CN109225301A - A kind of Ir/Co0.8Fe0.2Se2Monatomic catalyst of-NF and preparation method thereof, application - Google Patents
A kind of Ir/Co0.8Fe0.2Se2Monatomic catalyst of-NF and preparation method thereof, application Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910002505 Co0.8Fe0.2 Inorganic materials 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical group [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 29
- 238000004070 electrodeposition Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 15
- 239000002135 nanosheet Substances 0.000 claims abstract description 7
- 150000002503 iridium Chemical class 0.000 claims abstract description 5
- 239000011669 selenium Substances 0.000 claims description 112
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 239000006260 foam Substances 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052759 nickel Inorganic materials 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- CALMYRPSSNRCFD-UHFFFAOYSA-J tetrachloroiridium Chemical group Cl[Ir](Cl)(Cl)Cl CALMYRPSSNRCFD-UHFFFAOYSA-J 0.000 claims description 12
- 230000002441 reversible effect Effects 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 239000002060 nanoflake Substances 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000002798 polar solvent Substances 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 7
- 238000000151 deposition Methods 0.000 description 21
- 230000008021 deposition Effects 0.000 description 21
- 239000007864 aqueous solution Substances 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 4
- 230000010287 polarization Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- -1 platinum carbon-iridium dioxide Chemical compound 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000007172 homogeneous catalysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001052 transient effect 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention proposes a kind of Ir/Co0.8Fe0.2Se2Monatomic catalyst of-NF and preparation method thereof, application, the catalyst is equably to be supported on Co by monodisperse Ir atom0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted.Preparation method includes: electrochemical deposition to be carried out using three-electrode system, in the electrolyte solution comprising iridium salt with Co0.8Fe0.2Se2- NF two-dimensional nano thin slice carries out linear voltammetric scan as working electrode, makes iridium atom monodisperse, equably deposits to Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, the Ir/Co is obtained0.8Fe0.2Se2The monatomic catalyst of-NF.The Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF has high activity and high stability in the reaction of electrocatalytic decomposition water.
Description
Technical field
The present invention relates to catalyst technical field more particularly to a kind of Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF and
Preparation method, application.
Background technique
Electrocatalytic decomposition water is a kind of extremely important chemical reaction, and reacting obtained hydrogen can be used as high-efficiency cleaning energy
Source, the problems such as alleviating current energy shortage, environmental pollution.Traditional electrocatalytic decomposition water reaction is mainly catalyzed with platinum based catalyst
Cathode hydrogen evolution reaction, with iridium, ruthenium-based catalyst catalyticing anode oxygen evolution reaction, although there is preferable activity, platinum, iridium, ruthenium
Equal noble metals reserves are rare, with high costs, non-renewable, it is difficult to carry out large-scale industry application.By people research and
Exploitation, a series of low in cost, performances such as transient metal sulfide, selenides, phosphide and its oxide, hydroxide
Stable non-precious metal catalyst also occurs in succession, but its activity differs farther out with noble metal catalyst, and needs higher
Load capacity.Therefore, from the angle for reducing noble metal catalyst load capacity, the utilization rate of precious metal atom is improved, is developed low
Load, high activity, high stability electrocatalytic decomposition water catalyst be particularly important.
And emerging monatomic catalyst, it is that single metal atom is deposited on independently of each other on substrate material, is to connect
The bridge of homogeneous catalysis and heterocatalysis is connect, there is high atom utilization, metal active centres coordination unsaturation, cooperateed with substrate
A series of features such as effect, monatomic catalyst is in series reaction, such as electrolysis water, hydrogen reduction, carbon dioxide electroreduction are instead
Brilliant activity and stability are shown in answering.By designing your gold monatomic electrocatalytic decomposition water catalyst can be effectively reduced
The load capacity of category obtains efficient, stable catalyst.However, the generally existing load of the method for synthesizing monatomic catalyst at present
The problems such as too low, stability is poor, complex procedures, synthesis poor controllability is measured, convenient, effective monatomic catalyst synthesis side is researched and developed
Method is of great significance.
