CN109967080A - A kind of preparation method and application for amorphous (Ni, Fe) the OOH film elctro-catalyst being supported on foam nickel surface - Google Patents
A kind of preparation method and application for amorphous (Ni, Fe) the OOH film elctro-catalyst being supported on foam nickel surface Download PDFInfo
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- CN109967080A CN109967080A CN201910242914.1A CN201910242914A CN109967080A CN 109967080 A CN109967080 A CN 109967080A CN 201910242914 A CN201910242914 A CN 201910242914A CN 109967080 A CN109967080 A CN 109967080A
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- ooh
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 194
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 122
- 239000006260 foam Substances 0.000 title claims abstract description 69
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000010358 mechanical oscillation Effects 0.000 claims abstract description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 39
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000005868 electrolysis reaction Methods 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 229910002588 FeOOH Inorganic materials 0.000 claims description 3
- 229910002640 NiOOH Inorganic materials 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 42
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 33
- 239000012153 distilled water Substances 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 238000002604 ultrasonography Methods 0.000 description 8
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 4
- 239000010405 anode material Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 4
- 229910000863 Ferronickel Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005713 exacerbation Effects 0.000 description 1
- 239000000446 fuel 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
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
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- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of amorphous (Ni, Fe) OOH film elctro-catalyst for being supported on foam nickel surface, comprising the following steps: (1) is cleaned by ultrasonic nickel foam；(2) nickel foam after ultrasonic cleaning is immersed in iron nitrate solution, mechanical oscillation, generates amorphous (Ni, Fe) OOH film and is supported on foam nickel surface.Preparation method provided by the invention is simple, easily operated, and amorphous (Ni, Fe) the OOH film elctro-catalyst for being supported on foam nickel surface of preparation has high catalytic activity and better stability to electrolyzed alkaline water anode reaction at higher current densities.
Description
Technical field
The invention belongs to nano material technology and electrochemical energy transformation technology field, in particular to one kind is supported on foam
The preparation method and application of amorphous (Ni, Fe) the OOH film elctro-catalyst of nickel surface.
Background technique
With the increasingly exacerbation of energy crisis and problem of environmental pollution.A kind of renewable energy of the Hydrogen Energy as green, phase
Than in other traditional fuels, such as coal, having the characteristics that cleaning, efficient.Electrolysis water is a kind of up-and-coming renewable
Energy storage method can convert on a large scale water to the cleaning hydrogen and oxygen of high-energy density.The two of electrocatalytic decomposition water
It was found that anodic process all refers to the transfer of four electronics under acid-base condition in a half-reaction, kinetics inertia is needed
Wanting higher overpotential is the reaction bottleneck that electrolysis water prepares hydrogen.Therefore, many researchers are dedicated to efficient electro-catalysis
Decompose the developmental research of aquatic products oxygen reaction (OER) catalysis material.
Previous in research, most of OER elctro-catalysts are all based on noble metal (Ru and Ir) compound, because it
Have very high stability and good catalytic activity.However, reserves are rare on earth for these precious metal chemical complexs, limitation
Their large-scale application.Therefore it explores the OER elctro-catalyst of one kind efficiently, stable, inexpensive to be of great significance, such as three
Tie up transition metal (Fe, Co, Ni etc.), metal oxide, metal hydroxides (oxyhydroxide), metal chalcogenides, gold
Belong to phosphorus family compound etc..
Many studies have shown that: the hydroxide of pure nickel and iron has poor electrocatalysis characteristic, and ferronickel base hydroxide
Object then shows efficient OER catalytic performance.The preparation method of ferronickel base oxide has electrodeposition process, hydro-thermal to close in the prior art
At method and the method for other complexity.But these preparation methods are usually directed to the either harsh reaction condition of complicated presoma.
Such as: high temperature, additional voltage input and some other complicated reaction condition.
