CN108796535A - One kind having three metallic coppers-cobalt-molybdenum/nickel foam porous electrode material and the preparation method and application thereof - Google Patents
One kind having three metallic coppers-cobalt-molybdenum/nickel foam porous electrode material and the preparation method and application thereof Download PDFInfo
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- CN108796535A CN108796535A CN201810532644.3A CN201810532644A CN108796535A CN 108796535 A CN108796535 A CN 108796535A CN 201810532644 A CN201810532644 A CN 201810532644A CN 108796535 A CN108796535 A CN 108796535A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 91
- 239000006260 foam Substances 0.000 title claims abstract description 84
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 17
- 239000010941 cobalt Substances 0.000 claims abstract description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- -1 molybdenum salt compound Chemical class 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 150000002739 metals Chemical class 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 27
- 239000001257 hydrogen Substances 0.000 claims description 27
- 239000002243 precursor Substances 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 150000001868 cobalt Chemical class 0.000 claims description 6
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 5
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 150000002751 molybdenum Chemical class 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 235000016768 molybdenum Nutrition 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 239000007809 chemical reaction catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 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
- 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
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
-
- 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
-
- 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)
- 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)
- Catalysts (AREA)
Abstract
The invention discloses one kind having three Ni metal-Co-Mo/ nickel foam porous electrode materials and the preparation method and application thereof, and this method includes：1) it defoams nickel surface greasy dirt and oxide layer first with organic solution and acid；2) copper, cobalt, molybdenum salt compound presoma and nickel foam are collectively disposed at confined reaction in autoclave, are washed out drying, obtain the nickel foam for having hydrothermal synthesis product in surface growth；3) by nickel foam obtained by step (2) in H2Atmosphere high temperature is calcined, and subsequent natural cooling is to get to having the three porous electrolysis water catalyst of Ni metal-Co-Mo/ nickel foams.The binding ability of three metal alloys and substrate nickel by force, under alkaline condition stablize by performance in the composite material, and has larger electrochemical surface area, greatly improves the catalytic activity of material；The preparation method realizes the combination of three metals and foam nickel base by solvent-thermal method, and preparation process is simple, sintering temperature is low, low energy consumption in preparation process, is convenient for industrialized production.
Description
Technical field
The present invention relates to electrolysis water catalytic hydrogen evolution technical fields, and in particular to one kind having three metallic coppers-cobalt-molybdenum (Cu-
Co-Mo)/nickel foam porous electrode material and the preparation method and application thereof.
Background technology
The limited of fossil energy uses and environmental degradation increasingly sharpens so that developing clean, reproducible novel energy
Become the task of top priority with energy storage device.Hydrogen as energy source is because energy density is high, pollution-free, sustainable use is considered as due to the advantages that
The ideal feasible substitute of fossil fuel.However Hydrogen Energy is not a kind of a large amount of energy resources for being present in nature, and
It is to need to be produced.In the method for current numerous hydrogen makings, electrolysis water preparation process is simple, and technology is more mature,
Cleanliness without any pollution is one of the hydrogen production process for being known and approving at present.Water electrolysis hydrogen production reaction is happened at electrode surface, including
Cathode hydrogen evolution reacts and Oxygen anodic evolution reacts two basic half-reactions.How electrode catalytic materials are improved for water electrolysis hydrogen production
Activity, reduce evolving hydrogen reaction overpotential, and improve electrode material stability be electro-catalysis area research emphasis and pass
Key.At present in electrocatalytic hydrogen evolution reaction, best liberation of hydrogen catalyst is the noble metals such as Pt series, but because its price is high
Expensive, material is rare, can not seriously limit the application of water electrolysis hydrogen production large-scale commercial in electro-catalysis field large-scale promotion
Process.Therefore, the high-efficient electrolytic water liberation of hydrogen catalyst and electrode material that exploitation is cheap, overpotential is low and stability is good are current
Research hotspot.