Specific atoms are deposited to substrate surface and obtain required structure by electro-deposition techniques using electric power as driving force, are a kind of
Traditional but simple and effective, the small, component of pollution and the adjustable synthetic technology of flexible structure.Electro-deposition is mostly used to prepare film, super brilliant
The structures such as lattice, nano particle, nanocluster, these be all by adjusting raw material species concentration, sedimentation potential and sedimentation time, from
And it controls crystal nucleation, growth course to realize, therefore theoretically in the item that raw material species concentration is extremely low, sedimentation time is shorter
Under part, the continuously adjustable of nanocrystalline size may be implemented, this will provide important thinking for the preparation of monatomic structure.
Summary of the invention
Technical problems based on background technology, the present invention propose a kind of Ir/Co0.8Fe0.2Se2The monatomic catalysis of-NF
Agent and preparation method thereof, application, the Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF is based on electro-deposition and constructs monatomic knot
Structure, by the way that electro-deposition method can quickly, efficiently, controllably deposition Ir be monatomic, the Ir/Co of acquisition0.8Fe0.2Se2- NF is monatomic
Catalyst is reacted due to the synergistic effect with monoatomic high atom utilization and between substrate in electrocatalytic decomposition water
In have high activity and high stability, while its low Ir atom load capacity make catalyst keep it is high performance under the premise of it is right
The consumption of noble metal substantially reduces, to play its potential advantages promoted and applied on a large scale in the reaction of electrocatalytic decomposition water.
A kind of Ir/Co proposed by the present invention0.8Fe0.2Se2The monatomic catalyst of-NF, the catalyst are by monodisperse Ir
Atom is equably supported on Co0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted, Co0.8Fe0.2Se2- NF two-dimensional nano thin slice
It is Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam.
Preferably, Ir atom and Co0.8Fe0.2Se2The mass ratio of-NF two-dimensional nano thin slice is 2-4:95-105.
A kind of Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, comprising: molten in the electrolyte comprising iridium salt
In liquid, electrochemical deposition is carried out using three-electrode system, with Co0.8Fe0.2Se2- NF two-dimensional nano thin slice as working electrode, into
Line voltammetric scan makes iridium atom monodisperse, equably deposits to Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, institute is obtained
State Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF.
Preferably, the iridium salt be iridic chloride, and in the electrolyte solution also include potassium hydroxide, potassium hydroxide and
The mass volume ratio of deionized water is 56-57mg:0.8-1.2mL, and the mass ratio of potassium hydroxide and iridic chloride is 56-57:
0.03-0.04。
Preferably, the Co is prepared0.8Fe0.2Se2The method of-NF two-dimensional nano thin slice includes: under room temperature by sheet-formed foam
Nickel and molal volume ratio are 3-4mmol:0.15-0.2mmol:9.5-10.5mmol:11-12mmol:15-25mL:150- 200mL
Cobalt chloride, iron chloride, sodium chloride, hexa, ethyl alcohol, deionized water mixing, after mixing evenly at 80-100 DEG C
Hydrolysis 1.5-3h is cooled to room temperature, filters, and washs, dry, obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；
By the Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and molal volume ratio are 3-4mmol:7-8mmol:0.1-0.2mL:20-
The selenium powder of 30mL, sodium hydroxide, hydrazine hydrate, n,N-Dimethylformamide mixing, hydro-thermal is anti-at 160-200 DEG C after mixing evenly
1-2h is answered, room temperature is cooled to, is filtered, is washed, it is dry, obtain Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；Preferably, sheet
The size specification of nickel foam is 0.8-1.2cm*2.6-3.5cm.
Preferably, the electrochemical deposition is cathodic electrochemical deposition, the scanning current potential of cathodic electrochemical deposition relative to
Reversible hydrogen electrode is -0.3-0.1V, and scanning speed 4.8-5.2mV/s, scanning times are 8-12 times.