Therefore, a kind of simple and easy to do preparation of developmental research has high electrochemical activity and the oxidation of the ferronickel base hydroxyl of stability
The method of object elctro-catalyst is extremely important.
Summary of the invention
The purpose of the present invention is intended to provide a kind of amorphous (Ni, Fe) OOH film electro-catalysis for being supported on foam nickel surface
The preparation method of agent, preparation method provided by the invention is simple, easily operated, and preparation is supported on the amorphous of foam nickel surface
(Ni, Fe) OOH film elctro-catalyst at higher current densities to electrolyzed alkaline water anode reaction have high catalytic activity and preferably
Stability.
The technical scheme adopted by the invention is that:
A kind of preparation method for amorphous (Ni, Fe) the OOH film elctro-catalyst being supported on foam nickel surface, including it is following
Step:
(1) nickel foam is cleaned by ultrasonic；
(2) nickel foam after ultrasonic cleaning is immersed in iron nitrate solution, mechanical oscillation, is generated amorphous (Ni, Fe)
OOH film is simultaneously supported on foam nickel surface.
(2) nickel foam after ultrasonic cleaning is immersed in iron nitrate solution, mechanical oscillation, is generated amorphous (Ni, Fe)
OOH obtains amorphous (Ni, Fe) the OOH film elctro-catalyst for being supported on foam nickel surface.
In step (1), successively it is cleaned by ultrasonic foam with hydrochloric acid solution, acetone soln, ethanol solution and distilled water
Nickel, the impurity for the nickel surface that defoams.
In step (2), the concentration of the ferric nitrate is 0.05~0.8mol/L, and duration of oscillation is 0.5~5 min.
Preferably, in step (2), the concentration of the ferric nitrate is 0.2~0.3mol/L, and duration of oscillation is 3~4min.
The concentration and duration of oscillation of ferric nitrate influence the generation of amorphous (Ni, Fe) OOH and the content of NiOOH and FeOOH, in above-mentioned model
Enclose it is interior can comparatively fast generate amorphous (Ni, Fe) OOH, and there is efficient electro catalytic activity and good stability.
It is further preferred that the concentration of the ferric nitrate is 0.2mol/L, duration of oscillation 3min in step (2).System
The electro catalytic activity and stability of standby obtained amorphous (Ni, Fe) the OOH film elctro-catalyst for being supported on foam nickel surface are most
It is good.
Preferably, in step (2), amorphous (Ni, Fe) the OOH film electro-catalysis for being supported on foam nickel surface
The content of NiOOH is greater than the content of FeOOH in agent, and the content is mole.
The preparation principle of amorphous (Ni, Fe) the OOH film elctro-catalyst provided by the invention for being supported on foam nickel surface
Are as follows: nickel foam is etched under the conditions of mechanical oscillation by ferric nitrate, after reacting with iron nitrate solution, generates at room temperature amorphous
(Ni, Fe) OOH material.Relative to other methods for preparing effective OER catalyst, method provided by the present invention is very simple
Effectively and not it is related to the presoma or toxic chemical of any complexity.
The present invention generates amorphous (Ni, Fe) OOH film using mechanical oscillation method and is supported on foam nickel surface, in high electricity
OER property retention is stable under current density, with good stability, amorphous (Ni, Fe) OOH film conduct under alkaline condition
Elctro-catalyst has efficient catalytic activity.
The present invention also provides a kind of amorphous (Ni, Fe) OOH film elctro-catalysts for being supported on foam nickel surface to be electrolysed
Application in water oxygen evolution reaction.
