CN110498451A - A kind of nickel doping Fe3O4The preparation and electrocatalytic decomposition water application of nano-powder - Google Patents
A kind of nickel doping Fe3O4The preparation and electrocatalytic decomposition water application of nano-powder Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 80
- 239000011858 nanopowder Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000354 decomposition reaction Methods 0.000 title claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 63
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 229910000863 Ferronickel Inorganic materials 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 18
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 4
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 4
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims description 3
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 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 2
- 229940078494 nickel acetate Drugs 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
- 238000011056 performance test Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000001257 hydrogen Substances 0.000 abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 11
- 238000012546 transfer Methods 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 238000001027 hydrothermal synthesis Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 238000002484 cyclic voltammetry Methods 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 230000005611 electricity Effects 0.000 description 8
- 238000005070 sampling Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 229920000557 Nafion® Polymers 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000001548 drop coating Methods 0.000 description 4
- 229910021397 glassy carbon Inorganic materials 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- YHGPYBQVSJBGHH-UHFFFAOYSA-H iron(3+);trisulfate;pentahydrate Chemical compound O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YHGPYBQVSJBGHH-UHFFFAOYSA-H 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910005093 Ni3C Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- FLESAADTDNKLFJ-UHFFFAOYSA-N nickel;pentane-2,4-dione Chemical compound [Ni].CC(=O)CC(C)=O FLESAADTDNKLFJ-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 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
-
- B01J35/23—
-
- B01J35/33—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention provides a kind of nickel to adulterate Fe3O4The preparation method and its electro-catalysis application of nano-powder.Firstly, the obtained ferronickel pre-reaction liquid of a certain proportion of nickel, source of iron is added in special reaction solution, pre-reaction liquid certain time is heated, collection obtains ferronickel predecessor nano-powder;Then, ferronickel predecessor nano-powder, which is placed in tube furnace, is made annealing treatment to obtain under nitrogen protection nickel doping Fe3O4Nano-powder.The introducing of active atomic nickel is benefited from, nickel adulterates Fe3O4Nano-powder shows excellent catalytic activity in decomposing aquatic products oxygen reaction (OER), and overpotential is down to 0.293 V(relative standard hydrogen electrode), Tafel slope is reduced to 43 mV/dec, and charge transfer resistance is reduced to 34 Ω.
Description
Technical field
The present invention relates to the preparation of inorganic nanometer powder and application fields, and in particular to one kind prepares nickel based on solvent-thermal method
Adulterate Fe3O4The method of nano-powder and its application in electro-catalysis water decomposition field.
Background technique
Fossil energy is as the current main energy, as its consumption sharply and incident environmental pollution are asked
Topic, the novel alternative energy source for seeking clean and effective have become the focus of current whole world research.Wherein, there is very high energies density
Hydrogen Energy attracted the sight of a large number of researchers.In all voluminous hydrogen approach, electrocatalytic decomposition aquatic products hydrogen can due to reaction safety
The advantages that control, product is Ke Xunhuanliyong, environment friendly and pollution-free makes it promise to be the important process of preparation Hydrogen Energy.However, due to
Four electronics course dynamics of its half-reaction (electro-catalysis production oxygen) complexity are slow, and the efficiency of electrocatalytic decomposition aquatic products hydrogen is right by its
Electrode produces the very big limitation of oxygen reaction.Therefore it explores and develops efficient electrocatalytic decomposition aquatic products VPO catalysts, for promoting to decompose
Aquatic products hydrogen is significant.So far, the catalyst of efficient oxygen evolution reaction remains as precious metal iridium, ruthenium and its compound, holds high
Expensive price and rare content, which limit, produces oxygen reaction further development.In order to solve this problem, design synthesis it is cheap,
It is easy to get, efficient oxygen-separating catalyst becomes the essential step for realizing energy revolution.