Preferably, the electrochemical deposition be anode electrochemical deposition, anode electrochemical deposition scanning current potential relative to
Reversible hydrogen electrode is 1.3-1.8V, and scanning speed 4.8-5.2mV/s, scanning times are 8-12 times.
Preferably, when carrying out electrochemical deposition, electrolyte solution is stirred by the way of magnetic agitation, stirring rate is
1300-1500r/min。
Preferably, the preparation method further include: after the completion of linear voltammetric scan, take out working electrode, use polar solvent
It rinses, repeats above-mentioned flushing process 4-6 times；Preferably, washing time 1-2min, it is highly preferred that polar solvent is deionization
Water.
The present invention also proposes above-mentioned Ir/Co0.8Fe0.2Se2Application of the monatomic catalyst of-NF in the reaction of complete solution water.
Compared with prior art, the present invention has the advantage that
Ir/Co of the present invention0.8Fe0.2Se2The monatomic catalyst of-NF is to load the monatomic uniform, monodisperse of Ir
To Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, the Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is substantially to be grown in nickel foam
On two-dimensional selenizing ferro-cobalt thin slice composition, finally construct a kind of Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF.The Ir/
Co0.8Fe0.2Se2The monatomic catalyst of-NF both reduces noble metal dosage, and out-phase structure is conducive to the recycling of catalyst, reduces
Catalyst cost；Again there is high atom utilization and substrate to act synergistically based on monatomic polymolecularity on substrate,
Make gained Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF has very high catalytic activity and catalysis steady in electrocatalytic decomposition water
It is qualitative.At the same time, as a kind of novel, simple, effective monatomic method for preparing catalyst, this will be electrocatalytic decomposition water
The industrialization of reaction provides huge power-assisted.
Detailed description of the invention
Fig. 1 is gained Co in the embodiment of the present invention 10.8Fe0.2Se2The transmission electron microscope picture of-NF two-dimensional nano thin slice；
Fig. 2 is gained Co in the embodiment of the present invention 10.8Fe0.2Se2The X-ray electron diffraction diagram of-NF two-dimensional nano thin slice
Picture；
Fig. 3 is cathode deposition gained Ir/Co in the embodiment of the present invention 10.8Fe0.2Se2The scanning of the monatomic catalyst of-NF is saturating
Penetrate electron microscope angle of elevation annular dark；
Fig. 4 is that 1 Anodic of the embodiment of the present invention deposits gained Ir/Co0.8Fe0.2Se2The scanning of the monatomic catalyst of-NF is saturating
Penetrate electron microscope angle of elevation annular dark；
Fig. 5 is 1 gained Ir/Co of the embodiment of the present invention0.8Fe0.2Se2The monatomic catalyst electrocatalytic decomposition water reaction of-NF
Polarization curve and its and Co0.8Fe0.2Se2The comparison of-NF nanocatalyst and commercial platinum carbon-iridium dioxide combination catalyst；
Fig. 6 is 1 gained Ir/Co of the embodiment of the present invention0.8Fe0.2Se2The monatomic catalyst electrocatalytic decomposition water reaction of-NF
Constant current mode stability curve.
