen-precipitating electrodes.
In the present invention, before the plating preferred pair Ni substrate polished successively, oil removing and pickling, the polishing is preferred
For：The oxide that mechanical grinding removes surface is carried out to Ni substrate, is cleaned up with deionized water after making its metal luster；Institute
Oil removing preferably electrochemical deoiling is stated, is preferably specially：10~30min of sonic oscillation carries out chemistry and removes in inorganic caustic solutions
Oil, the inorganic caustic solutions preferably include the component of following mass concentration：15g/L NaOH、60g/L Na3PO4·12H2O、
25g/L Na2CO3With 15g/L Na2SiO3, it is described ultrasound time be preferably 15~20min；Then it is dry with deionized water rinsing
Only；The pickling is preferably：5~20min of etch, the quality of the hydrochloric acid are boiled in the hydrochloric acid that mass concentration is 20~40%
Concentration is preferably 25~30%, and the etch time is preferably 10~15min.After the pickling, the present invention will preferably be obtained
Ni substrate deionized water rinses rear natural air drying well.
In the present invention, the distance between the cathode and anode is preferably 0.5~3cm, more preferably 2~2.5cm.
In the present invention, the plating is preferably pulse electrodeposition；In the electroplating process, the temperature of electroplating aqueous solution
Preferably 30~60 DEG C, most preferably more preferably 35~50 DEG C, 40~45 DEG C；The time of the plating is preferably 30~
90min, more preferably 50~70min, most preferably 60~65min.
In the present invention, the current density of the plating is preferably 2~6A/dm2, more preferably 3~4A/dm2；The electricity
The pulse frequency of plating is preferably 50~250Hz, more preferably 100~150Hz；The dutycycle of the plating is preferably 0.30~
0.85, more preferably 0.4~0.5.
Present invention also offers application of the Ni-S-W-C hydrogen-precipitating electrodes in chlorine industry, electrochemical hydrogen storage.
The invention provides a kind of Ni-S-W-C hydrogen-precipitating electrodes, including Ni substrate and it is deposited on the Ni substrate surface
Ni-S-W-C coating, the Ni-S-W-C coating includes the simple substance of following weight percentage：Ni：50~80%, S：5~
20%, W：0.1~1.5%, the C of surplus.The present invention is plated using formation Ni-S-W-C during W, C element are doped into Ni-S coating
Layer, Ni-S-W-C coating has relatively low overpotential of hydrogen evolution, catalytic activity for hydrogen evolution higher and excellent stability, can widely make
It is alkaline water electrolytic hydrogen evolution electrode material, the Ni-S-W-C hydrogen-precipitating electrode overpotential of hydrogen evolution provided from embodiment, the application
It is 270mA, apparent current density is 5.27 × 10-2mA/cm2, with catalytic activity for hydrogen evolution higher.
Ni-S-W-C hydrogen-precipitating electrodes provided the present invention with reference to embodiment and preparation method thereof are carried out specifically
It is bright, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) pretreatment of Ni matrixes
The oxide that mechanical grinding removes surface is carried out to Ni pieces first, is cleaned with deionized water after making its metal luster
Totally；Then sonic oscillation 20min carries out electrochemical deoiling in alkali lye and absolute ethyl alcohol respectively, and wherein alkali lye is 15g/L
NaOH、60g/L Na3PO4·12H2O、25g/L Na2CO3And 15g/LNa2SiO3Mixed aqueous solution；Then deionized water is used
Rinse well, in 20% hydrochloric acid, boil deionized water rinsing after etch 5 minutes it is clean after natural air drying, immersion absolute ethyl alcohol is molten
It is standby in liquid；
(2) pulse electrodeposition prepares Ni-S-W-C hydrogen-precipitating electrodes
Using double anode list cathode systems, the Ni matrixes handled well with step (1) are as cathode and anode.Ni-S-W-C plating solutions
Composition：140g/L NiSO4·6H2O, 100g/L thiocarbamide, 15g/L Na2WO4·2H2O, 1g/L lysine, 70g/L
Na3C6H5O7·2H2O, 40g/L H3BO3, 20g/L NaCl, 1.5g/L saccharin, 5g/L sulfosalicylic acids, the pH value of plating solution is 4,
Bath temperature is 45 DEG C；Pulse peak current density is 2A/dm2, dutycycle is 0.85, and pulse frequency is 100Hz, during electro-deposition
Between be 60min.Plating uses deionized water rinsing after terminating, and to remove residual plating solution, natural air drying is obtained Ni-S-W-C electrodes, its
Surface topography and power spectrum are as shown in Figure 1.
As seen from Figure 1, Ni-S-W-C electrode surfaces generation island is raised, with larger specific surface area, is conducive to
The avtive spot of electrode is exposed, catalysis activity is improved.
(3) Ni-S-W-C hydrogen evolution electrode materials Hydrogen Evolution Performance test：Using electrochemical workstation (CHI660B, Shanghai Hua Chen
Instrument company), electrochemical property test is carried out to the Ni-S-W-C hydrogen evolution electrode materials for preparing in three-electrode system.Work electricity
Pole Ni-S-W-C hydrogen evolution electrode materials (area is 1cm2, and the electrode back side is sealed with epoxy resin), auxiliary electrode is platinized platinum, reference electricity
Extremely saturated calomel electrode (Saturated calomel electrode, SCE).Using the KOH solution of mass ratio 30% as electricity
Solution liquid, temperature is 25 DEG C, and sweep speed under the conditions of 1mV/s to test its liberation of hydrogen linear scan curve, and curve is as shown in Figure 2.