Amorphous (Ni, Fe) the OOH film elctro-catalyst prepared by the present invention for being supported on foam nickel surface is used for electro-catalysis
Oxygen is produced, three-electrode system is used, working electrode is foamed nickel supported (Ni, Fe) OOH material, is platinized platinum electricity to electrode
Pole, reference electrode are saturation silver/silver chloride electrode, and electrolyte is 1.0M- potassium hydroxide solution.The table in electrolysis water oxygen evolution reaction
Reveal excellent electrocatalysis characteristic
Compared with prior art, the present invention has following breakthrough sexual clorminance:
(1) amorphous (Ni, Fe) the OOH film elctro-catalyst provided by the invention for being supported on foam nickel surface, in alkalinity
Good stability is shown in electrolyte, using it as anode material, electrolysis water, anode are close in electric current under alkaline condition
Degree is 500mA cm-2When, overpotential is only 280mV, has both efficient electro catalytic activity and good stability, close in high current
Lower OER property retention is spent to stablize；
(2) the film elctro-catalyst provided by the invention for being supported on foam nickel surface, amorphous (Ni, Fe) OOH electro-catalysis
Strong combination between agent and nickel foam, it is ensured that good conductive characteristic and effective electricity between elctro-catalyst and nickel foam
Lotus transfer.
(3) present invention is supported on amorphous (Ni, Fe) the OOH film elctro-catalyst of foam nickel surface, and preparation method is one
Step synthesis.Synthetic method mild condition, reaction time are short and easily operated, are supported on amorphous (Ni, the Fe) of foam nickel surface
OOH film shows excellent catalytic performance and stability to electrolysis water OER reaction, easy to industrialized production.
Detailed description of the invention
Fig. 1 is the SEM of amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface prepared by the embodiment of the present invention 1
Figure；
Fig. 2 is the XPS of amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface prepared by the embodiment of the present invention 1
Figure；
Fig. 3 is amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface of the preparation of the embodiment of the present invention 1 in 1.0M
The polarization curve of electrolysis water OER in KOH solution；
Fig. 4 is amorphous (Ni, Fe) the OOH film electro-catalysis for being supported on foam nickel surface prepared by the embodiment of the present invention 1
Agent, in 1.0M KOH solution under the constant current of electrolysis water precipitated oxygen, voltage changes over time curve graph.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, with reference to the accompanying drawings and embodiments to this
Invention is described in further detail.It should be appreciated that the specific embodiments described herein are only used to explain the present invention,
And the scope of protection of the present invention is not limited.
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Embodiment 1
1. the preparation of iron nitrate solution
(1) 3.096g Fe(NO3)39H2O is weighed, is dissolved in 8mL distilled water, is stirred under room temperature to being completely dissolved, preparation
Iron nitrate solution is 1.6mol/L.
(2) 1.6mol/L iron nitrate solution 1mL is pipetted using 1000 μ L liquid-transfering guns, then pipettes the dilution of 7 mL distilled water, obtained
To 0.2mol/L iron nitrate solution.
2. the preparation of nickel foam
(1) nickel foam is successively impregnated in 0.1mol/L hydrochloric acid solution, acetone soln, ethanol solution to ultrasound
10min is finally washed three times with distilled water ultrasound.
3. the preparation of 1.0M KOH solution
(1) about 50mL ultrapure water is measured, 5.61g potassium hydroxide is dissolved with ultrapure water and stirred, in 100mL capacity after cooling
Constant volume in bottle.
4. being supported on the preparation of amorphous (Ni, Fe) the OOH film of foam nickel surface
(1) pretreated nickel foam is immersed in the iron nitrate solution of 0.2mol/L, mechanical oscillation 3min；
(2) after the completion of vibrating, naturally dry at room temperature；
(3) it by step (2) obtained product distilled water repeated flushing, dries at room temperature, obtains being supported on nickel foam
Amorphous (Ni, Fe) the OOH film on surface.
The SEM figure and XPS figure point of amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface prepared by embodiment 1
Not not as depicted in figs. 1 and 2.
Embodiment 2
1. the preparation of iron nitrate solution
(1) 3.096g Fe(NO3)39H2O is weighed, is dissolved in 8mL distilled water, is stirred under room temperature to being completely dissolved, preparation
Iron nitrate solution is 1.6mol/L.