Specific embodiment
Embodiment 1
A kind of Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, the Ir/Co0.8Fe0.2Se2- NF is single former
Muonic catalysis agent is equably to be supported on Co by monodisperse iridium atom0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted,
Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam, preparation
Method includes:
(1) Co is prepared0.8Fe0.2Se2- NF two-dimensional nano thin slice:
Under room temperature by the nickel foam of 1cm*3cm and 3.3mmol cobalt chloride, 0.2mmol iron chloride, 10mmol sodium chloride,
12mmol hexa, 20mL ethyl alcohol, the mixing of 180mL deionized water, after mixing evenly, the hydrolysis 2h at 90 DEG C,
It is cooled to room temperature, is filtered, ethanol washing, drying at room temperature obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；It will be described
Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and 3.7mmol selenium powder, 7.5mmol sodium hydroxide, 0.14mL hydrazine hydrate, 25mL
N,N-Dimethylformamide mixing, after mixing evenly, the hydro-thermal reaction 1h at 180 DEG C is cooled to room temperature, and filtering, ethyl alcohol is washed
It washs, drying at room temperature obtains Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；
(2) Ir/Co is prepared0.8Fe0.2Se2The monatomic catalyst of-NF:
By above-mentioned Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is used as working electrode, graphite rod conduct in three-electrode system
To electrode, silver/silver chloride electrode is as reference electrode；100 are added into the potassium hydroxide aqueous solution that 100mL concentration is 1mol/L
It is stirred evenly in the iridic chloride aqueous solution that μ L concentration is 0.1mol/L, obtains the electrolyte solution comprising iridic chloride, and iridium
Concentration be 0.1mmol/L, using Shanghai Chen Hua company CHI 660E electrochemical workstation, in the scanning speed of 5mV/s, and yin
Pole deposition scanning current potential (relative to reversible hydrogen electrode) is -0.3-0.1V or anodic deposition scans current potential (relative to reversible hydrogen
Electrode) to carry out linear voltammetric scan respectively 10 times under conditions of 1.3-1.8V, in scanning process, by the way of magnetic agitation
Electrolyte solution is stirred, stirring rate 1400r/min makes iridium atom monodisperse, is uniformly deposited on Co0.8Fe0.2Se2-NF
On two-dimensional nano thin slice, working electrode is further taken out, rinses 1.5min with deionized water, is repeated above-mentioned flushing process 5 times, it is dry,
Respectively obtain the Co that cathode deposition gained area load has iridium0.8Fe0.2Se2Table obtained by-NF two-dimensional nano thin slice and anodic deposition
Face loads the Co for having iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice, i.e. Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF, and the list
The monatomic middle metallic atom mass fraction of iridium is all 4.00% in catalyst atom.
Embodiment 2
A kind of Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, the Ir/Co0.8Fe0.2Se2- NF is single former
Muonic catalysis agent is equably to be supported on Co by monodisperse iridium atom0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted,
Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam, preparation
Method includes:
(1) Co is prepared0.8Fe0.2Se2- NF two-dimensional nano thin slice:
By the nickel foam of 0.8cm*3.5cm and 3mmol cobalt chloride, 0.25mmol iron chloride, 9.5mmol chlorination under room temperature
Sodium, 12.5mmol hexa, 15mL ethyl alcohol, the mixing of 200mL deionized water hydrolyze anti-at 80 DEG C after mixing evenly
3h is answered, room temperature is cooled to, is filtered, ethanol washing, drying at room temperature obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；It will
The Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and 3mmol selenium powder, 8mmol sodium hydroxide, 0.1mL hydrazine hydrate, 30mL N,
Dinethylformamide mixing, after mixing evenly, the hydro-thermal reaction 2h at 160 DEG C is cooled to room temperature, filtering, ethanol washing,
Drying at room temperature obtains Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；
(2) Ir/Co is prepared0.8Fe0.2Se2The monatomic catalyst of-NF:
By above-mentioned Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is used as working electrode, graphite rod conduct in three-electrode system
To electrode, silver/silver chloride electrode is as reference electrode；It is added into the potassium hydroxide aqueous solution that 100mL concentration is 0.83mol/L
It is stirred evenly in the iridic chloride aqueous solution that 75 μ L concentration are 0.1mol/L, obtains the electrolyte solution comprising iridic chloride, and
The concentration of iridium is 0.075mmol/L, using Shanghai Chen Hua company CHI 660E electrochemical workstation, in the scanning speed of 4.8mV/s
Degree, and cathode deposition scanning current potential (relative to reversible hydrogen electrode) be -0.3-0.1V or anodic deposition scan current potential (relative to
Reversible hydrogen electrode) to carry out linear voltammetric scan respectively 10 times under conditions of 1.3-1.8V, in scanning process, using magnetic agitation
Mode stir electrolyte solution, stirring rate 1500r/min makes iridium atom monodisperse, is uniformly deposited on
Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, working electrode is further taken out, 1min is rinsed with deionized water, repeats above-mentioned flushed
It is journey 6 times, dry, respectively obtain the Co that cathode deposition gained area load has iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice and anode
Deposition gained area load has the Co of iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice, i.e. Ir/Co0.8Fe0.2Se2The monatomic catalysis of-NF
Agent, and the monatomic middle metallic atom mass fraction of iridium is all 1.86% in the monatomic catalyst.