According to experimental study, find the principal element for influencing cathode hydrogen evolution catalyst performance have geometrical factor (electrode it is true
Real surface area) and capacity factor (electronic structure of material).Preferably hydrogen-precipitating electrode is：Overpotential of hydrogen evolution is low as possible, catalytic
It can stablize as possible and price is cheap as possible.Similar to other different-phase catalysts, evolving hydrogen reaction catalyst catalytic performance receptor 1 activity position
The influence of the density and reactivity of point, it is unstable etc. under low electric conductivity, low specific surface area, operating voltage in catalyst at present
Factor is the major reason for causing catalytic activity low.Transition metal element has stability high, and rich reserves are at low cost etc. excellent
Point promises to be good evolving hydrogen reaction catalyst.Not only there is higher electricity to evolving hydrogen reaction additionally, due to nickel-base material
Catalytic activity, and the advantages that corrosion resistance is strong, price is relatively low and be concerned.In the research in relation to nickel base electrode, Ren Menfa
Now influencing electrode performance, mainly there are two factors：(1) electrode metal ingredient and its composition ratio：When electrode metal ingredient reaches conjunction
Suitable ratio enables electrode to have adsorption strength appropriate at chemical bond with active H-shaped, and H can preferably be desorbed2, reduce analysis
Polarization resistance in hydrogen electrochemical reaction；(2) the real table area of electrode：When the real table area of electrode is much larger than apparent area
When, under same current density, real current density ratio apparent current density is small, usual its overpotential of smaller current density
It is smaller.In recent years it surrounds optimized alloy and forms and increase electrode surface area these two aspects, nickel base electrode type and structure obtain very big
Development.
Invention content
Based on the above the deficiencies in the prior art, the present invention provides one kind and having three metallic coppers-cobalt-molybdenum (Cu-Co-Mo)/bubble
Foam nickel porous electrode material and the preparation method and application thereof, the binding ability of three metal alloys and substrate nickel in the composite material
By force, performance is stablized under good corrosion resistance, alkaline condition；The preparation method realizes three metals and foam nickel base by solvent-thermal method
Combination, preparation process is simple, sintering temperature is low, low energy consumption in preparation process, be convenient for industrialized production.
As a preferred embodiment of the above technical solution, it is porous to have three Ni metal-Co-Mo/ nickel foams for one kind provided by the invention
Electrode material and the preparation method and application thereof further comprises some or all of following technical characteristic：
A kind of preparation method having three Ni metal-Co-Mo/ nickel foam porous electrode materials, includes the following steps：
1) it is defoamed nickel surface greasy dirt and oxide layer using organic solvent and acid soak, nickel foam is pre-processed；
2) mantoquita, cobalt salt, molybdenum salt, deionized water are configured to copper, cobalt, molybdenum salt compound precursor solution in proportion, it will
Copper, cobalt, molybdenum salt compound presoma and nickel foam are collectively disposed at confined reaction in autoclave, after reaction, wash drying, obtain
To the nickel foam for having hydrothermal synthesis product in surface growth；
3) by nickel foam obtained by step (2) in H2Atmosphere high temperature is calcined, and subsequent natural cooling is to get to having three metals
The porous electrolysis water catalyst of Cu-Co-Mo/ nickel foams.
As an improvement of the above technical solution, in the copper, cobalt, molybdenum salt compound precursor solution copper, cobalt, molybdenum mole
Than being 1:0.7~1.2:0.2~1.
As an improvement of the above technical solution, mantoquita, cobalt salt and molybdenum in the copper, cobalt, molybdenum salt compound precursor solution
A concentration of 0.01~0.05mol/L of salting liquid.
As an improvement of the above technical solution, the mantoquita is CuCl2, the cobalt salt is Co (NO3)2, the molybdenum salt is
Na2MoO4。
As an improvement of the above technical solution, hydrothermal temperature is 100 DEG C~200 DEG C, and the reaction time is 4~12h.
As an improvement of the above technical solution, the copper, cobalt, molybdenum salt compound presoma and nickel foam are high in tube furnace
It is 5%H that temperature, which restores used gas,2/ 95%Ar atmosphere is raised to 300~500 with the heating rate of 5~10 DEG C/min from room temperature
DEG C, 1~3h of insulation reaction, after reaction natural cooling obtain the porous electrolysis water catalyst of Cu-Co-Mo/ nickel foams.
