CN110227496A - A kind of microspheroidal Fe the doping three nickel nano structural material of curing, preparation method and application of nanometer sheet composition - Google Patents
A kind of microspheroidal Fe the doping three nickel nano structural material of curing, preparation method and application of nanometer sheet composition Download PDFInfo
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- CN110227496A CN110227496A CN201910521743.6A CN201910521743A CN110227496A CN 110227496 A CN110227496 A CN 110227496A CN 201910521743 A CN201910521743 A CN 201910521743A CN 110227496 A CN110227496 A CN 110227496A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000000463 material Substances 0.000 title claims abstract description 54
- 239000000203 mixture Substances 0.000 title claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000006260 foam Substances 0.000 claims abstract description 22
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 150000002815 nickel Chemical class 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 14
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000004502 linear sweep voltammetry Methods 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 230000010287 polarization Effects 0.000 description 9
- 238000005868 electrolysis reaction Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 238000002083 X-ray spectrum Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910003298 Ni-Ni Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000005595 deprotonation Effects 0.000 description 1
- 238000010537 deprotonation reaction Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 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
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- 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
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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
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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)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of microspheroidal Fe of nanometer sheet composition to adulterate three nickel nano structural material of curing, preparation method and application.Nickel salt, molysite and thiocarbamide are dissolved in ethylene glycol, solution is transferred in reaction kettle, nickel foam inclination is placed in solution, carry out solvent thermal reaction, it is cooled to room temperature after reaction, product is washed, dry, can be prepared by the microspheroidal Fe doping Ni of nanometer sheet composition3S2Nano structural material.Compared with prior art, the present invention designs the microspheroidal Fe doping Ni for having synthesized nanometer sheet composition in conductive foam nickel substrate3S2Nanostructure.The electrochemical surface area and electric conductivity for improving material are adulterated using Fe.The microspheroidal Fe of nanometer sheet composition provided by the invention adulterates Ni3S2Nano structural material reacts elctro-catalyst as oxygen evolution reaction, evolving hydrogen reaction and total moisture solution, has the advantages that catalytic activity height and excellent in stability and preparation process are simple, low in cost.
Description
Technical field
The invention belongs to preparation method of nano material and electro-catalysis application fields, and in particular to a kind of nanometer sheet composition it is micro-
Spherical Fe adulterates Ni3S2Nano structural material, preparation method and application.
Background technique
Electro-catalysis water resolves into hydrogen and oxygen provides a kind of perspective and competing technology, sustainable and can to generate
The renewable sources of energy.However, the high overpotential of oxygen evolution reaction (OER) and evolving hydrogen reaction (HER) half-cell reaction, seriously limits full water
The practical application of decomposition.The progress of this technology needs activity high, and stability is by force and electrocatalysis material at low cost is to reduce energy
Measure the total energy efficiency that potential barrier improves OER and HER process.
In recent years, a large amount of research work is dedicated to OER the and HER elctro-catalyst that earth resource is abundant, cost performance is high.3d
Transistion metal compound can obtain high catalytic performance by adjusting its Nomenclature Composition and Structure of Complexes, attract extensive attention.In these catalysis
In agent, nickel based compound, such as nickel sulfide have unique structure and high electric conductivity, are that a kind of promising water decomposition electricity is urged
Agent.Ni3S2In Ni-Ni key than other Ni based compounds, there are more covalent bonds, under similar operating condition have anti-corruption
Corrosion energy.Control pattern or the other elements of doping enter Ni3S2Lattice can be improved electro-catalysis water dispersible energy.Building one meticulously
The nanometer nickel sulfide structural material of kind of heteroatom doping, while regulating and controlling pattern and electronic structure obtains high electric conductivity and solely
Special surface chemistry is conducive to the dissociation of water, and then further increases electro-catalysis water decomposition behavior, extremely important to practical application,
It but still is a very big challenge.
Summary of the invention
The purpose of the present invention is to provide a kind of microspheroidal Fe of nanometer sheet composition to adulterate Ni3S2Nano structural material and its
Preparation method, using cryochemistry liquid phase method, directly design synthesizes the microspheroidal that nanometer sheet forms in conductive foam nickel substrate
Fe adulterates Ni3S2Nanostructure, synthesis technology is simple, at low cost.
