CN110152673A - Iron nickel layered double hydroxide/nickel foam composite material and preparation method and application - Google Patents
Iron nickel layered double hydroxide/nickel foam composite material and preparation method and application Download PDFInfo
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- CN110152673A CN110152673A CN201910389773.6A CN201910389773A CN110152673A CN 110152673 A CN110152673 A CN 110152673A CN 201910389773 A CN201910389773 A CN 201910389773A CN 110152673 A CN110152673 A CN 110152673A
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- nickel
- iron
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 64
- 239000006260 foam Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 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 8
- 230000035484 reaction time Effects 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 4
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 4
- YPJCVYYCWSFGRM-UHFFFAOYSA-H iron(3+);tricarbonate Chemical compound [Fe+3].[Fe+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O YPJCVYYCWSFGRM-UHFFFAOYSA-H 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000004277 Ferrous carbonate Substances 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 3
- 229960004652 ferrous carbonate Drugs 0.000 claims description 3
- 235000019268 ferrous carbonate Nutrition 0.000 claims description 3
- 230000036571 hydration Effects 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- 229910000015 iron(II) carbonate Inorganic materials 0.000 claims description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- DEOPWJHDYPLPRX-UHFFFAOYSA-M iron chloride hydrate Chemical compound O.[Cl-].[Fe] DEOPWJHDYPLPRX-UHFFFAOYSA-M 0.000 claims description 2
- HIIGGQNLPWIVAG-UHFFFAOYSA-L nickel(2+);diacetate;hydrate Chemical compound O.[Ni+2].CC([O-])=O.CC([O-])=O HIIGGQNLPWIVAG-UHFFFAOYSA-L 0.000 claims description 2
- DWAHIRJDCNGEDV-UHFFFAOYSA-N nickel(2+);dinitrate;hydrate Chemical compound O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DWAHIRJDCNGEDV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- HGGYAQHDNDUIIQ-UHFFFAOYSA-L dichloronickel;hydrate Chemical compound O.Cl[Ni]Cl HGGYAQHDNDUIIQ-UHFFFAOYSA-L 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 11
- 230000003197 catalytic effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910021607 Silver chloride Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- 238000004502 linear sweep voltammetry Methods 0.000 description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 239000002023 wood Substances 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of iron nickel layered double hydroxide/nickel foam composite material and preparation method and applications, the preparation method includes: 1) in the presence of the solvent, source of iron, ammonium fluoride, urea and nickel foam to be carried out solvent thermal reaction so that reaction product A is made；2) nickel source, ammonium fluoride, urea, reaction product A in the presence of the solvent, are subjected to solvent thermal reaction so that iron nickel layered double hydroxide/foam nickel composite material is made.The iron nickel layered double hydroxide/foam nickel composite material has the characteristic of low overpotential and high stability, and then it can be applied in oxygen evolution reaction and evolving hydrogen reaction, while the preparation method raw material is simple and convenient to operate.
Description
Technical field
The present invention relates to composite materials, and in particular, to a kind of iron nickel layered double hydroxide/nickel foam composite wood
Material and its preparation method and application.
Background technique
Since the pollution of the current world is increasingly severe, people increasingly thirst for the demand of clean energy resource, are sent out at present
Now or what may be utilized by people includes solar energy, wind energy, nuclear energy, Hydrogen Energy.Wherein solar energy and wind energy are by region and time
It is affected, nuclear energy is due to possible potential safety rather than is widely received.And Hydrogen Energy is able to use convenient, unit matter
The heat of amount is high, completely pollution-free for environment, is the research emphasis of new energy research field.
Hydrogen producing technology is divided into water electrolysis hydrogen production and photolysis water hydrogen at present, but develops more mature technological means at present
Wider with application is water electrolysis hydrogen production.The voltage under alkaline condition of industrial water electrolysis hydrogen production used is much higher than at present
Water decomposition is the theoretical voltage of oxygen and hydrogen, has a large amount of electric energy to be used to overcome the overpotential of electrode surface, and electrolysis water
It is divided into Anodic oxygen evolution reaction and cathode hydrogen evolution reaction, therefore developing colleges and universities, stable analysis oxygen and Electrocatalytic Activity for Hydrogen Evolution Reaction agent is electrolysis water
Industry urgent problem to be solved.