Embodiment 2
Step (1) is with step (1) in embodiment 1；
(2) pulse electrodeposition prepares Ni-S-W-C hydrogen-precipitating electrodes
Using double anode list cathode systems, the nickel sheet handled well with step (1) is as cathode and anode.The group of Ni-S-W-C plating solutions
Into：120g/L NiSO4·6H2O, 80g/L thiocarbamide, 10g/L Na2WO4·2H2O, 3g/L lysine, 80g/L Na3C6H5O7·
2H2O, 40g/L H3BO3, 20g/L NaCl, 1.5g/L saccharin, 5g/L sulfosalicylic acids, the pH value of plating solution is 3, and bath temperature is
50℃；Pulse peak current density is 1A/dm2, dutycycle is 0.85, and pulse frequency is 100Hz, and electrodeposition time is 70min.
Plating uses deionized water rinsing after terminating, and to remove residual plating solution, natural air drying is obtained Ni-S-W-C hydrogen-precipitating electrodes.
Step (3) is with step (3) in embodiment 1, and the liberation of hydrogen linear scan curve for measuring is as shown in Figure 2.
Embodiment 3
Step (1) is with step (1) in embodiment 1；
(2) pulse electrodeposition prepares Ni-S-W-C hydrogen-precipitating electrodes
Using double anode list cathode systems, the nickel sheet handled well with step (1) is as cathode and anode.The group of Ni-S-W-C plating solutions
Into：90g/L NiSO4·6H2O, 110g/L thiocarbamide, 35g/L Na2WO4·2H2O, 2g/L lysine, 100g/L Na3C6H5O7·
2H2O, 40g/L H3BO3, 20g/L NaCl, 1.5g/L saccharin, 5g/L sulfosalicylic acids, the pH value of plating solution is 5, and bath temperature is
35℃；Pulse peak current density is 3A/dm2, dutycycle is 0.85, and pulse frequency is 100Hz, and electrodeposition time is 80min.
Plating uses deionized water rinsing after terminating, and to remove residual plating solution, natural air drying is obtained Ni-S-W-C hydrogen-precipitating electrodes.
Step (3) is with step (3) in embodiment 1, and the liberation of hydrogen linear scan curve for measuring is as shown in Figure 2.
As seen from Figure 2, the overpotential of hydrogen evolution of embodiment 1,2 and 3 is much smaller than Ni-S electrodes, according to Tafel formula
Calculate and understand, the apparent current density of embodiment 1,2,3 and Ni-S hydrogen-precipitating electrodes is respectively 5.27 × 10-2、2.22×10-2、
3.91×10-2With 2.69 × 10-3mA/cm2, show that Ni-S-W-C electrodes have catalytic activity for hydrogen evolution higher.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of Ni-S-W-C hydrogen-precipitating electrodes, including Ni substrate and the Ni-S-W-C coating for being deposited on the Ni substrate surface, institute
State simple substance of the Ni-S-W-C coating including following weight percentage：Ni：50~80%, S：5~20%, W：0.1~1.5%,
The C of surplus.
2. Ni-S-W-C hydrogen-precipitating electrodes according to claim 1, it is characterised in that described Ni-S-W-C coating include with
The component of lower weight percentage：Ni：60~70%, S：10~15%, W：0.5~1%, the C of surplus.
3. Ni-S-W-C hydrogen-precipitating electrodes according to claim 1, it is characterised in that the thickness of described Ni-S-W-C coating
It is 20~50 μm.
4. the preparation method of the Ni-S-W-C hydrogen-precipitating electrodes described in claim 1 or 2, comprises the following steps：
(1) electroplating aqueous solution is provided, the electroplating aqueous solution includes the component of following concentration：80~160g/L of nickel source, thiocarbamide 80
~130g/L, 10~45g/L of tungsten source, 1~5g/L of lysine, complexing agent 60~100g/L, H3BO320~60g/L, conductive agent 20
~60g/L, 0.5~5.0g/L of saccharin, 5~30g/L of sulfosalicylic acid；
(2) with Ni substrate as cathode and anode, the distance between cathode and anode is 0.5~3.0cm, the plating obtained with the step (1)
The aqueous solution is electroplated, and obtains Ni-S-W-C hydrogen-precipitating electrodes.
5. preparation method according to claim 4, it is characterised in that in the electroplating process of the step (2), electroplates water-soluble
The temperature of liquid is 30~60 DEG C, and the time of the plating is 30~90min.
6. the preparation method according to claim 4 or 5, it is characterised in that the current density of plating is in the step (2)
2~6A/dm2, the pulse frequency of the plating is 50~250Hz, and the dutycycle of the plating is 0.30~0.85.
7. preparation method according to claim 4, it is characterised in that nickel source includes water soluble nickel salt in the step (1)
In the mixture of one or more.
8. preparation method according to claim 4, it is characterised in that tungsten source includes soluble wolframic acid in the step (1)
The mixture of one or more in salt.
9. preparation method according to claim 4, it is characterised in that step (1) complexing agent includes Na3C6H5O7
And/or (NH4)3C6H5O7。
10. preparation method according to claim 4, it is characterised in that in the step (1) conductive agent include alkali metal without
Machine salt and/or soluble ammonium salt.
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