CN110280275A - A kind of Fe doping four three nanosized nickel rods of selenizing/nanometer sheet hierarchical array structural material, preparation method and applications - Google Patents
A kind of Fe doping four three nanosized nickel rods of selenizing/nanometer sheet hierarchical array structural material, preparation method and applications Download PDFInfo
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- CN110280275A CN110280275A CN201910521779.4A CN201910521779A CN110280275A CN 110280275 A CN110280275 A CN 110280275A CN 201910521779 A CN201910521779 A CN 201910521779A CN 110280275 A CN110280275 A CN 110280275A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 239000000463 material Substances 0.000 title claims abstract description 58
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000243 solution Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000006260 foam Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000002505 iron Chemical class 0.000 claims abstract description 3
- 239000011669 selenium Substances 0.000 claims description 79
- 238000004458 analytical method Methods 0.000 claims description 5
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 4
- 238000013019 agitation Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 3
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 17
- 230000010287 polarization Effects 0.000 description 15
- 238000006555 catalytic reaction Methods 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000005611 electricity Effects 0.000 description 7
- 239000012467 final product Substances 0.000 description 7
- -1 nickelous selenide Chemical class 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- 238000004502 linear sweep voltammetry Methods 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 5
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 238000012546 transfer Methods 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
- 238000004140 cleaning Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 150000003346 selenoethers Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005595 deprotonation Effects 0.000 description 1
- 238000010537 deprotonation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 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
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005259 measurement Methods 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
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
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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
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- 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
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- 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
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Abstract
The invention discloses a kind of Fe to adulterate four three nanosized nickel rods of selenizing/nanometer sheet hierarchical array structural material, preparation method and applications.The preparation method comprises the following steps: Se powder and reducing agent being dissolved in ammonium hydroxide and the mixed solution of deionized water, nickel foam inclination is placed in mixed solution, obtains the nickel foam of presoma through hydro-thermal reaction；Iron salt dissolved is put into the nickel foam of presoma in the mixed solution of ethyl alcohol and NaClO again, obtains product through solvent thermal reaction.Compared with prior art, the present invention utilizes low temperature liquid phase synthetic method, by Fe3+Ion doping is to Ni3Se4In the lattice of classification nanostructure, method is simple, at low cost；The advantages that reacting the big active area of elctro-catalyst, good conductivity as oxygen evolution reaction (OER), evolving hydrogen reaction (HER) and total moisture solution；Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is able to achieve efficient total moisture solution at higher current densities, and it is low, outstanding stability is shown under high current density.
Description
Technical field
The invention belongs to preparation method of nano material and electro-catalysis cross-application fields, and in particular to a kind of four selenium of Fe doping
Change three nanosized nickel rods/nanometer sheet hierarchical array structural material, preparation method and applications.
Background technique
Electro-catalysis water decomposition generates cleaning and recyclable fuel includes Oxygen anodic evolution reaction (OER) and cathode hydrogen evolution reaction
(HER).The progress of the technology needs active, stable and cheap elctro-catalyst to reduce overpotential and accelerate moving for OER and HER
Mechanics.3d transistion metal compound accurately controls the good catalytic performance of its Nomenclature Composition and Structure of Complexes acquisition due to that can pass through, and is considered
It is ideal water decomposition elctro-catalyst.Wherein, nickel based compound, such as nickelous selenide, have unique electronic structure, it is cheap and
It is easily obtained, is explored as OER and HER elctro-catalyst.
However, selenizing nickel material higher overpotential in electro-catalysis water decomposition increases energy consumption, after long-time service
It is easy to change in structure, limits its practical application in electro-catalysis water decomposition.Heterogeneous cation doping nickelous selenide can be adjusted
Its electronic structure is saved, exposed active sites are increased, OER and total moisture solution performance can be obviously improved.In selenides, Ni3Se4Than it
He is selenides such as NiSe and NiSe2With higher electric conductivity, has and improve the active potentiality of electro-catalysis water decomposition.But about change
Learn the Ni of doping3Se4For being rarely reported for electro-catalysis total moisture solution application.Therefore a kind of specific cation is constructed meticulously to mix
Miscellaneous Ni3Se4Nanostructure, regulates and controls pattern and electronic structure, and enhancing electric conductivity increases active sites to realize electro-catalysis water outstanding
Degrading activity and stability have great importance.