Traditional analysis oxygen and liberation of hydrogen catalyst is noble metal and part metal oxide containing precious metals (IrO2And RuO2), catalytic performance
It is excellent, but it is at high price, and scarcity of resources makes it be difficult to widespread adoption.
Summary of the invention
The object of the present invention is to provide a kind of iron nickel layered double hydroxide/foam nickel composite material and its preparation sides
Method and application, the iron nickel layered double hydroxide/foam nickel composite material have the characteristic of low overpotential and high stability,
And then it can be applied in oxygen evolution reaction and evolving hydrogen reaction, while the preparation method raw material is simple and convenient to operate.
To achieve the goals above, the present invention provides a kind of iron nickel layered double hydroxide/nickel foam composite woods
The preparation method of material, comprising:
1) source of iron, ammonium fluoride, urea in the presence of the solvent, are subjected to solvent thermal reaction with nickel foam and react production to be made
Object A；
2) nickel source, ammonium fluoride, urea, reaction product A in the presence of the solvent, are subjected to solvent thermal reaction so that iron nickel is made
Layered double hydroxide/foam nickel composite material.
The present invention also provides a kind of iron nickel layered double hydroxide/foam nickel composite material, the iron nickel layer shape is double
Metal hydroxides/foam nickel composite material is prepared by above-mentioned preparation method.
Invention further provides a kind of as above-mentioned iron nickel layered double hydroxide/foam nickel composite material exists
Application in evolving hydrogen reaction and oxygen evolution reaction.
In the above-mentioned technical solutions, iron nickel layered double hydroxide/bubble is made by two step solvent-thermal methods in the present invention
Foam nickel composite material, the lamellar structure with molecule being attached in nickel foam, crystallinity is high, is conducive in high current feelings
Maintain the stability of electrode material self structure that it is made not collapse under condition；The composite material has low overpotential and high stability
Characteristic, while it being demonstrated by good analysis oxygen and Hydrogen Evolution Performance under alkaline condition, in 10mAcm-2Current density under, oxygen analysis
Overpotential out is 197mV, and the overpotential that hydrogen is precipitated is 129mV, and then it can be considered as instead of noble metal and its oxide work
For the good material for analysing oxygen and Electrocatalytic Activity for Hydrogen Evolution Reaction agent.The preparation method is simple with step simultaneously, energy consumption is lower, post-processing letter
List, raw material sources are extensive, cheap, and then can further be convenient for being widely popularized for the preparation method.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the SEM figure for detecting B1 in example 1；
Fig. 2 is the TEM figure for detecting B1 in example 2；
Fig. 3 is the XRD diagram for detecting B1 in example 3；
Fig. 4 is the LSV figure for the linear volt-ampere curve that the oxygen of B1 in application examples 1 is precipitated；
Fig. 5 is the LSV figure for the linear volt-ampere curve that the hydrogen of B1 in application examples 1 is precipitated.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of preparation methods of iron nickel layered double hydroxide/foam nickel composite material, comprising:
1) source of iron, ammonium fluoride, urea in the presence of the solvent, are subjected to solvent thermal reaction with nickel foam and react production to be made
Object A；
2) nickel source, ammonium fluoride, urea, reaction product A in the presence of the solvent, are subjected to solvent thermal reaction so that iron nickel is made
Layered double hydroxide/foam nickel composite material.
In the step 1) of above-mentioned preparation method, the dosage of each material can select in a wide range, but in order into
One step improves overpotential, stability and the catalytic performance of iron nickel layered double hydroxide/foam nickel composite material obtained,
Preferably, in step 1), source of iron, ammonium fluoride, urea and nickel foam amount ratio be 0.75mmol:1-8mmol:2-18mmo:
1cm × 1cm-2.5cm × 4cm, the nickel foam with a thickness of 1.5mm.