(2) 1.6mol/L iron nitrate solution 1mL is pipetted using 1000 μ L liquid-transfering guns, then pipettes the dilution of 15mL distilled water, obtained
To 0.1mol/L iron nitrate solution.
2. the preparation of nickel foam
(1) nickel foam is successively impregnated in 0.1mol/L hydrochloric acid solution, acetone soln, ethanol solution to ultrasound
10min is finally washed three times with distilled water ultrasound.
3. the preparation of 1.0M KOH solution
(1) about 50mL ultrapure water is measured, 5.61g potassium hydroxide is dissolved with ultrapure water and stirred, in 100mL capacity after cooling
Constant volume in bottle.
4. being supported on the preparation of amorphous (Ni, Fe) the OOH film of foam nickel surface
(1) pretreated nickel foam is immersed in the iron nitrate solution of 0.1mol/L, mechanical oscillation 2min；
(2) after the completion of vibrating, naturally dry at room temperature；
(3) it by step (2) obtained product distilled water repeated flushing, dries at room temperature, obtains being supported on nickel foam
The elctro-catalyst on surface.
Embodiment 3
1. the preparation of iron nitrate solution
(1) 3.096g Fe(NO3)39H2O is weighed, is dissolved in 8mL distilled water, is stirred under room temperature to being completely dissolved, preparation
Iron nitrate solution is 1.6mol/L.
(2) 1.6mol/L iron nitrate solution 1mL is pipetted using 1000 μ L liquid-transfering guns, then pipettes the dilution of 3 mL distilled water, obtained
To 0.4mol/L iron nitrate solution.
2. the preparation of nickel foam
(1) nickel foam is successively impregnated in 0.1mol/L hydrochloric acid solution, acetone soln, ethanol solution to ultrasound
10min is finally washed three times with distilled water ultrasound.
3. the preparation of 1.0M KOH solution
(1) about 50mL ultrapure water is measured, 5.61g potassium hydroxide is dissolved with ultrapure water and stirred, in 100mL capacity after cooling
Constant volume in bottle.
4. being supported on the preparation of amorphous (Ni, Fe) the OOH film of foam nickel surface
(1) pretreated nickel foam is immersed in the iron nitrate solution of 0.4mol/L, mechanical oscillation 3min；
(2) after the completion of vibrating, naturally dry at room temperature；
(3) it by step (2) obtained product distilled water repeated flushing, dries at room temperature, obtains being supported on nickel foam
The elctro-catalyst on surface.
Embodiment 4
1. the preparation of iron nitrate solution
(1) 3.096g Fe(NO3)39H2O is weighed, is dissolved in 8mL distilled water, is stirred under room temperature to being completely dissolved, preparation
Iron nitrate solution is 1.6mol/L.
(2) 1.6mol/L iron nitrate solution 1mL is pipetted using 1000 μ L liquid-transfering guns, then pipettes the dilution of 31mL distilled water, obtained
To 0.05mol/L iron nitrate solution.
2. the preparation of nickel foam
(1) nickel foam is successively impregnated in 0.1mol/L hydrochloric acid solution, acetone soln, ethanol solution to ultrasound
10min is finally washed three times with distilled water ultrasound.
3. the preparation of 1.0M KOH solution
(1) about 50mL ultrapure water is measured, 5.61g potassium hydroxide is dissolved with ultrapure water and stirred, in 100mL capacity after cooling
Constant volume in bottle.
4. being supported on the preparation of amorphous (Ni, Fe) the OOH film of foam nickel surface
(1) pretreated nickel foam is immersed in the iron nitrate solution of 0.2mol/L, mechanical oscillation 1min；
(2) after the completion of vibrating, naturally dry at room temperature；
(3) by step (2) obtained product distilled water repeated flushing, naturally dry, obtains being supported on bubble at room temperature
The elctro-catalyst of foam nickel surface.