Summary of the invention
The purpose of the present invention is to provide a kind of Fe to adulterate four three nanosized nickel rods of selenizing/nanometer sheet hierarchical array structural material
And preparation method thereof, using low temperature liquid phase synthetic method, Fe is synthesized as conductive substrates using nickel foam and adulterates Ni3Se4Nanometer rods/nanometer
Piece hierarchical array structural material, the synthetic method are simple, at low cost.
The present invention also provides a kind of Fe to adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical array 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 Fe provided by the invention adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material preparation method, packet
Include following steps:
(1) Se powder and reducing agent are dissolved in ammonium hydroxide and the mixed solution of deionized water, are stirred by ultrasonic, obtain solution A,
Then solution A is transferred in reaction kettle, nickel foam inclination is placed in solution A, hydro-thermal reaction is carried out, naturally cools to room
Temperature, washing, dry, the obtained nickel foam for having presoma；
(2) by iron salt dissolved in ethyl alcohol and the mixed solution of NaClO, solution B is obtained, is then transferred to solution B instead
It answers in kettle, the nickel foam for having presoma prepared by step (1) is tiltedly placed in solution B, solvent thermal reaction is carried out, to the end of reacting
Cooled to room temperature afterwards, washing, dry, obtained Fe doping Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material.
Further, in step (1), the ratio between amount of substance of the Se powder and reducing agent be 1:2.3-2.8, preferably 1:
2.5。
The reducing agent is NaBH4；The molysite is Fe (NO3)3·9H2O。
In step (1), the volume ratio of the ammonium hydroxide and deionized water is 5-15:35-25；The selenium powder is in solution A
Concentration is 20-30mM, preferably 25mM.
In step (1), the condition of the hydro-thermal reaction is to react 8-12h, preferably 120 DEG C reaction 8h at 120 DEG C.
In step (1), the nickel foam is using preceding needing to be cleaned, specific cleaning method are as follows: first uses 6M salt acid soak
15min removes the oxidation film of outer layer, then uses deionized water and washes of absolute alcohol, and when use is cut into 2 × 3cm size.
In step (1), the hydro-thermal reaction carries out in the stainless steel cauldron of polytetrafluoroethyllining lining；The washing
Are as follows: it is first washed with deionized 3-5 times, then is washed 3-5 times with dehydrated alcohol；The drying are as follows: in 55-60 DEG C of vacuum oven
Dry 6-12h.
In step (2), concentration of the molysite in solution B is 20-30mM, preferably 25.8mM.
In step (2), the ratio between volume of the ethyl alcohol and NaClO is 150~180:1, preferably 160:1.
In step (2), the condition of the solvent thermal reaction is to react 4-8h at 140 DEG C, reacts 6h at preferably 140 DEG C.
In step (2), the solvent thermal reaction carries out in the stainless steel cauldron of polytetrafluoroethyllining lining；The washing
Are as follows: it is first washed with deionized 3-5 times, then is washed 3-5 times with dehydrated alcohol；The drying are as follows: in 55-60 DEG C of vacuum oven
Dry 6-12h.
The present invention also provides a kind of Fe being prepared such as above-mentioned preparation method to adulterate Ni3Se4Nanometer rods/nanometer sheet point
Grade array structure materials, the Fe adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material pattern is in average diameter
To grow the nanometer sheet that lateral dimension is 180~200nm in the nanometer rods of 50~70nm
The present invention also provides the Fe to adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is anti-as analysis oxygen
The application for the elctro-catalyst for answering (OER) or evolving hydrogen reaction (HER) or total moisture solution to react.
The Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is anti-as oxygen evolution reaction (OER) or liberation of hydrogen
Answer the elctro-catalyst of (HER) in application, method particularly includes: Ni is adulterated with the Fe3Se4Nanometer rods/nanometer sheet hierarchical array knot
Structure material is as working electrode, with platinum filament (OER reaction) or carbon-point (HER reaction) and Ag/AgCl electrode respectively as to electrode
And reference electrode, electrolyte are 1.0M KOH solution, carry out electro-chemical test using CHI760E electrochemical workstation.Linearly sweep
Polarization curve (LSV) is retouched in 2.0mVs-1Sweep speed under carry out, ohm compensation be 90%.By being surveyed under constant voltage
Constant current density time curve obtains stability.Electrochemical surface area (ECSA) without obvious faraday region difference by sweeping
(2,4,6,8,10 and 12mVs is retouched under rate-1) cyclic voltammetry measurement electrochemical double layer capacitor (Cdl) assessed；Electrochemistry
Impedance (EIS) open-circuit voltage in the frequency range of 100kHz to 0.1Hz is tested.With business RuO2It is supported on Pt/C
Electrode is used as in nickel foam, the performance for testing OER and HER respectively, which is used as, to be compared.
The Fe adulterates Ni3Se4The electro-catalysis that nanometer rods/nanometer sheet hierarchical array structural material is reacted as total moisture solution
Agent in application, method particularly includes: with the Fe adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material respectively as
Anode and cathode is assembled in dual-electrode electrolysis slot, tests linear scan polarization curve (LSV) and perseverance under 90% ohm of compensation
Current density time stability under constant voltage.As a comparison, your gold being supported in nickel foam in dual-electrode electrolysis slot had studied
Belong to RuO2LSV polarization curve as anode and Pt/C as cathode.
Fe provided by the invention adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material, Fe doping have adjusted
Ni3Se4Electronic structure, significantly enhance the electric conductivity and mass transfer behavior of material.Fe3+Ion doping enters Ni3Se4It is brilliant
Lattice can expose bigger catalytic active site, improve the practical contact interface area between electrolyte, ensure that quick boundary
Surface charge transfer, is conducive to electrocatalytic reaction.Metal cation is overlapping by the d-d track of intracell, realize charge from
Lewis acidity is promoted in domain, promotes the absorption and activation of water, increases the electrophilicity of absorption oxygen, then passes through nucleophilic attack shape
At O-OH species, O is further generated by the deprotonation of electrophilic inductive effect2.Charge delocalization turns to oxygen between cation
Reversible adsorption provides donor-receptor chemisorption position, is conducive to OER catalysis reaction.In strong alkaline electrolytes, catalyst surface
Oxide layer is formd in electrolytic process or surface hydroxide layer is actual active sites, more high conductivity under surface
Fe adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical structure can speed up electrode and metal oxide or metal hydroxides shell
Between electronics transfer.At the same time, the thin oxide shell layer in surface or hydroxide shell can stablize Fe as protective layer
Adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical structure.The a large amount of solid solid interfaces being formed in situ promote the chemistry of oxygen and hydrogen intermediate to inhale
It is attached, OER activity can not only be promoted and HER behavior can be promoted, to have excellent total moisture solution electrocatalysis characteristic.