In the step 1) of above-mentioned preparation method, the dosage of solvent can select in a wide range, but in order into one
Step improves overpotential, stability and the catalytic performance of iron nickel layered double hydroxide/foam nickel composite material obtained, excellent
Selection of land, in step 1), source of iron, solvent amount ratio be 0.75mmol:10-40mL.
In the step 1) and step 2) of above-mentioned preparation method, the reaction condition of solvent thermal reaction can be in a wide range
Selection, but in order to further improve the overpotential of iron nickel layered double hydroxide/foam nickel composite material obtained, steady
Qualitative and catalytic performance, it is preferable that in step 1) and step 2), solvent thermal reaction at least meets the following conditions: in closed
Under the conditions of carry out, reaction temperature be 100-200 DEG C, reaction time 2-72h；It is highly preferred that reaction temperature is 120-180 DEG C,
Reaction time is 6-15h；.
In the step 2) of above-mentioned preparation method, the dosage of each material can select in a wide range, but in order into
One step improves overpotential, stability and the catalytic performance of iron nickel layered double hydroxide/foam nickel composite material obtained,
Preferably, relative to 1cm × 1cm-2.5cm × 4cm nickel foam, in step 2), the dosage of nickel source is 0.015-
1.5mmol, the dosage of ammonium fluoride are 0.1-0.8mmol, and the dosage of urea is 0.2-1.8mmol；
In the step 2) of above-mentioned preparation method, the dosage of solvent can select in a wide range, but in order into one
Step improves overpotential, stability and the catalytic performance of iron nickel layered double hydroxide/foam nickel composite material obtained, excellent
Selection of land, relative to 1cm × 1cm-2.5cm × 4cm nickel foam, in step 2), the dosage of solvent is 10-40mL.
In the present invention, the specific type of source of iron, nickel source and solvent can select in a wide range, but from cost
Consider, it is preferable that source of iron is selected from ferric nitrate, ferric nitrate hydrate, iron chloride, iron chloride hydrate, ferric acetate, ferric acetate hydration
Object, ferric carbonate, ferric carbonate hydrate, frerrous chloride, frerrous chloride hydrate, ferrous acetate, ferrous acetate hydrate, carbonic acid are sub-
One of iron, ferrous carbonate hydrate are a variety of；Nickel source is selected from nickel nitrate, nickel nitrate hydrate, nickel chloride, nickel chloride hydration
One of object, nickel acetate, nickel acetate hydrate are a variety of；Solvent is water.
In the step 2) of above-mentioned preparation method, nickel foam can select in a wide range, but in order to further change
Overpotential, stability and the catalytic performance of kind iron nickel layered double hydroxide/foam nickel composite material obtained, preferably
Ground, the specification of the single side of nickel foam are 1cm × 1cm to 2.5cm × 4cm；It is highly preferred that nickel foam passes through acetone, hydrochloric acid and go
Ion is pre-processed to remove oxide on surface.
In the above-described embodiment, multiple in order to further improve iron nickel layered double hydroxide/nickel foam obtained
Overpotential, stability and the catalytic performance of condensation material, it is preferable that after solvent thermal reaction in step 1) and 2), the preparation side
Method is equal further include: reaction system is cooled to 15-35 DEG C in a manner of natural cooling.
The present invention also provides a kind of iron nickel layered double hydroxide/foam nickel composite material, the iron nickel layer shape is double
Metal hydroxides/foam nickel composite material is prepared by above-mentioned preparation method.
Invention further provides a kind of as above-mentioned iron nickel layered double hydroxide/foam nickel composite material exists
Application in evolving hydrogen reaction and oxygen evolution reaction.
The present invention will be described in detail by way of examples below.In following embodiment, the specification of the single side of nickel foam
Are as follows: surface density 380g/m2, the hole count of per inch is 110, with a thickness of 1.5mm.