Embodiment 3
A kind of Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, the Ir/Co0.8Fe0.2Se2- NF is single former
Muonic catalysis agent is equably to be supported on Co by monodisperse iridium atom0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted,
Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam, preparation
Method includes:
(1) Co is prepared0.8Fe0.2Se2- NF two-dimensional nano thin slice:
By the nickel foam of 1.2cm*2.6cm and 4mmol cobalt chloride, 0.15mmol iron chloride, 10.5mmol chlorination under room temperature
Sodium, 11.5mmol hexa, 25mL ethyl alcohol, the mixing of 150mL deionized water hydrolyze anti-at 100 DEG C after mixing evenly
1.5h is answered, room temperature is cooled to, is filtered, ethanol washing, drying at room temperature obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；
By the Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and 4mmol selenium powder, 7mmol sodium hydroxide, 0.2mL hydrazine hydrate, 30mL
N,N-Dimethylformamide mixing, after mixing evenly, the hydro-thermal reaction 1h at 200 DEG C is cooled to room temperature, and filtering, ethyl alcohol is washed
It washs, drying at room temperature obtains Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；
(2) Ir/Co is prepared0.8Fe0.2Se2The monatomic catalyst of-NF:
By above-mentioned Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is used as working electrode, platinum electrode conduct in three-electrode system
To electrode, saturated calomel electrode is as reference electrode；It is added into the potassium hydroxide aqueous solution that 100mL concentration is 1.27mol/L
It is stirred evenly in the iridic chloride aqueous solution that 150 μ L concentration are 0.1mol/L, obtains the electrolyte solution comprising iridic chloride, and
The concentration of iridium is 0.15mmol/L, using Shanghai Chen Hua company CHI 660E electrochemical workstation, in the scanning speed of 5.2mV/s
Degree, and cathode deposition scanning current potential (relative to reversible hydrogen electrode) be -0.3-0.1V or anodic deposition scan current potential (relative to
Reversible hydrogen electrode) to carry out linear voltammetric scan respectively 10 times under conditions of 1.3-1.8V, in scanning process, using magnetic agitation
Mode stir electrolyte solution, stirring rate 1300r/min makes iridium atom monodisperse, is uniformly deposited on
Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, working electrode is further taken out, 2min is rinsed with deionized water, repeats above-mentioned flushed
It is journey 4 times, dry, respectively obtain the Co that cathode deposition gained area load has iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice and anode
Deposition gained area load has the Co of iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice, i.e. Ir/Co0.8Fe0.2Se2The monatomic catalysis of-NF
Agent, and the monatomic middle metallic atom mass fraction of iridium is all 3.98% in the monatomic catalyst.