Compared with the prior art, the present invention uses NaBH by simple chemical liquid phase reaction4It restores Se powder and forms Se2-Ion, with
The Ni reaction of foam nickel surface generates NiSe seed, and under the coordination of ammonium hydroxide molecule, NiSe seed oriented growth obtains selenium
Change nanosized nickel rods predecessor.Further ClO-Ion is by the Ni in NiSe2+Partial oxidation is at Ni3+, form Ni3Se4, nanometer rods portion
Dissolution is divided to be epitaxially grown to a nanometer chip architecture, while Fe3+Ion is coupled into Ni3Se4In lattice, fabricated in situ Fe3+Ion
The Ni of doping3Se4Nanometer rods/nanometer sheet hierarchical array structure.OER, HER and total moisture solution elctro-catalyst provided by the present invention
The application of material, low with overpotential under high current density, stability is good and preparation process is environmental-friendly, simply, at low cost
Honest and clean feature.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction (XRD) of predecessor NiSe nanometer stick array structural material prepared by embodiment 1
Figure；
Fig. 2 is that Fe prepared by embodiment 1 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material X-ray powder
Last diffraction (XRD) figure；
Fig. 3 is the scanning electron microscope (SEM) of predecessor NiSe nanometer stick array structural material prepared by embodiment 1
Figure；
Fig. 4 is that Fe prepared by embodiment 1 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material scanning electron
Microscope (SEM) figure；
Fig. 5 is that Fe prepared by embodiment 1 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material energy dispersion X
Ray (EDX) spectrum；
Fig. 6 is that Fe prepared by embodiment 1 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material transmitted electron
Microscope (TEM) figure；
Fig. 7 is that Fe prepared by embodiment 1 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material high-resolution is brilliant
Glazing bar line (HRTEM) image；
Fig. 8 is the scanning electron microscope (SEM) that Fe prepared by comparative example 1 adulterates NiSe nanometer stick array structural material
Figure；
Fig. 9 is that Fe prepared by embodiment 1 adulterates Ni3Se4Prepared by nanometer rods/nanometer sheet hierarchical array structure and comparative example 1
The OER polarization curve of Fe doping NiSe nanometer stick array structure.
Figure 10 is that Fe prepared by embodiment 1 adulterates Ni3Se4It is prepared by nanometer rods/nanometer sheet hierarchical array structure and comparative example 1
Fe doping NiSe nanometer stick array structure HER polarization curve.
Figure 11 is that Fe adulterates Ni in embodiment 23Se4Nanometer rods/nanometer sheet hierarchical array structural material OER linear polarization
Curve graph (illustration is the polarization curve under high current density)；
Figure 12 is that Fe adulterates Ni in embodiment 23Se4Nanometer rods/nanometer sheet hierarchical array structural material OER current density
Time plot；
Figure 13 is that Fe adulterates Ni in embodiment 23Se4Nanometer rods/nanometer sheet hierarchical array structural material is swept under speed in difference
Capacitance current figure；
Figure 14 is that Fe adulterates Ni in embodiment 23Se4Nanometer rods/nanometer sheet hierarchical array structural material impedance diagram；
Figure 15 is that Fe adulterates Ni in embodiment 33Se4Nanometer rods/nanometer sheet hierarchical array structural material HER linear polarization
Curve graph (illustration is the polarization curve under high current density)；
Figure 16 is that Fe adulterates Ni in embodiment 33Se4Nanometer rods/nanometer sheet hierarchical array structural material HER current density
Time plot；
Figure 17 is that Fe adulterates Ni in embodiment 43Se4Nanometer rods/nanometer sheet hierarchical array structural material is in two electrode systems
The polarization curve of total moisture solution (illustration is the polarization curve under high current density)；
Figure 18 is that Fe adulterates Ni in embodiment 43Se4Nanometer rods/nanometer sheet hierarchical array structural material is in two electrode systems
The current density time plot of total moisture solution；
Figure 19 is that Fe adulterates Ni in embodiment 53Se4Nanometer rods/nanometer sheet hierarchical array structural material dry electricity of one section 1.5V
The figure (figure that illustration is the amplification of two electrodes) of pond driving.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention is described in detail.
Embodiment 1
A kind of Fe doping Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material preparation method, comprising the following steps:
(1) nickel foam (NF) that a piece of area is 2 × 3cm is put into 6M hydrochloric acid and impregnates 15min, then use deionized water
It is respectively washed with dehydrated alcohol 3 times.It measures 15mL ammonium hydroxide to be added in 25mL deionized water, after mixing evenly, accurately weighs 1mmol
Se powder and 2.5mmol NaBH4Above-mentioned mixed solution is added, 30min is stirred by ultrasonic, red tan solution is then transferred to 50mL
Polytetrafluoroethylene (PTFE) be liner stainless steel cauldron in, the nickel foam pre-processed is tiltedly put into solution, 120 DEG C bakings
8h is reacted in case.To cooled to room temperature after reaction, the nickel foam A that black sample is covered1With deionized water and nothing
Water-ethanol respectively cleans 3 times, and obtained predecessor sample puts 60 DEG C of dry 10h in a vacuum drying oven.