As an improvement of the above technical solution, the nickel foam purity for being used as material substrate is 99.8% or more, surface density
300-450g/m2。
As an improvement of the above technical solution, the nickel foam preprocessing process includes：First in methanol, ethyl alcohol, tetrahydrochysene
In one or more solvents in furans, chloroform impregnate be ultrasonically treated 10~50min, then again with dilute hydrochloric acid impregnate ultrasound 10~
50 minutes, after treatment was cleaned 3~4 times using deionized water.
The technical solution of the application can also be accomplished by the following way, and it is porous to have three Ni metal-Co-Mo/ nickel foams
Electrode material uses above-mentioned preparation method.
The technical solution of the application can also be accomplished by the following way, described to have three Ni metal-Co-Mo/ nickel foams
Application of the porous electrode material in water electrolysis hydrogen production electrode is used as the electrode or catalyst of water electrolysis hydrogen production.
Compared with prior art, technical scheme of the present invention has the advantages that：
(1) present invention uses nickel foam for substrate, good corrosion resistance, while can be with Reinforced Cu-Co-Mo alloys and substrate
Binding ability；Cheap using elements such as copper, cobalt, molybdenums, performance is stablized under alkaline condition.
(2) preparation of water electrolysis hydrogen production electrode material (tri- metal porous electrolysis water catalyst of Cu-Co-Mo) of the present invention
Simple for process, sintering temperature is low, and low energy consumption in preparation process, is convenient for industrialized production.
(3) the tri- metal porous electrolysis water catalyst of Cu-Co-Mo prepared by the present invention has larger electro-chemical activity face
Product, greatly improves the catalytic activity of material.
(4) activearm becomes amorphous state knot in the tri- metal porous electrolysis water catalyst of Cu-Co-Mo prepared by the present invention
Structure has excellent performance and preferable stability, can be widely used as electrolyzed alkaline water hydrogen evolution electrode material, has wide answer
Use foreground.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will simply be situated between to the attached drawing of embodiment below
It continues.
Fig. 1 is to have three Ni metal-Co-Mo/ nickel foam porous electrode material surface shapes prepared by the embodiment of the present invention 1
Looks scanning electron microscope (SEM) photograph；
Fig. 2 is to have three Ni metal-Co-Mo/ nickel foam porous electrode material surface shapes prepared by the embodiment of the present invention 2
Looks scanning electron microscope (SEM) photograph；
Fig. 3 is to have three Ni metal-Co-Mo/ nickel foam porous electrode material surface shapes prepared by the embodiment of the present invention 3
Looks scanning electron microscope (SEM) photograph；
Fig. 4 is to have three Ni metal-Co-Mo/ nickel foam porous electrode materials prepared by the embodiment of the present invention 1~3
Linear sweep voltammetry curve graph.
Specific implementation mode
The following detailed description of the present invention specific implementation mode, as part of this specification, by embodiment come
Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
The preparation method of the present invention for having three Ni metal-Co-Mo/ nickel foam porous electrode materials specifically includes following
Step：
A, the pretreatment of conductive substrates
Choose the 1 × 1cm cut2Nickel foam impregnate one kind first in methanol, ethyl alcohol, tetrahydrofuran, chloroform
Or impregnated in multi-solvents and be ultrasonically treated 10~50min, it then uses hydrochloric acid solution instead and is ultrasonically treated 15min, carry out electrochemical deoiling
Dirty and oxide on surface；Finally nickel substrate is rinsed well with deionized water, wherein used concentration of hydrochloric acid is 1mol/L.
B, hydrothermal synthesis product is grown in nickel foam
Using hydro-thermal method by CuCl2、Co(NO3)2、Na2MoO4Three kinds of precursor species are dissolved in 50mL deionized waters, obtain
Copper, cobalt, molybdenum salt compound precursor solution, the wherein molar ratio of tri- kinds of elements of Cu, Co, Mo are 1:1:0.25, with above-mentioned pre- place
Nickel foam after reason is collectively disposed at confined reaction in autoclave, and 180 DEG C, reaction time 8h of reaction temperature waits for washing after reaction
Wash desciccate.