Embodiment 1
1) by 0.3030g Fe(NO3)39H2O (0.75mmol), 0.1666g ammonium fluoride (4.49mmol), 0.54g urea
(9mmol), 30mL deionized water are uniformly mixed in beaker and obtain uniform solution,
2) above-mentioned uniform solution is transferred in the stainless steel cauldron of polytetrafluoroethylene (PTFE) set and nickel foam (2cm is added
× 3cm), be placed directly in 120 DEG C of baking oven, and react 12h at 120 DEG C, to the reaction time after, naturally cool to
25 DEG C to get arrive reaction product A1.
3) 0.0218g Nickelous nitrate hexahydrate (0.075mmol), 0.01666g ammonium fluoride (0.449mmol), 0.054g are urinated
Plain (0.9mmol), 30mL deionized water are uniformly mixed in beaker and obtain uniform solution,
4) above-mentioned uniform solution is transferred in the stainless steel cauldron of polytetrafluoroethylene (PTFE) set and by above-mentioned reaction product
A1 be added, be placed directly in 120 DEG C of baking oven, and react 12h at 120 DEG C, to the reaction time after, naturally cool to
25 DEG C to get arrive iron nickel layered double hydroxide/foam nickel composite material B1.
Embodiment 2
The procedure of Example 1 was followed except that step 1) and 2) in, ammonium fluoride 1mmol, urea 2mmol,
Nickel foam 1cm × 1cm.
Embodiment 3
The procedure of Example 1 was followed except that step 1) and 2) in, ammonium fluoride 8mmol, urea 18mmol,
Nickel foam 2.5cm × 4cm.
Embodiment 4
The procedure of Example 1 was followed except that step 3) and 4) in, Nickelous nitrate hexahydrate 0.015mmol,
Ammonium fluoride 0.1mmol, urea 0.2mmol.
Embodiment 5
The procedure of Example 1 was followed except that step 3) and 4) in, Nickelous nitrate hexahydrate 1.5mmol, fluorine
Change ammonium 0.8mmol, urea 1.8mmol.
Embodiment 6
The procedure of Example 1 was followed except that step 2) and 4) in baking oven temperature be 180 DEG C, reaction
Time is 6h.
Embodiment 7
The procedure of Example 1 was followed except that Fe(NO3)39H2O lithium is changed to iron chloride, nickel nitrate changes
At nickel chloride.
Embodiment 8
The procedure of Example 1 was followed except that Fe(NO3)39H2O lithium is changed to iron chloride, nickel nitrate changes
At nickel acetate.
Detect example 1
Electronic display is scanned to composite material B1 by scanning electron microscope Hitachi s-4800 (Hitachi, Japan)
Micro mirror detection, concrete outcome are shown in Fig. 1, can be learnt by Fig. 1: obtained B1 is to be attached in nickel foam to have lamella knot
Substance.
The product of embodiment 2-8 is detected in the same manner, the SEM figure of testing result and B1 are basic to keep one
It causes.
Detect example 2
Projection electron microscope inspection is carried out to B1 by projection electron microscope Hitachi, HT-7700 (Hitachi, Japan)
Survey, concrete outcome is shown in Fig. 2, can be learnt by Fig. 2: obtained B1 be the substance with lamella knot being attached in nickel foam and
There is molecule on lamellar structure surface.
The product of embodiment 2-8 is detected in the same manner, the TEM figure of testing result and B1 are basic to keep one
It causes.
Detect example 3
By the analysis of Rigaku D/max-2500V type x ray diffractometer x, (x-ray source is Cu K α line, through K α2At removing
Reason, λ=0.15406nm, acceleration voltage 40kV, electric current 100mA, scanning speed 8o/min, 2 θ of scanning range are 20-
80 °, step-length is 0.02 °) X-ray powder diffraction detection is carried out to B1, concrete outcome is shown in Fig. 3, with standard card PDF#49-
0188 comparison is it is found that resulting substance B 1 is iron nickel layered double-hydroxide.
The product of embodiment 2-8 is detected in the same manner, the XRD diagram of testing result and B1 keep one substantially
It causes.