(2) it first measures 40mL dehydrated alcohol to be added in clean small beaker, then pipettes 0.25mL liquor natrii hypochloritis addition
In dehydrated alcohol, stir evenly；Weigh 1mmol Fe (NO3)3·9H2O is added above-mentioned mixed solution, after stirring and dissolving, by solution
It is transferred in the stainless steel cauldron that 50mL polytetrafluoroethylene (PTFE) is liner, then nickel foam A1It is tiltedly put into solution, at 140 DEG C
8h is reacted in baking oven.Cooled to room temperature after complete reaction will cover the nickel foam deionized water and anhydrous second of sample
Alcohol respectively cleans 3 times, obtained sample A260 DEG C of dry 10h in a vacuum drying oven are put, Fe doping Ni can be obtained3Se4Nanometer
Stick/nanometer sheet hierarchical array structural material.
The structure and morphology characterization of product:
Discriminating materials are carried out to 1 gained predecessor of embodiment and final product with X-ray powder diffraction instrument (XRD), respectively
As shown in Figure 1, 2.Fig. 1 shows that predecessor is hexagonal phase NiSe (JCPDS no.75-0610) and orthorhombic phase NiSe (JCPDS
No.29-0935 mixed phase).Fig. 2 shows diffraction maximum and monoclinic system Ni all on final product3Se4Coincide (JCPDS
no.18-0890)。
Morphology analysis is carried out to 1 gained predecessor of embodiment and final product with scanning electron microscope (SEM), respectively such as
Fig. 3, shown in 4.Fig. 3 show predecessor be nanometer stick array structure, Fig. 4 show final sample be it is in the same size, be evenly distributed
Nanometer rods/nanometer sheet hierarchical structure.
Final product ingredient is analyzed using energy dispersion X-ray (EDX) spectrum.As shown in figure 5, the success of Fe element
Ground is coupled in sample, is 4.6% according to the doping that atomic percent calculates Fe element.
Transmission electron microscope (TEM) image of final product as shown in fig. 6, show that the diameter of nanometer rods is 50-70nm,
The lateral dimension of nanometer sheet is 180-200nm.
High resolution transmission electron microscopy (HRTEM) image of final product as shown in fig. 7, interplanar distance is 0.22nm,
Corresponding to Ni3Se4(211) crystal face.
Comparative example 1
(1) by 1mmol Se powder and 2.5mmol NaBH4It is dissolved in the mixed solution of 15mL ammonium hydroxide and 25mL deionized water
In, 30min is stirred by ultrasonic, obtains solution A, solution A is then transferred to the stainless steel reaction that 50mL polytetrafluoroethylene (PTFE) is liner
In kettle, nickel foam inclination is placed in solution A, reacts 8h in 120 DEG C of baking ovens.To cooled to room temperature after reaction,
The nickel foam A that black sample is covered1It is respectively cleaned 3 times with deionized water and dehydrated alcohol, obtained predecessor sample is placed on very
60 DEG C of dry 10h in empty drying box；
(2) by 1mmol Fe (NO3)3·9H2O is dissolved in 40mL dehydrated alcohol, obtains solution B, then turns solution B
It moves in the stainless steel cauldron that 50mL polytetrafluoroethylene (PTFE) is liner, the nickel foam for having presoma prepared by step (1) is tiltedly put
In solution B, 8h is reacted in 140 DEG C of baking ovens, to cooled to room temperature after reaction, washing, dry, obtained Fe doping
NiSe nanometer stick array structural material.
Morphology analysis is carried out to 1 gained final product of comparative example with scanning electron microscope (SEM).Fig. 8 shows finally to produce
Object is nanometer stick array structure.
Fig. 9 is that the Fe that embodiment 1 obtains adulterates Ni3Se4What nanometer rods/nanometer sheet hierarchical array structure and comparative example 1 obtained
The OER polarization curve of Fe doping NiSe nanometer stick array structure.Show that Fe adulterates Ni3Se4Sample adulterates NiSe sample better than Fe.