C, the high-temperature calcination of hydrothermal synthesis product restores
There is the nickel foam of hydrothermal synthesis product in 5%H the growth of above-mentioned surface2500 DEG C of calcining reductions in/95%Ar atmosphere
1-3h, subsequent natural cooling have three Ni metal-Co-Mo/ to get to tri- metal porous electrolysis water catalyst of Cu-Co-Mo
The porous electrolysis water catalyst of nickel foam.
Fig. 1 is the three porous electrolysis water catalyst of Ni metal-Co-Mo/ nickel foams being prepared under this material rate
Surface topography scanning electron microscope (SEM) photograph.
Embodiment 2
Step a is the same as embodiment 1
B, hydrothermal synthesis product is grown in nickel foam
Using hydro-thermal method by CuCl2、Co(NO3)2、Na2MoO4Three kinds of precursor species are dissolved in 50mL deionized waters, obtain
Copper, cobalt, molybdenum salt compound precursor solution, the wherein molar ratio of tri- kinds of elements of Cu, Co, Mo are 1:1:0.5, with above-mentioned pretreatment
Nickel foam afterwards is collectively disposed at confined reaction in autoclave, and 180 DEG C, reaction time 8h of reaction temperature waits for washing after reaction
Desciccate.
C, the high-temperature calcination of hydrothermal synthesis product restores
There is the nickel foam of hydrothermal synthesis product in 5%H the growth of above-mentioned surface2500 DEG C of calcining reductions in/95%Ar atmosphere
5h, subsequent natural cooling have three Ni metal-Co-Mo/ bubbles to get to tri- metal porous electrolysis water catalyst of Cu-Co-Mo
The porous electrolysis water catalyst of foam nickel.
Fig. 2 is the three porous electrolysis water catalyst of Ni metal-Co-Mo/ nickel foams being prepared under this material rate
Surface topography scanning electron microscope (SEM) photograph.
Embodiment 3
Step a is the same as embodiment 1
B, hydrothermal synthesis product is grown in nickel foam
Using hydro-thermal method by CuCl2、Co(NO3)2、Na2MoO4Three kinds of precursor species are dissolved in 50mL deionized waters, obtain
Copper, cobalt, molybdenum salt compound precursor solution, the wherein molar ratio of tri- kinds of elements of Cu, Co, Mo are 1:1:Behind 1, with above-mentioned pretreatment
Nickel foam be collectively disposed at confined reaction in autoclave, 180 DEG C, reaction time 8h of reaction temperature waits for washing after reaction dry
Dry product.
C, the high-temperature calcination of hydrothermal synthesis product restores
There is the nickel foam of hydrothermal synthesis product in 5%H the growth of above-mentioned surface2500 DEG C of calcining reductions in/95%Ar atmosphere
5h, subsequent natural cooling have three Ni metal-Co-Mo/ bubbles to get to tri- metal porous electrolysis water catalyst of Cu-Co-Mo
The porous electrolysis water catalyst of foam nickel.
Fig. 3 is the three porous electrolysis water catalyst of Ni metal-Co-Mo/ nickel foams being prepared under this material rate
Surface topography scanning electron microscope (SEM) photograph.
Interpretation of result：By the porous electrolysis water catalysis of three Ni metal-Co-Mo/ nickel foams can be obtained in Fig. 1-3 stereoscan photographs
The active constituent of agent uniform load in nickel foam, combines closely with foam nickel base, significantly reduces in electrolysis water process
In electric current resistance, improve the catalytic performance of material.
The preparation-obtained porous electrolysis water catalyst of three Ni metals-Co-Mo/ nickel foams in above-mentioned example 1-3 is applied to
Catalytic electrolysis water hydrogen manufacturing.
The three porous electrolysis water catalyst materials of Ni metal-Co-Mo/ nickel foams that pure foam nickel, three embodiments are prepared respectively
The linear sweep voltammetry curve of material is tested：
Using three-electrode system, using 1mol/L KOH as electrolyte, wherein carbon-point is used as to electrode, Ag/AgCl conducts
Reference electrode, the three porous electrolysis water catalyst of Ni metal-Co-Mo/ nickel foams that pure foam nickel, three embodiments are prepared respectively
Material is tested as working electrode successively respectively, wherein ensureing three Ni metal-Co-Mo/ of pure foam nickel, three kinds of rate of charges
The geometric area for having equivalent of the porous electrolysis water catalyst of nickel foam in the measurements, test results are shown in figure 4.