The present invention also provides a kind of microspheroidal Fe of nanometer sheet composition to adulterate Ni3S2Nano structural material is anti-as analysis oxygen
Answer the application of (OER), evolving hydrogen reaction (HER) or total moisture solution reaction elctro-catalyst.
A kind of microspheroidal Fe of nanometer sheet composition provided by the invention adulterates Ni3S2The preparation method of nano structural material, packet
Include following steps:
A kind of microspheroidal Fe doping Ni of nanometer sheet composition3S2The preparation method of structural material, the preparation method include with
Lower step:
Nickel salt, molysite and thiocarbamide are dissolved in ethylene glycol, solution is transferred in reaction kettle, nickel foam inclination is placed in
In solution, solvent thermal reaction is carried out, is cooled to room temperature after reaction, product is washed, dry, can be prepared by nanometer sheet composition
Microspheroidal Fe adulterate Ni3S2Nano structural material.
Further, the nickel salt is Nickelous nitrate hexahydrate；The molysite is Fe(NO3)39H2O.
The ratio between amount of substance of the nickel salt, molysite, thiocarbamide is 0.75~1.25:0.2~0.5:0.75, preferably
0.75~1.25:0.3:0.75.
Concentration of the thiocarbamide in ethylene glycol is 0.0375M.
The condition of the solvent thermal reaction is to react 6-10h, preferably 140 DEG C reaction 8h at 140 DEG C.
It needs to be cleaned before nickel foam (NF) use, specific cleaning step are as follows: first removed with 6M salt acid soak 15min
Then the oxidation film of outer layer is respectively cleaned 3-5 times with deionized water and dehydrated alcohol；In use, to be cut into 2 × 3cm big for nickel foam
It is small.
The washing is respectively to be cleaned 3-5 times with deionized water and dehydrated alcohol.
The drying is the dry 6-12h in 55-60 DEG C of vacuum oven.
The present invention also provides a kind of microspheroidal Fe doping of nanometer sheet composition being prepared such as above-mentioned preparation method
Ni3S2Nano structural material, the microspheroidal Fe adulterate Ni3S2The pattern of nano structural material is the average ruler of nanometer sheet composition
The very little microspheroidal structure for being 250~350nm.
The present invention also provides the microspheroidal Fe of nanometer sheet composition to adulterate Ni3S2Nano structural material is anti-as analysis oxygen
Answer or evolving hydrogen reaction or total moisture solution reaction elctro-catalyst application.
The Fe of the nanometer sheet composition adulterates Ni3S2Nano structural material is as oxygen evolution reaction (OER) or evolving hydrogen reaction
(HER) elctro-catalyst in application, method particularly includes: by the nanometer sheet prepared in nickel foam composition microspheroidal Fe adulterate
Ni3S2Nano structural material is cut into 1 × 1cm size as working electrode, using 1M KOH solution as electrolyte, with CHI 760E electricity
Chem workstation is tested.With platinum filament (OER reaction) or carbon-point (HER reaction) and Ag/AgCl electrode respectively as to electrode
And reference electrode.Using linear sweep voltammetry (LSV) in 2.0mVs-1Sweep speed and ohm compensation lower obtained for 90%
Polarization curve；Stability is obtained by measuring current density time graph under constant voltage.Electrochemical surface area (ECSA)
Pass through (2,4,6,8,10, the 12 and 14mVs under without apparent faraday region different scanning rates-1) cyclic voltammetric (CV) survey
Measure electric double layer capacitance (Cdl) assessed；Electrochemical impedance (EIS) open-circuit electricity in the frequency range of 100kHz to 0.1Hz
Pressure is tested.With business RuO2It is supported in nickel foam with Pt/C as electrode, measures the performance conduct of OER and HER respectively
Compare.
The Fe adulterates Ni3S2The elctro-catalyst that nano structural material is reacted as total moisture solution in application, specific method
Are as follows: the microspheroidal Fe of the nanometer sheet prepared in nickel foam composition is adulterated into Ni3S2It is big that nano structural material is cut into 21 × 1cm
It is small respectively as cathode and anode assembling in dual-electrode electrolysis slot, by 90%iR compensation LSV polarization curve and constant
Voltage, current density time curve tests total moisture solution performance.As a comparison, it has studied and is supported on bubble in dual-electrode electrolysis slot
Noble metal RuO on foam nickel2LSV polarization curve as anode and Pt/C as cathode.