Figure 10 is that the Fe that embodiment 1 obtains adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structure and comparative example 1 obtain
Fe doping NiSe nanometer stick array structure OER polarization curve.Show that Fe adulterates Ni3Se4Sample adulterates NiSe sample better than Fe
Product.
Embodiment 2
A kind of Fe doping Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is as oxygen evolution reaction (OER) catalyst
Using.
Concrete application method are as follows: the Fe that usable floor area is 0.5 × 0.5cm adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array
Structural material is as working electrode, with platinum filament and Ag/AgCl electrode respectively as to electrode and reference electrode.In 1.0M KOH electricity
Electro-chemical test is carried out under room temperature (25 DEG C) using CHI760E electrochemical workstation in electrolyte solution.With business RuO2Load
On the basis of electrode, compare OER performance.Using linear sweep voltammetry (LSV) in 2.0mVs-1Sweep speed and ohm compensate
For 90% lower acquisition polarization curve.As shown in figure 11, Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structure has significant
OER activity, it is only necessary to 220mV low overpotential can reach 100mAcm-2Current density, respectively than NiSe nanometer rods (its
For the presoma of step (1) preparation in embodiment 1) and business RuO2The overpotential of catalyst small 99mV and 73mV；In addition, Fe
Adulterate Ni3Se4Nanometer rods/nanometer sheet hierarchical array structure can reach under the fairly small overpotential of 253mV and 264mV
500mA·cm-2And 800mAcm-2High current density.The current density time graph of Figure 12 shows that Fe adulterates Ni3Se4Nanometer
Stick/nanometer sheet hierarchical array structure shows good stability under low, high current density, after the test of 11h, electricity
Current density is held in 96.8% or more.Figure 13 is the different capacitance current figures swept under speed, shows that Fe adulterates Ni3Se4Electric double layer electricity
Holding is 3.4mFcm-2, 1.9mFcm greater than NiSe-2, therefore Fe adulterates Ni3Se4With bigger electrochemical surface area.
The bright Fe of electrochemical impedance (EIS) chart of Figure 14 adulterates Ni3Se4Half circular diameter of nanometer rods/nanometer sheet hierarchical array structure is small,
Straight slope is big, illustrates that its resistance is small, has faster catalytic kinetics.
Embodiment 3
A kind of Fe doping Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is as evolving hydrogen reaction (HER) catalyst
Using.
Concrete application method are as follows: the Fe that usable floor area is 0.5 × 0.5cm adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array
Structural material is as working electrode, with carbon-point and Ag/AgCl electrode respectively as to electrode and reference electrode.In 1.0M KOH electricity
Electro-chemical test is carried out under room temperature (25 DEG C) using CHI760E electrochemical workstation in electrolyte solution.It is lied prostrate using linear scan
Peace method (LSV) is in 2.0mVs-1Sweep speed and ohm compensation lower obtained for 90%.As shown in figure 15, Fe adulterates Ni3Se4
Nanometer rods/nanometer sheet hierarchical array structure has outstanding HER activity, it is only necessary to which the low potential of 153mV can reach 10mA
cm-2Current density, better than the 182mV of NiSe nanometer rods.Although business Pt/C electrode has lower under low current density
Overpotential, but at higher current densities, material easily falls off and influences activity.In addition, Fe adulterates Ni3Se4Nanometer rods/nanometer sheet
Hierarchical array structure can reach 100mAcm under the fairly small overpotential of 233mV and 269mV-2And 500mAcm-2It is big
Current density.The current density time graph of Figure 16 shows that Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structure it is low,
Excellent stability is all shown under high current density, after the test of 11h, current density is held in 96.2% or more.
Embodiment 4
A kind of Fe doping Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material reacts elctro-catalyst as total moisture solution
Application.