Up to the present, the electro-catalysis for being dedicated to being promoted non-noble metallic materials in spite of a large amount of research produces oxygen performance for cut-off
And many breakthrough progress are had been achieved for, but due to being related to four complicated electronic transfer process, produce oxygen reaction still face
The problem of Lingao overpotential, is difficult to solve.It is well known that nano material had been assigned compared with other block materials it is many special
Physics, chemical property, this feature makes nano material become the important research object in electro-catalysis field.With nanometer skill
The development of art and various control measures gradually mature, and transition metal oxide nano-material is due to its cheap, nontoxic, easy system
The advantages that standby, electronic structure is easily adjusted is hopeful to realize efficient electrocatalysis characteristic.However, transition metal oxide is inherently
Low electric conductivity significantly limits the improvement of its overpotential, therefore needs efficient control measures and optimize its electronic structure to adjust
Realize the promotion of catalytic performance.It is reported before us, the electronic structure of S doping meeting Effective Regulation cobalt oxide reduces band gap width
And active site is created to optimize overpotential and charge transfer resistance brings the promotion of catalytic performance.Fe3O4As transition
The disadvantages of one kind of metal oxide, itself poor active site and poor electric conductivity, becomes electro-catalysis and produces oxygen
Catalyst face significant challenge.There is a large amount of research to be dedicated to regulating and controlling Fe3O4Electronic structure to realize its catalysis live
The promotion of property, but it is limited by itself rare active site, the promotion of catalytic activity encounters bottleneck.In view of nickel-base material
Higher electro-catalysis produces oxygen performance, such as: Qingyu Yan seminar reports Ni3C nano point is grown on N doping carbon nanosheet
It can be used as efficient electro-catalysis and produce VPO catalysts.
In view of nickel and iron be all the 8th subgroup element period 4 and have similar valence electron structure (nickel:
3d84s2, iron: 3d64s2), indeed it is contemplated that nickle atom can be successfully introduced into Fe3O4In lattice, and its electronic structure is generated
The optimising and adjustment effect that can not ignore.Meanwhile the high catalytic activity of nickel-base material is benefited from, nickle atom can be used as active atomic
The activity of activation iron atom significantly promotes Fe to create more active sites3O4Catalytic activity.In consideration of it, we develop
The Fe of nickel doping3O4Catalyst is used to produce the effective catalyst of oxygen reaction, benefits from nickle atom to Fe3O4The tune of electronic structure
Control, a large amount of active site, the electric conductivity of promotion improve its activity significantly to realize that efficient electro-catalysis produces oxygen performance.
Specifically, charge transfer resistance is reduced to 34 Ω by 120 Ω after nickle atom introduces.Meanwhile nickel introduce after overpotential down to
0.293 V, Tafel slope shows nickel doping Fe down to 43 mV/dec3O4Excellent catalytic activity.In consideration of it, this nickel is mixed
Miscellaneous Fe3O4The successful synthesis of catalyst and its electrocatalysis characteristic application are cheap, efficient electrocatalytic decomposition water catalyst
Further development provides guiding theory.
Summary of the invention
Present invention solves the problem in that providing a kind of nickel doping Fe3O4The preparation method and its electrocatalysis of nano-powder
It can apply.In order to solve the above problem the technical solution of the present invention is as follows:
1. a kind of nickel adulterates Fe3O4The preparation method of nano-powder, preparation step are as follows: (1) adding in special reaction solution
Enter nickel, ferronickel pre-reaction liquid is made in source of iron, certain time is heated at a certain temperature after mixing evenly, with anhydrous after natural cooling
Ethanol washing is collected for several times obtains ferronickel predecessor nano-powder;(2) ferronickel predecessor nano-powder is placed in tube furnace, nitrogen
Annealing for a period of time, finally obtains nickel doping Fe at a certain temperature in gas atmosphere3O4Nano-powder.
2. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
Special reaction solution is ethylene glycol, isopropanol, combination one or more of in glycerine, and optimal is glycerine and isopropanol group
It closes, optimal volume ratio is glycerine: isopropanol=1: 7.
3. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
Source of iron is Iron(III) chloride hexahydrate, Fe(NO3)39H2O, ferric sulfate, ferrous acetate, and optimal is Iron(III) chloride hexahydrate and vinegar
The combination of one or more of sour ferrous iron, optimal is iron chloride and ferrous acetate.
4. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
The concentration of source of iron solution is the mol/L of 0.01 mol/L ~ 0.10, and optimal is the mol/L of 0.03 mol/L ~ 0.08.
5. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
Nickel source is Nickelous nitrate hexahydrate, Nickel dichloride hexahydrate, nickel acetate, nickel acetylacetonate, and optimal is Nickel dichloride hexahydrate and acetyl
Acetone nickel.
6. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
The concentration of nickel source solution is the mol/L of 0.01 mol/L ~ 0.03, and optimal is the mol/L of 0.01 mol/L ~ 0.02.
7. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, in the step (1),
The molar ratio of nickel source and source of iron is 1 ~ 2: 4 ~ 8, and optimal is 1: 6.
A kind of 8 nickel doping Fe according to claim 13O4The preparation method of nano-powder, in the step (1),
After mixing evenly by gained ferronickel pre-reaction liquid, reaction temperature 150oC ~ 200 oC, optimal is 190oC。
9. benefit require 1 described in a kind of nickel doping Fe3O4The preparation method of nano-powder, in the step (1), when reaction
Between be the h of 8 h ~ 20, optimal is 12 h.
10. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, the step (2)
In, annealing temperature 100oC ~ 400 oC, annealing time are the h of 1 h ~ 4;Optimal is 200oC ~ 300 oC, 2 h ~ 3
h。
11. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, the step (2)
In, heating rate is 1 when annealingoC/min, nitrogen flow rate are the mL/min of 10 mL/min ~ 30.
12. a kind of nickel adulterates Fe3O4The simple preparation and electro-catalysis application of nano-powder, are surveyed using three-electrode system
Examination carries out the oxygen performance test of electrocatalytic decomposition aquatic products on electrochemical workstation, to be coated with nickel doping Fe3O4The glass of nano-powder
Carbon electrode is working electrode, is to electrode, using Ag/AgCl electrode as reference electrode with carbon-point;It is molten with 1 mol/L potassium hydroxide
Liquid is electrolyte;Using H-type electrolytic cell as electrolysis reaction device.
Specific embodiment mode
In order to further appreciate that the present invention, the preferred embodiment of the invention is described below with reference to embodiment, these descriptions
It is only further explanation the features and advantages of the present invention, rather than limiting to the claimed invention.
Embodiment 1
Step 1: taking 50 mL hydrothermal reaction kettles, hydrothermal reaction kettle has stainless steel casing, polytetrafluoroethylliner liner.Take 40 mL
Ethylene glycol is added in 50 mL beakers, and Fe(NO3)39H2O (0.3232 g, 0.8 mmol), vinegar are sequentially added under magnetic agitation
Magneton suction is transferred in polytetrafluoroethylliner liner by sour nickel (0.0707 g, 0.4 mmol) after stirring 10 min.Seal hydro-thermal
150 °C of 18 h of baking oven inside holding is placed it in after reaction kettle.After natural cooling, with dehydrated alcohol wash for several times, vacuum drying
After obtain light blue ferronickel predecessor nano-powder.
Step 2: ferronickel predecessor nano-powder is placed in tube furnace, made annealing treatment under nitrogen atmosphere.Annealing temperature
Degree is 100oC, the time is 4 h;Nitrogen flow rate is 10 mL/min, heating rate 1oC/min is obtained black after being cooled to room temperature
Color nickel adulterates Fe3O4Nano-powder.
Step 3: nickel adulterates Fe3O4Nano-powder electrolysis water application
1. weighing 5 mg nickel doping Fe3O4Nano-powder, be added to 1 mL ethyl alcohol and water in the mixed solvent (ethyl alcohol and water
Volume ratio is 3: 7), while 50 μ L Nafion solutions is added, 1 h of ultrasound obtains black even dispersion liquid.Take 4 μ L above-mentioned
Dispersion liquid, drop coating is in glassy carbon electrode surface, and wherein glass-carbon electrode diameter is 3 mm, naturally dry.
2. using three-electrode system, electrocatalytic decomposition aquatic products oxygen performance is carried out on occasion China 660E electrochemical workstation and is surveyed
Examination.To be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is to electrode with carbon-point, Ag/AgCl electrode is
Reference electrode.Using 1 mol/L potassium hydroxide solution as electrolyte, using H-type glass electrolytic cell as reaction unit.
3. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is followed in three-electrode system
The test of ring volt-ampere, activates sample.Cyclic voltammetry voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode), highest electricity
0.8 V of position, 0 V of potential minimum, beginning current potential are 0 V, and termination current potential is 0.8 V.Sweep speed is 0.05 V/s.Sampling interval
For 0.001 V, time of repose is 2 s, and scanning number of segment is 500.
4. after cyclic voltammetry, to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, three
Linear voltage sweep test is carried out in electrode system, voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode).Initial potential
For 0 V, termination current potential is 0.8 V.Sweep speed is 5 mV/s.Sampling interval is 0.001 V.Time of repose is 2 s.
5. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, carries out AC impedance to catalyst
Test, to carry out kinetic Process Analysis.Parameter setting is as follows, and initial potential is 0.6 V(with respect to Ag/AgCl electrode), high frequency
For 100000 Hz, low frequency 0.1Hz.Amplitude is 0.005 V, and quiescent time is 2 s.After data processing and calculating, nickel doping
Fe3O4For application of nanopowder to OER excellent effect, being catalyzed water electrolysis and producing the overpotential of oxygen is 0.295 V(relative standard hydrogen electricity
Pole), Tafel slope is 45 mV/dec, and charge transfer resistance is 35 Ω.
Embodiment 2
Step 1: taking 50 mL hydrothermal reaction kettles, hydrothermal reaction kettle has stainless steel casing, polytetrafluoroethylliner liner.Take 5 mL third
Triol, 35 mL isopropanols are added in 50 mL beakers, sequentially added under magnetic agitation ferric chloride hexahydrate (0.6487 g, 2.4
Mmol), magneton suction is transferred to polytetrafluoroethylene (PTFE) after Nickel dichloride hexahydrate (0.0951 g, 0.4 mmol), 10 min of stirring
In liner.190 °C of 12 h of baking oven inside holding is placed it in after sealing hydrothermal reaction kettle.After natural cooling, washed with dehydrated alcohol
Wash for several times, vacuum drying after obtain light blue ferronickel predecessor nano-powder.
Step 2: ferronickel predecessor nano-powder is placed in tube furnace, made annealing treatment under nitrogen atmosphere.Annealing temperature
Degree is 300oC, the time is 2 h;Nitrogen flow rate is 20 mL/min, heating rate 1oC/min is obtained black after being cooled to room temperature
Color nickel adulterates Fe3O4Nano-powder.
Step 3: nickel adulterates Fe3O4Nano-powder electrolysis water application
1. weighing 5 mg nickel doping Fe3O4Nano-powder, be added to 1 mL ethyl alcohol and water in the mixed solvent (ethyl alcohol and water
Volume ratio is 3: 7), while 50 μ L Nafion solutions is added, 1 h of ultrasound obtains black even dispersion liquid.Take 4 μ L above-mentioned
Dispersion liquid, drop coating is in glassy carbon electrode surface, and wherein glass-carbon electrode diameter is 3 mm, naturally dry.
2. using three-electrode system, electrocatalytic decomposition aquatic products oxygen performance is carried out on occasion China 660E electrochemical workstation and is surveyed
Examination.To be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is to electrode with carbon-point, Ag/AgCl electrode is
Reference electrode.Using 1 mol/L potassium hydroxide solution as electrolyte, using H-type glass electrolytic cell as reaction unit.
3. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is followed in three-electrode system
The test of ring volt-ampere, activates sample.Cyclic voltammetry voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode), highest electricity
0.8 V of position, 0 V of potential minimum, beginning current potential are 0 V, and termination current potential is 0.8 V.Sweep speed is 0.05 V/s.Sampling interval
For 0.001 V, time of repose is 2 s, and scanning number of segment is 500.
4. after cyclic voltammetry, to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, three
Linear voltage sweep test is carried out in electrode system, voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode).Initial potential
For 0 V, termination current potential is 0.8 V.Sweep speed is 5 mV/s.Sampling interval is 0.001 V.Time of repose is 2 s.
5. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, carries out AC impedance to catalyst
Test, to carry out kinetic Process Analysis.Parameter setting is as follows, and initial potential is 0.6 V(with respect to Ag/AgCl electrode), high frequency
For 100000 Hz, low frequency 0.1Hz.Amplitude is 0.005 V, and quiescent time is 2 s.After data processing and calculating, nickel doping
Fe3O4For application of nanopowder to OER excellent effect, being catalyzed water electrolysis and producing the overpotential of oxygen is 0.293 V(relative standard hydrogen electricity
Pole), Tafel slope is 43 mV/dec, and charge transfer resistance is 34 Ω.
Embodiment 3
Step 1: taking 50 mL hydrothermal reaction kettles, hydrothermal reaction kettle has stainless steel casing, polytetrafluoroethylliner liner.Take 5 mL third
Triol, 35 mL isopropanols are added in 50 mL beakers, sequentially added under magnetic agitation ferrous acetate (0.5566 g, 3.2
Mmol), magneton suction is transferred in polytetrafluoroethylene (PTFE) by nickel acetylacetonate (0.1028 g, 0.4 mmol) after stirring 10 min
In gallbladder.190 °C of 12 h of baking oven inside holding is placed it in after sealing hydrothermal reaction kettle.After natural cooling, washed with dehydrated alcohol
For several times, light blue ferronickel predecessor nano-powder is obtained after being dried in vacuo.
Step 2: ferronickel predecessor nano-powder is placed in tube furnace, made annealing treatment under nitrogen atmosphere.Annealing temperature
Degree is 200oC, the time is 3 h;Nitrogen flow rate is 20 mL/min, heating rate 1oC/min is obtained black after being cooled to room temperature
Color nickel adulterates Fe3O4Nano-powder.
Step 3: nickel adulterates Fe3O4Nano-powder electrolysis water application
1. weighing 5 mg nickel doping Fe3O4Nano-powder, be added to 1 mL ethyl alcohol and water in the mixed solvent (ethyl alcohol and water
Volume ratio is 3: 7), while 50 μ L Nafion solutions is added, 1 h of ultrasound obtains black even dispersion liquid.Take 4 μ L above-mentioned
Dispersion liquid, drop coating is in glassy carbon electrode surface, and wherein glass-carbon electrode diameter is 3 mm, naturally dry.
2. using three-electrode system, electrocatalytic decomposition aquatic products oxygen performance is carried out on occasion China 660E electrochemical workstation and is surveyed
Examination.To be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is to electrode with carbon-point, Ag/AgCl electrode is
Reference electrode.Using 1 mol/L potassium hydroxide solution as electrolyte, using H-type glass electrolytic cell as reaction unit.
3. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is followed in three-electrode system
The test of ring volt-ampere, activates sample.Cyclic voltammetry voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode), highest electricity
0.8 V of position, 0 V of potential minimum, beginning current potential are 0 V, and termination current potential is 0.8 V.Sweep speed is 0.05 V/s.Sampling interval
For 0.001 V, time of repose is 2 s, and scanning number of segment is 500.
4. after cyclic voltammetry, to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, three
Linear voltage sweep test is carried out in electrode system, voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode).Initial potential
For 0 V, termination current potential is 0.8 V.Sweep speed is 5 mV/s.Sampling interval is 0.001 V.Time of repose is 2 s.
5. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, carries out AC impedance to catalyst
Test, to carry out kinetic Process Analysis.Parameter setting is as follows, and initial potential is 0.6 V(with respect to Ag/AgCl electrode), high frequency
For 100000 Hz, low frequency 0.1Hz.Amplitude is 0.005 V, and quiescent time is 2 s.After data processing and calculating, nickel doping
Fe3O4For application of nanopowder to OER excellent effect, being catalyzed water electrolysis and producing the overpotential of oxygen is 0.293 V(relative standard hydrogen electricity
Pole), Tafel slope is 45 mV/dec, and charge transfer resistance is 34 Ω.