In the present invention, Fe adulterates the adjusting for realizing electronic structure, improves electric conductivity, increases electro-chemical activity face
Product.The overlapping of d-d track keeps charge delocalized between metal cation in lattice, enhances lewis acidity, promotes the absorption of water
And activation, increase the electrophilicity of absorption oxygen, O-OH species are then formed by nucleophilic attack, is further induced by electrophilic
Effect makes OOH species deprotonation, generates oxygen.Moreover, the delocalized of electronics provides the confession of oxygen reversible adsorption between cation
Receptor body chemisorption site.In strong alkaline electrolytes, catalyst surface forms thin surface oxidation in electrolytic process
Nitride layer or surface hydroxide layer are actual active sites, and the Fe of more high conductivity adulterates Ni under surface3S2Can speed up electrode and
Electronics transfer between metal oxide or metal hydroxides shell.At the same time, surface thin oxide or hydroxide
Shell can reduce S-HadsThe formation of key, and S-HadsKey is typically too stable and makes HadsIt is converted into H2It is difficult.The material is in alkalinity
Excellent activity and outstanding durability are shown to the reaction of oxygen evolution reaction, evolving hydrogen reaction and total moisture solution in electrolyte, it is right
The practical application of research water decomposition electro catalytic electrode material has value very much.
Compared with prior art, the present invention utilizes thiocarbamide by simple chemical liquid phase reaction in conductive substrates nickel foam
It decomposes and generates S2-Ion, with Ni2+Ionic reaction obtains Ni3S2Seed, while a small amount of Fe3+Ion mixes Ni3S2Lattice.In crystalline substance
Under the collective effect of the intrinsic layer structure driving of body and glycol molecule coordination effect, further growth obtains nanometer sheet composition
Microspheroidal Fe adulterate Ni3S2Nanostructure.The microspheroidal Fe of the nanometer sheet composition of preparation adulterates Ni3S2Nano structural material pair
Oxygen evolution reaction, evolving hydrogen reaction and the reaction of total moisture solution show excellent catalytic activity and stability, and preparation process ring
Border is friendly, simple, at low cost.
Detailed description of the invention
Fig. 1 is that the microspheroidal Fe of nanometer sheet composition prepared by embodiment 1 adulterates Ni3S2The X-ray powder of nano structural material
Last diffraction (XRD) figure；
Fig. 2 is that the microspheroidal Fe of nanometer sheet composition prepared by embodiment 1 adulterates Ni3S2The energy dispersion X of nano structural material
Ray spectrum (EDX) figure；
Fig. 3 is that the microspheroidal Fe of nanometer sheet composition prepared by embodiment 1 adulterates Ni3S2The scanning electron of nano structural material
Microscope (SEM) figure；
Fig. 4 is that the microspheroidal Fe of nanometer sheet composition prepared by embodiment 1 adulterates Ni3S2The transmitted electron of nano structural material
Microscope (TEM) figure；
Fig. 5 is that the microspheroidal Fe of nanometer sheet composition prepared by embodiment 1 adulterates Ni3S2The scanning transmission of nano structural material
Electron microscope picture (STEM) and corresponding distribution diagram of element；
Fig. 6 is the microspheroidal Fe doping for the nanometer sheet composition that Fe doping prepared by embodiment 2 is 14.0% and 20.9%
Ni3S2X-ray powder diffraction (XRD) figure of nano structural material；
Fig. 7 is the microspheroidal Fe doping for the nanometer sheet composition that Fe doping prepared by embodiment 2 is 14.0% and 20.9%
Ni3S2Energy dispersion X-ray spectrum (EDX) figure of nano structural material；
Fig. 8 is the microspheroidal Fe doping Ni for the nanometer sheet composition that Fe doping prepared by embodiment 2 is 14.0%3S2Nanometer
Scanning electron microscope (SEM) figure of structural material；
Fig. 9 is the microspheroidal Fe doping Ni for the nanometer sheet composition that Fe doping prepared by embodiment 2 is 20.9%3S2Nanometer
Scanning electron microscope (SEM) figure of structural material；
For different Fe contents prepared by embodiment 1 and embodiment 2, (14.0%, 16.9% and Fe 20.9%) mixes Figure 10
Miscellaneous Ni3S2The LSV curve graph of the oxygen evolution reaction (OER) of product；
For different Fe contents prepared by embodiment 1 and embodiment 2, (14.0%, 16.9% and Fe 20.9%) mixes Figure 11
Miscellaneous Ni3S2The LSV curve graph of the evolving hydrogen reaction (HER) of product.