As shown in Figure 4, three kinds of startings for having the three porous electrolysis water catalyst materials of Ni metal-Co-Mo/ nickel foams are excessively electric
Position is about 0.223V, is much smaller than the starting overpotential value of pure foam nickel.When current density is 10mA/cm2When, have three metals
The performance of the porous electrolysis water catalyst material of Cu-Co-Mo/ nickel foams all has a distinct increment for pure foam nickel, compares
For present electrolysis water catalysis material, material specific surface area can effectively be promoted as conductive substrates using nickel foam,
So that electrolysis water material is had 3D porous foam skeletons, greatly increase the electrochemical surface area of material, to significantly drop
The overpotential of hydrogen evolution of low material reduces energy consumption of material during electrolysis water.It can be obtained by above-mentioned comparison, system of the present invention
The three standby porous electrolysis water catalyst material catalytic performances of Ni metal-Co-Mo/ nickel foams are excellent, are expected to become water electrolysis hydrogen production
The alternative materials of noble metal catalyst in field.
The above is the preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of three Ni metals-Co-Mo/ nickel foam porous electrode materials, which is characterized in that including following step
Suddenly：
1) it is defoamed nickel surface greasy dirt and oxide layer using organic solvent and acid soak, nickel foam is pre-processed；
2) mantoquita, cobalt salt, molybdenum salt, deionized water are configured to copper, cobalt, molybdenum salt compound precursor solution in proportion, by copper,
Cobalt, molybdenum salt compound presoma and nickel foam are collectively disposed at confined reaction in autoclave, after reaction, wash drying, obtain
On surface, growth has the nickel foam of hydrothermal synthesis product；
3) by nickel foam obtained by step (2) in H2/ Ar atmosphere high temperatures are calcined, and subsequent natural cooling is to get to having three metals
The porous electrolysis water catalyst of Cu-Co-Mo/ nickel foams.
2. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is, copper in the copper, cobalt, molybdenum salt compound precursor solution, cobalt, molybdenum molar ratio be 1:0.7~1.2:0.2~1.
3. the preparation method according to claim 1 or 2 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials,
It is characterized in that, mantoquita in the copper, cobalt, molybdenum salt compound precursor solution, cobalt salt and molybdenum salting liquid a concentration of 0.01~
0.05mol/L。
4. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is that the mantoquita is CuCl2, the cobalt salt is Co (NO3)2, the molybdenum salt is Na2MoO4。
5. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is that hydrothermal temperature is 100 DEG C~200 DEG C, and the reaction time is 4~12h.
6. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is that the copper, cobalt, molybdenum salt compound presoma and the used gas of nickel foam high temperature reduction in tube furnace are 5%H2/
95%Ar gaseous mixtures are raised to 300~500 DEG C, 1~3h of insulation reaction, reaction knot with the heating rate of 5~10 DEG C/min from room temperature
Natural cooling obtains the porous electrolysis water catalyst of Cu-Co-Mo/ nickel foams after beam.
7. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is that the nickel foam purity for being used as material substrate is 99.8% or more, surface density 300-450g/m2。
8. the preparation method according to claim 1 for having three Ni metal-Co-Mo/ nickel foam porous electrode materials, special
Sign is that the nickel foam preprocessing process includes：It is one or more molten first in methanol, ethyl alcohol, tetrahydrofuran, chloroform
In agent impregnate be ultrasonically treated 10~50min, then again with dilute hydrochloric acid impregnate ultrasound 10~50 minutes, after treatment use go from
Sub- water cleans 3~4 times.
9. what a kind of preparation method according to any one of claim 1-8 obtained has three Ni metal-Co-Mo/ bubbles
Foam nickel porous electrode material, which is characterized in that have three Ni metal-Co-Mo/ nickel foam porous electrode materials and use above-mentioned preparation
Method.
10. what a kind of preparation method according to any one of claim 1-8 obtained has three Ni metal-Co-Mo/ bubbles
The application of foam nickel porous electrode material, which is characterized in that described have three Ni metal-Co-Mo/ nickel foam porous electrode materials and exist
Application in water electrolysis hydrogen production electrode.
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