Concrete application method are as follows: the Fe that 2 areas are 0.5 × 0.5cm is adulterated into Ni3Se4Nanometer rods/nanometer sheet is classified battle array
Array structure material in dual-electrode electrolysis slot, is tested complete respectively as cathode and anode assembling in 1.0M KOH electrolyte solution
Water dispersible energy.Using linear sweep voltammetry (LSV) in 2.0mVs-1Sweep speed and ohm compensation lower obtained for 90%
Polarization curve.As shown in figure 17, Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material has excellent electro-catalysis
Total moisture solution activity, can reach 10mAcm under the voltage of 1.58V-2Current density, it is only necessary to the voltage energy of 1.94V
Drive 500mAcm-2High current density.Although business RuO2With Pt/C composition electricity under low current density activity slightly
Height, but 500mAcm is unable to reach because material easily falls off-2High current density.The current density time graph table of Figure 18
Bright Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structure shows good stability under low, high current density,
After the test of 11h, current density is held in 93.5% or more.
Embodiment 5
By a kind of Fe doping Ni prepared by the present invention3Se4Nanometer rods/nanometer sheet hierarchical array structural material be cut into 21 ×
1cm size, in a cell respectively as cathode and anode assembling, electrolyte solution 1.0MKOH, with the dry electricity of a section 1.5V
Pond drives its work, as a result as shown in figure 19.It can continue to generate bubble on two electrodes, it was demonstrated that Fe adulterates Ni3Se4Nanometer rods/
Nanometer sheet hierarchical array structural material can be used low-voltage and persistently drive total moisture solution.
It is above-mentioned that four three nanosized nickel rods of selenizing/nanometer sheet hierarchical array structural material, system are adulterated to a kind of Fe referring to embodiment
The detailed description that Preparation Method and its application carry out, is illustrative without being restrictive, can enumerate according to limited range
Several embodiments, therefore the change and modification in the case where not departing from present general inventive concept, should belong to protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of Fe adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material preparation method, which is characterized in that described
Preparation method the following steps are included:
(1) Se powder and reducing agent are dissolved in ammonium hydroxide and the mixed solution of deionized water, ultrasonic agitation obtains solution A, then
Solution A is transferred in reaction kettle, nickel foam inclination is placed in solution A, is sealed, heating reaction, to natural after reaction
It is cooled to room temperature, washs, dries, the nickel foam for having presoma is made；
(2) by iron salt dissolved in ethyl alcohol and the mixed solution of NaClO, solution B is obtained, solution B is then transferred to reaction kettle
In, step (1) prepare the nickel foam for having presoma be tiltedly placed in solution B, sealing, heating reaction, to after reaction from
It is so cooled to room temperature, washs, dries, Fe is made and adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material.
2. preparation method according to claim 1, which is characterized in that in step (1), the substance of the Se powder and reducing agent
The ratio between amount be 1:2.3-2.8.
3. preparation method according to claim 1, which is characterized in that the reducing agent is NaBH4；The molysite is Fe
(NO3)3·9H2O。
4. preparation method according to claim 1 to 3, which is characterized in that in step (1), the ammonium hydroxide and go
The volume ratio of ionized water is 5-15:35-25；Concentration of the selenium powder in solution A is 20-30mM.
5. preparation method according to claim 1 to 3, which is characterized in that in step (1), the heating reaction
Condition be 120 DEG C at react 8-12h.
6. preparation method according to claim 1 to 3, which is characterized in that in step (2), the molysite is molten
Concentration in liquid B is 20-30mM.
7. preparation method according to claim 1 to 3, which is characterized in that in step (2), the ethyl alcohol and
The ratio between volume of NaClO is 150~180:1.
8. preparation method according to claim 1, which is characterized in that in step (2), the condition of the heating reaction is
4-8h is reacted at 140 DEG C.
9. a kind of Fe that the preparation method as described in claim 1-8 any one is prepared adulterates Ni3Se4Nanometer rods/nanometer
Piece hierarchical array structural material.
10. Fe according to claim 9 adulterates Ni3Se4Nanometer rods/nanometer sheet hierarchical array structural material is anti-as analysis oxygen
The application for the elctro-catalyst for answering (OER) or evolving hydrogen reaction (HER) or total moisture solution to react.
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