Figure 12 is that the microspheroidal Fe of 3 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material oxygen evolution reaction (OER)
LSV curve graph；
Figure 13 is that the microspheroidal Fe of 3 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material oxygen evolution reaction (OER)
Current density time plot；
Figure 14 is that the microspheroidal Fe of 3 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material sweeps the electricity under speed in difference
Capacitance current figure；
Figure 15 is that the microspheroidal Fe of 3 nanometer sheet of embodiment composition adulterates Ni3S2The impedance diagram of nano structural material；
Figure 16 is that the microspheroidal Fe of 4 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material evolving hydrogen reaction (HER)
LSV curve graph；
Figure 17 is that the microspheroidal Fe of 4 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material evolving hydrogen reaction (HER)
Current density time plot；
Figure 18 is that the microspheroidal Fe of 5 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material is complete in two electrode systems
The polarization curve of water decomposition；
Figure 19 is that the microspheroidal Fe of 5 nanometer sheet of embodiment composition adulterates Ni3S2Nano structural material is complete in two electrode systems
The current density time plot of water decomposition.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention is described in detail.
Embodiment 1
A kind of microspheroidal Fe doping Ni of nanometer sheet composition3S2The preparation method of nano structural material, comprising the following steps:
The nickel foam of 2 × 3cm size is immersed in 6M hydrochloric acid solution, after 15min, with deionized water and dehydrated alcohol point
Qing Xi not be nickel foam 3 times, it is dry, obtain the nickel foam of surface cleaning.Clean small beaker is added in the accurate 40mL ethylene glycol that measures
In, 2mmol Ni (NO is then weighed respectively3)2·6H2O, 0.6mmol Fe (NO3)3·9H2Small burning is added in O and 1.5mmol thiocarbamide
Cup, stirring and dissolving 20min obtain homogeneous solution.Solution is transferred to the stainless steel cauldron that 50mL polytetrafluoroethylene (PTFE) is liner
In, the nickel foam oblique cutting pre-processed is entered in solution, seal simultaneously react 8h in 140 DEG C of baking ovens, to after reaction from
It is so cooled to room temperature, the nickel foam for covering sample deionized water and dehydrated alcohol is respectively cleaned 3 times, are then placed on nickel foam
The microspheroidal Fe doping Ni of nanometer sheet composition can be obtained in 60 DEG C of dry 10h in vacuum oven3S2Nano structural material.
It carries out object to 1 products therefrom of embodiment with X-ray powder diffraction instrument mutually to characterize, as a result as shown in Figure 1, all spread out
Penetrate peak with the hexagonal phase Ni in JCPDS no.44-1418 card3S2It coincide, compared to standard card number, diffraction maximum is obviously right
It moves, illustrates that Fe doping changes the electronic structure of material.
Product is analyzed using energy dispersion X-ray spectrum (EDX), as shown in Fig. 2, showing Fe element success coupling
It closes in sample, wherein Fe and S Elements Atom percentage is 0.38:1, and calculating Fe doping accordingly is 16.9%.
Morphology analysis, as shown in Fig. 3, table are carried out to sample prepared by embodiment 1 using scanning electron microscope (SEM)
Bright sample is the microspheroidal nanostructure of nanometer sheet composition, and microballoon average-size is 250~350nm.
The pattern of sample is further looked at using transmission electron microscope (TEM), as a result as shown in figure 4, showing that sample is
The microspheroidal nanostructure being made of flexible nanometer sheet.
The scanning transmission electron microscope picture (STEM) of Fig. 5 further illustrates that sample is the spherical knot of nanometer sheet composition
Structure, corresponding distribution diagram of element illustrate being uniformly distributed for Ni, Fe and S element.