Application examples 1
1. the activation processing of elctro-catalyst
(1) three-electrode system is used, working electrode is amorphous (Ni, Fe) the OOH thin-film electro for being supported on nickel foam surface
Catalyst is platinum plate electrode to electrode, and reference electrode is saturation silver/silver chloride electrode, and electrolyte is 1.0M KOH；
(2) cyclic voltammetry (CV) activates: Shanghai Chen Hua CHI 660E electrochemical workstation is used, using cyclic voltammetry
Program, in 0-0.8V vs.RHE, sweeping speed is 50mV/s in test section, and circulation 20 is enclosed, and electrode reaches stable state.
2. linear sweep voltammetry (LSV) is tested
After activation, changeover program is linear sweep voltammetry, and test section is 0-1.2V vs.RHE, and sweeping speed is 5mV/s.
In alkaline electrolyte, elctro-catalyst is in 500mA cm-2When, potential 280mV is shown in Fig. 3.
3. stability test
After activation, changeover program is more electric currents jump rank method program, and electric current is set as 0.06A, and the time is set as 40000s.Such as
Shown in Fig. 4, the voltage change of elctro-catalyst is little, it was demonstrated that its good stability.
Application examples 2
As shown in application examples 1, with amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface of the preparation of embodiment 2
As anode material, electrolysis water, anode are 500mA cm in current density under alkaline condition-2When, overpotential 300mV.
Application examples 3
As shown in application examples 1, with amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface of the preparation of embodiment 3
As anode material, electrolysis water, anode are 500mA cm in current density under alkaline condition-2When, overpotential 320mV.
Application examples 4
As shown in application examples 1, with amorphous (Ni, Fe) the OOH film for being supported on foam nickel surface of the preparation of embodiment 4
As anode material, electrolysis water, anode are 500mA cm in current density under alkaline condition-2When, overpotential 320mV.
Technical solution of the present invention and beneficial effect is described in detail in above-described specific embodiment, Ying Li
Solution is not intended to restrict the invention the foregoing is merely presently most preferred embodiment of the invention, all in principle model of the invention
Interior done any modification, supplementary, and equivalent replacement etc. are enclosed, should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method for amorphous (Ni, Fe) the OOH film elctro-catalyst for being supported on foam nickel surface, feature exist
In, comprising the following steps:
(1) nickel foam is cleaned by ultrasonic；
(2) nickel foam after ultrasonic cleaning is immersed in iron nitrate solution, mechanical oscillation, it is thin generates amorphous (Ni, Fe) OOH
Film is simultaneously supported on foam nickel surface.
2. the preparation of amorphous (Ni, Fe) the OOH film elctro-catalyst according to claim 1 for being supported on foam nickel surface
Method, which is characterized in that in step (2), the concentration of the ferric nitrate is 0.05~0.8mol/L, duration of oscillation is 0.5~
5min。
3. the preparation of amorphous (Ni, Fe) the OOH film elctro-catalyst according to claim 2 for being supported on foam nickel surface
Method, which is characterized in that in step (2), the concentration of the ferric nitrate is 0.1~0.2mol/L, duration of oscillation is 2~
3min。
4. the preparation of amorphous (Ni, Fe) the OOH film elctro-catalyst according to claim 1 for being supported on foam nickel surface
Method, which is characterized in that in step (2), amorphous (Ni, Fe) the OOH film electro-catalysis for being supported on foam nickel surface
The content of NiOOH is greater than the content of FeOOH in agent.
5. amorphous (Ni, Fe) the OOH film elctro-catalyst according to claim 1 to 4 for being supported on foam nickel surface
Application in electrolysis water oxygen evolution reaction.
6. amorphous (Ni, Fe) the OOH film elctro-catalyst according to claim 5 for being supported on foam nickel surface is answered
With, which is characterized in that three-electrode system is used in electrolysis water oxygen evolution reaction, working electrode is that amorphous (Ni, Fe) OOH is thin
Film, is platinum plate electrode to electrode, and reference electrode is saturation silver/silver chloride electrode.
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