Embodiment 4
Step 1: taking 50 mL hydrothermal reaction kettles, hydrothermal reaction kettle has stainless steel casing, polytetrafluoroethylliner liner.Take 40 mL
Isopropanol is added in 50 mL beakers, and ferric sulfate (1.5994 g, 4 mmol), six nitric hydrates are sequentially added under magnetic agitation
Magneton suction is transferred in polytetrafluoroethylliner liner by nickel (0.1454 g, 0.5 mmol) after stirring 10 min.It is anti-to seal hydro-thermal
It answers and places it in 200 °C of 8 h of baking oven inside holding after kettle.After natural cooling, washed for several times, after vacuum drying with dehydrated alcohol
Obtain light blue ferronickel predecessor nano-powder.
Step 2: ferronickel predecessor nano-powder is placed in tube furnace, made annealing treatment under nitrogen atmosphere.Annealing temperature
Degree is 400oC, the time is 1 h;Nitrogen flow rate is 30 mL/min, heating rate 1oC/min is obtained black after being cooled to room temperature
Color nickel adulterates Fe3O4Nano-powder.
Step 3: nickel adulterates Fe3O4Nano-powder electrolysis water application
1. weighing 5 mg nickel doping Fe3O4Nano-powder, be added to 1 mL ethyl alcohol and water in the mixed solvent (ethyl alcohol and water
Volume ratio is 3: 7), while 50 μ L Nafion solutions is added, 1 h of ultrasound obtains black even dispersion liquid.Take 4 μ L above-mentioned
Dispersion liquid, drop coating is in glassy carbon electrode surface, and wherein glass-carbon electrode diameter is 3 mm, naturally dry.
2. using three-electrode system, electrocatalytic decomposition aquatic products oxygen performance is carried out on occasion China 660E electrochemical workstation and is surveyed
Examination.To be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is to electrode with carbon-point, Ag/AgCl electrode is
Reference electrode.Using 1 mol/L potassium hydroxide solution as electrolyte, using H-type glass electrolytic cell as reaction unit.
3. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, is followed in three-electrode system
The test of ring volt-ampere, activates sample.Cyclic voltammetry voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode), highest electricity
0.8 V of position, 0 V of potential minimum, beginning current potential are 0 V, and termination current potential is 0.8 V.Sweep speed is 0.05 V/s.Sampling interval
For 0.001 V, time of repose is 2 s, and scanning number of segment is 500.
4. after cyclic voltammetry, to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, three
Linear voltage sweep test is carried out in electrode system, voltage range is 0 ~ 0.8 V(with respect to Ag/AgCl electrode).Initial potential
For 0 V, termination current potential is 0.8 V.Sweep speed is 5 mV/s.Sampling interval is 0.001 V.Time of repose is 2 s.
5. to be coated with nickel doping Fe3O4The glass-carbon electrode of nano-powder is working electrode, carries out AC impedance to catalyst
Test, to carry out kinetic Process Analysis.Parameter setting is as follows, and initial potential is 0.6 V(with respect to Ag/AgCl electrode), high frequency
For 100000 Hz, low frequency 0.1Hz.Amplitude is 0.005 V, and quiescent time is 2 s.After data processing and calculating, nickel doping
Fe3O4For application of nanopowder to OER excellent effect, being catalyzed water electrolysis and producing the overpotential of oxygen is 0.294 V(relative standard hydrogen electricity
Pole), Tafel slope is 46 mV/dec, and charge transfer resistance is 34 Ω.
Claims (7)
1. a kind of nickel adulterates Fe3O4The preparation method of nano-powder, which is characterized in that preparation step is as follows: (1) special anti-
It answers and the obtained ferronickel pre-reaction liquid of nickel, source of iron is added in solvent, after mixing evenly heating pre-reaction liquid certain time, after natural cooling
Washing collects and obtains ferronickel predecessor nano-powder;(2) ferronickel predecessor nano-powder is placed in tube furnace, in nitrogen atmosphere
Annealing a period of time at a certain temperature finally obtains nickel doping Fe3O4Nano-powder.
2. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, which is characterized in that the step
(1) in, special reaction dissolvent is the combination of one or more of ethylene glycol, isopropanol, glycerine.
3. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, which is characterized in that the step
(1) in, source of iron is Iron(III) chloride hexahydrate, Fe(NO3)39H2O, ferric sulfate, acetic acid weight, and the concentration of source of iron solution is 0.01
mol/L ~ 0.1 mol/L。
4. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, which is characterized in that the step
(1) in, nickel source is Nickelous nitrate hexahydrate, Nickel dichloride hexahydrate, nickel acetate, nickel acetylacetonate, and the concentration of nickel source solution is 0.01
mol/L ~ 0.03 mol/L;Wherein, the molar ratio of nickel source and source of iron is 1 ~ 2: 4 ~ 8.
5. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, which is characterized in that the step
(1) in, after mixing evenly by gained ferronickel pre-reaction liquid, 150 are placed inoC ~ 200 oIn the baking oven of C, 8 h of heating reaction ~
20 h。
6. a kind of nickel according to claim 1 adulterates Fe3O4The preparation method of nano-powder, which is characterized in that the step
(2) in, annealing temperature 100oC ~ 400 oC, annealing time are the h of 1 h ~ 4, heating rate 1oC/min, nitrogen stream
Speed is the mL/min of 10 mL/min ~ 30,.
7. a kind of nickel adulterates Fe3O4The simple preparation and electro-catalysis application of nano-powder, which is characterized in that use three-electrode system
It is tested, the oxygen performance test of electrocatalytic decomposition aquatic products is carried out on electrochemical workstation, to be coated with nickel doping Fe3O4Nano powder
The glass-carbon electrode of body is working electrode, is to electrode, using Ag/AgCl electrode as reference electrode with carbon-point;With 1 mol/L hydrogen-oxygen
Change potassium solution is electrolyte;Using H-type electrolytic cell as electrolysis reaction device.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113102693A (en) * | 2021-05-06 | 2021-07-13 | 四川固锐德科技有限公司 | Preparation method of planetary wheel set for wheel edge system of heavy-duty vehicle |
CN113604829A (en) * | 2021-07-22 | 2021-11-05 | 西安交通大学 | Alkaline electrolytic water oxygen evolution catalytic electrode, preparation method and application thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5460704A (en) * | 1994-09-28 | 1995-10-24 | Motorola, Inc. | Method of depositing ferrite film |
CN1454851A (en) * | 2002-04-17 | 2003-11-12 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
CN106848256A (en) * | 2017-03-24 | 2017-06-13 | 中南大学 | A kind of nickel iron cell core duplex shell structure negative pole nano material and its preparation method and application |
CN108400296A (en) * | 2018-02-05 | 2018-08-14 | 北京理工大学 | Heterogeneous element doped ferroferric oxide/graphene negative material |
CN109046360A (en) * | 2018-06-11 | 2018-12-21 | 扬州大学 | A kind of Fe that catalytic activity improves3O4Nano enzyme and its preparation method and application |
-
2019
- 2019-08-30 CN CN201910812075.2A patent/CN110498451A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5460704A (en) * | 1994-09-28 | 1995-10-24 | Motorola, Inc. | Method of depositing ferrite film |
CN1454851A (en) * | 2002-04-17 | 2003-11-12 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
CN106848256A (en) * | 2017-03-24 | 2017-06-13 | 中南大学 | A kind of nickel iron cell core duplex shell structure negative pole nano material and its preparation method and application |
CN108400296A (en) * | 2018-02-05 | 2018-08-14 | 北京理工大学 | Heterogeneous element doped ferroferric oxide/graphene negative material |
CN109046360A (en) * | 2018-06-11 | 2018-12-21 | 扬州大学 | A kind of Fe that catalytic activity improves3O4Nano enzyme and its preparation method and application |
Non-Patent Citations (1)
Title |
---|
卢帮安: "纳米过渡金属氧化物作为析氧电极的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113102693A (en) * | 2021-05-06 | 2021-07-13 | 四川固锐德科技有限公司 | Preparation method of planetary wheel set for wheel edge system of heavy-duty vehicle |
CN113604829A (en) * | 2021-07-22 | 2021-11-05 | 西安交通大学 | Alkaline electrolytic water oxygen evolution catalytic electrode, preparation method and application thereof |
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