Embodiment 2
The accurate 40mL ethylene glycol that measures is added in clean small beaker, then weighs the Ni (NO of 2mmol respectively3)2·
6H2Fe (the NO of O, 0.4mmol or 0.8mmol3)3·9H2Small beaker is added in the thiocarbamide of O and 1.5mmol, stirs evenly.It will dry
Nickel foam oblique cutting afterwards enters in the stainless steel cauldron that 50mL polytetrafluoroethylene (PTFE) is liner, is transferred to after completely dissolution to solution anti-
Answer in kettle, after sealing in an oven 140 DEG C react 8 hours.To fully reacting, cooled to room temperature will cover the bubble of sample
Foam nickel deionized water and washes of absolute alcohol several times, then by the nickel foam for covering sample put in a vacuum drying oven 60 DEG C it is dry
Dry 12 hours, the Fe that the nanometer sheet that Fe doping is 14.0% and 20.9% forms can be obtained and adulterate Ni3S2Microspheroidal nano junction
Structure.
It carries out object to 2 products therefrom of embodiment with X-ray powder diffraction instrument mutually to characterize, as a result as shown in fig. 6, all spread out
Penetrate peak with the hexagonal phase Ni in JCPDS no.44-1418 card3S2It coincide, compared to standard card number, diffraction maximum is moved to right.
Product is analyzed using energy dispersion X-ray spectrum (EDX), as shown in fig. 7, wherein Fe and S Elements Atom
Percentage is respectively 0.303:1 and 0.493:1, and calculating Fe doping accordingly is 14.0% and 20.9%.
Morphology analysis, Fig. 8 and Fig. 9 difference are carried out to sample prepared by embodiment 2 using scanning electron microscope (SEM)
It is that the Fe that Fe doping is 14.0% and 20.9% adulterates Ni3S2SEM figure, show sample be nanometer sheet composition microspheroidal
Nanostructure.
Figure 10 is that the Fe with 14.0%, 16.9% and 20.9% difference Fe content adulterates Ni3S2The oxygen evolution reaction of product
(OER) polarization curve.Showing Fe doping significantly influences OER activity, and the sample of Fe doping 16.9% is better than 14.0% He
20.9% sample.
Figure 11 is that the Fe with 14.0%, 16.9% and 20.9% difference Fe content adulterates Ni3S2The evolving hydrogen reaction of product
(HER) polarization curve.Show that Fe doping also significantly affects the HER activity of catalyst, the sample of Fe doping 16.9% reaches
Most preferably.
Embodiment 3
A kind of microspheroidal Fe doping Ni of nanometer sheet composition3S2Nano material is answered as oxygen evolution reaction (OER) catalyst
With.
Concrete application method are as follows: the microspheroidal Fe for forming the nanometer sheet of 1 × 1cm of area adulterates Ni3S2Nano material conduct
Working electrode is made in 1.0M KOH electrolyte solution with platinum filament and Ag/AgCl electrode respectively as to electrode and reference electrode
It is tested with CHI760E electrochemical workstation.Using linear sweep voltammetry (LSV) in 2.0mVs-1Sweep speed and
Ohm compensation is 90% lower acquisition polarization curve.As shown in figure 12, Fe adulterates Ni3S2The mistake that nanostructure only needs 233mV low
Current potential can realize 50mAcm-2Current density, compare Ni respectively3S2With business RuO2Small 92mV and 57mV, Ni3S2System
Standby is the Fe (NO eliminated in raw material on the basis of embodiment 13)3·9H2What O was prepared.It is adopted at overpotential 248mV
OER electro-catalysis stability is assessed with current density time graph, as a result as shown in figure 13.Continuous electrolysis by 14 hours is anti-
It answers, current density remains initial 98.3%, shows excellent electro-catalysis stability.With electric double layer capacitance assessment material
Electrochemical surface area, as shown in figure 14, Fe adulterate Ni3S2Electric double layer capacitance is 7.93mFcm-2, it is greater than Ni3S2's
3.87mF·cm-2, show that Fe doping increases the electrochemical surface area of sample.Electrochemical impedance (EIS) chart of Figure 15 is bright
Fe adulterates Ni3S2Half circular diameter of nanostructure is small, and straight slope is big, illustrates that its resistance is small, has faster catalytic kinetic
It learns.
Embodiment 4
A kind of microspheroidal Fe doping Ni of nanometer sheet composition3S2Nano structural material is as evolving hydrogen reaction (HER) catalyst
Application.