Application examples 1
Using B1 as working electrode, platinum electrode is used as to electrode, and Ag/AgCl is as reference electrode in oxygen or nitrogen
Under the premise of saturation, linear sweep voltammetry song is carried out using occasion China CHI760 electrochemical workstation in 1mol/L KOH solution
The scanning voltage of line, polarization curve is 0-0.7V (vs.Ag/AgCl) or 0~-1.5V (vs.Ag/AgCl), is linearly being swept
Retouching volt-ampere curve scanning is that oxygen or nitrogen holding are passed through, and testing conditions are room temperature normal pressure, and concrete outcome is shown in Fig. 4 and Fig. 5, by
Oxygen is precipitated in 10mA cm- known to Fig. 42When, current potential is 0.413V (vs.Ag/AgCl), overpotential 197mV；Hydrogen as shown in Figure 5
It is precipitated in 10mA cm-2When, current potential is -1.152V (vs.Ag/AgCl), overpotential 129mV.
The product of embodiment 2-8 is detected in the same manner, the testing result of testing result and B1 are protected substantially
It holds consistent.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of preparation method of iron nickel layered double hydroxide/foam nickel composite material characterized by comprising
1) source of iron, ammonium fluoride, urea and nickel foam in the presence of the solvent, are subjected to solvent thermal reaction so that reaction product A is made；
2) nickel source, ammonium fluoride, urea, reaction product A in the presence of the solvent, are subjected to solvent thermal reaction so that the iron nickel is made
Layered double hydroxide/foam nickel composite material.
2. preparation method according to claim 1, wherein in step 1), the source of iron, ammonium fluoride, urea and foam
The amount ratio of nickel be 0.75mmol:1-8mmol:2-18mmol:1cm × 1cm-2.5cm × 4cm, the nickel foam with a thickness of
1.5mm；
Preferably, in step 1), the source of iron, solvent amount ratio be 0.75mmol:10-40mL.
3. preparation method according to claim 1, wherein in step 1) and step 2), the solvent thermal reaction is extremely
Meet the following conditions less: in carrying out under confined conditions, reaction temperature is 100-200 DEG C, reaction time 2-72h；
Preferably, reaction temperature is 120-180 DEG C, reaction time 6-15h；.
4. preparation method according to claim 1, wherein relative to 1cm × 1cm-2.5cm × 4cm nickel foam, in step
It is rapid 2) in, the dosage of the nickel source is 0.015-1.5mmol, and the dosage of the ammonium fluoride is 0.1-0.8mmol, the urea
Dosage is 0.2-1.8mmol；
Preferably, relative to 1cm × 1cm-2.5cm × 4cm nickel foam, in step 2), the dosage of the solvent is 10-
40mL。
5. preparation method according to claim 1, wherein the source of iron is selected from ferric nitrate, ferric nitrate hydrate, chlorination
Iron, iron chloride hydrate, ferric acetate, ferric acetate hydrate, ferric carbonate, ferric carbonate hydrate, frerrous chloride, frerrous chloride hydration
One of object, ferrous acetate, ferrous acetate hydrate, ferrous carbonate, ferrous carbonate hydrate are a variety of,；The nickel source choosing
From one of nickel nitrate, nickel nitrate hydrate, nickel chloride, nickel chloride hydrate, nickel acetate, nickel acetate hydrate or a variety of；
The solvent is water.
6. preparation method according to claim 1, wherein the specification of the single side of the nickel foam are as follows: surface density be 380 ±
20g/m2, the hole count of per inch is 110.
7. preparation method according to claim 1, wherein after solvent thermal reaction in step 1) and 2), the preparation
Method is equal further include: reaction system is cooled to 15-35 DEG C in a manner of natural cooling.
8. a kind of iron nickel layered double hydroxide/foam nickel composite material, which is characterized in that the iron nickel layered bi-metal
Hydroxide/foam nickel composite material is prepared by preparation method described in any one of claim 1-7.
9. a kind of iron nickel layered double hydroxide/foam nickel composite material as claimed in claim 8 in evolving hydrogen reaction and
Application in oxygen evolution reaction.
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