Concrete application method are as follows: the microspheroidal Fe for forming the nanometer sheet of 1 × 1cm of area adulterates Ni3S2Nano structural material
As working electrode, with carbon-point and Ag/AgCl electrode respectively as to electrode and reference electrode, in 1.0M KOH electrolyte solution
It is middle to be tested using CHI760E electrochemical workstation.Using linear sweep voltammetry (LSV) in 2.0mVs-1Scanning speed
Rate and ohm compensation are 90% lower acquisition polarization curve.As shown in figure 16, Fe adulterates Ni3S2Nanostructure is under 130mV overpotential
10mAcm can be reached-2Current density is much smaller than Ni3S2The 193mV of catalyst.Although Pt/C electrode is under low current density
Show HER outstanding activity, but overpotential increase is quickly at higher current densities.Because Pt/C is being steeped by adhesive load
It is easy to fall off on foam nickel.The stability of HER electro-catalysis is assessed using current density time graph under constant overpotential 167mV,
As shown in figure 17, it is reacted by 14 hours continuous electrolysis, current density remains initial 93.9%, shows good
HER electro-catalysis stability.
Embodiment 5
A kind of microspheroidal Fe doping Ni of nanometer sheet composition3S2Nano structural material is as total moisture solution catalysts
Using.
Concrete application method are as follows: the Fe that 2 areas are 1 × 1cm is adulterated into Ni3S2Nanostructure is respectively as anode and yin
Pole is assembled in dual-electrode electrolysis slot, passes through current density under the LSV polarization curve (Figure 18) and constant voltage of 90%iR compensation
Time graph (Figure 19) tests total moisture solution performance in 1.0M KOH electrolyte solution.Fe adulterates Ni3S2Nanostructure exists
10mAcm can be reached under the voltage of 1.58V-2Current density, although slightly above Pt/C//RuO2The voltage 1.50V of electricity pair, but
There is no apparent decaying occurs, current density remains initial continuous electrolysis within 14 hours at constant voltage 1.627V for it
98.6%, illustrate that it has excellent durability in dual-electrode electrolysis slot.
A kind of above-mentioned microspheroidal Fe doping three nickel nano structural material of curing that nanometer sheet is formed referring to embodiment, system
The detailed description that Preparation Method and application carry out, is illustrative without being restrictive, if can enumerate according to limited range
Dry embodiment, therefore the change and modification in the case where not departing from present general inventive concept, should belong within protection scope of the present invention.
Claims (9)
1. a kind of microspheroidal Fe of nanometer sheet composition adulterates Ni3S2The preparation method of nano structural material, which is characterized in that described
Preparation method the following steps are included:
Nickel salt, molysite and thiocarbamide are dissolved in ethylene glycol, solution is transferred in reaction kettle, nickel foam inclination is placed in solution
In, solvent thermal reaction is carried out, is cooled to room temperature after reaction, product is washed, dry, can be prepared by the micro- of nanometer sheet composition
Spherical Fe adulterates Ni3S2Nano structural material.
2. preparation method according to claim 1, which is characterized in that the nickel salt is Nickelous nitrate hexahydrate；The molysite
For Fe(NO3)39H2O.
3. preparation method according to claim 1 or 2, which is characterized in that the nickel salt, molysite, thiocarbamide substance amount
The ratio between be 0.75~1.25:0.2~0.5:0.75.
4. preparation method according to claim 1 or 2, which is characterized in that concentration of the thiocarbamide in ethylene glycol is
0.0375 M。
5. preparation method according to claim 1 or 2, which is characterized in that the condition of the solvent thermal reaction is at 140 DEG C
React 6-10h.
6. a kind of microspheroidal Fe of the nanometer sheet that the preparation method as described in claim 1-5 any one is prepared composition mixes
Miscellaneous Ni3S2Nano structural material.
7. the microspheroidal Fe of nanometer sheet composition according to claim 6 adulterates Ni3S2Nano structural material is as oxygen evolution reaction
(OER) application of elctro-catalyst.
8. the microspheroidal Fe of nanometer sheet composition according to claim 6 adulterates Ni3S2Nano structural material is as evolving hydrogen reaction
(HER) application of elctro-catalyst.
9. the microspheroidal Fe of nanometer sheet composition according to claim 6 adulterates Ni3S2Nano structural material is as total moisture solution
React the application of elctro-catalyst.
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