Embodiment 4
A kind of Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, the Ir/Co0.8Fe0.2Se2- NF is single former
Muonic catalysis agent is equably to be supported on Co by monodisperse iridium atom0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted,
Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam, preparation
Method includes:
(1) Co is prepared0.8Fe0.2Se2- NF two-dimensional nano thin slice:
Under room temperature by the nickel foam of 1cm*3cm and 3.5mmol cobalt chloride, 0.22mmol iron chloride, 10.3mmol sodium chloride,
11.8mmol hexa, 20mL ethyl alcohol, the mixing of 160mL deionized water, after mixing evenly, the hydrolysis at 90 DEG C
3h is cooled to room temperature, and filtering, ethanol washing, drying at room temperature obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；By institute
State Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and 3.5mmol selenium powder, 7.5mmol sodium hydroxide, 0.15mL hydrazine hydrate, 25mL
N,N-Dimethylformamide mixing, after mixing evenly, the hydro-thermal reaction 1.5h at 190 DEG C is cooled to room temperature, filtering, ethyl alcohol
Washing, drying at room temperature obtain Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；
(2) Ir/Co is prepared0.8Fe0.2Se2The monatomic catalyst of-NF:
By above-mentioned Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is used as working electrode, platinum electrode conduct in three-electrode system
To electrode, saturated calomel electrode electrode is as reference electrode；It is added into the potassium hydroxide aqueous solution that 100mL concentration is 1mol/L
It is stirred evenly in the iridic chloride aqueous solution that 90 μ L concentration are 0.1mol/L, obtains the electrolyte solution comprising iridic chloride, and
The concentration of iridium is 0.09mmol/L, using Shanghai Chen Hua company CHI 660E electrochemical workstation, in the scanning speed of 5mV/s,
And cathode deposition scanning current potential (relative to reversible hydrogen electrode) is that -0.3-0.1V or anodic deposition scan current potential (relative to can
Inverse hydrogen electrode) to carry out linear voltammetric scan respectively 10 times under conditions of 1.3-1.8V, in scanning process, using magnetic agitation
Mode stirs electrolyte solution, and stirring rate 1400r/min makes iridium atom monodisperse, is uniformly deposited on
Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, working electrode is further taken out, 1.5min is rinsed with deionized water, repeats above-mentioned flushing
It is process 5 times, dry, respectively obtain the Co that cathode deposition gained area load has iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice and sun
Pole deposition gained area load has the Co of iridium0.8Fe0.2Se2- NF two-dimensional nano thin slice, i.e. Ir/Co0.8Fe0.2Se2- NF is monatomic to be urged
Agent, and the monatomic middle metallic atom mass fraction of iridium is all 3.25% in the monatomic catalyst.
Experimental example
At room temperature to Ir/Co0.8Fe0.2Se2The performance of the monatomic catalyst of-NF is assessed: by 1 gained foam of embodiment
Cathode and anodic deposition gained area load have the Co of iridium on nickel0.8Fe0.2Se2- NF two-dimensional nano thin slice, that is, Ir/
Co0.8Fe0.2Se2The size that it is 0.5cm*1cm that the monatomic catalyst of-NF, which is cut out, is respectively assembled in two electrode systems, electricity consumption
Clamp the Co that area load obtained by cathode and anodic deposition has iridium in pole0.8Fe0.2Se2- NF two-dimensional nano thin slice is respectively as yin
Pole and anode, electrolyte solution are the potassium hydroxide solution of 1mol/L；In 1-2V potential region with the scanning speed of 5mV/s into
Line voltammetric scan obtains Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF polarization curve in the reaction of electrocatalytic decomposition water,
The compensation of solution ohmmic drop is 1.8 Ω；Equally in the system, 10mA/cm is applied respectively with constant current mode2、100mA/cm2、
500mA/cm2Current density, record operating voltage change with time, obtain Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF
Constant current mode stability curve in the reaction of electrocatalytic decomposition water, testing time 100h, the compensation of solution ohmmic drop are 1.8
Ω。
Ir/Co is made respectively0.8Fe0.2Se2The monatomic catalyst of-NF, Co0.8Fe0.2Se2- NF nanocatalyst and commercialization
Polarization curve of the platinum carbon-iridium dioxide combination catalyst in the reaction of electrocatalytic decomposition water, shown in result figure 5, while the Ir/
Co0.8Fe0.2Se2The monatomic catalyst of-NF is as shown in Figure 6 in the stability test curve that electrocatalytic decomposition water reacts.Referring to Fig. 5
With Fig. 6 it is found that present invention gained Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF shows Zhuo in the reaction of electrocatalytic decomposition water
Catalytic activity and catalytic stability more, are not only successfully realized the breakthrough of performance under noble metal low-load amount, stability and
High current has great potential to the industrialized development that electrocatalytic decomposition water reacts.
Similarly, area load obtained by cathode in nickel foam obtained by embodiment 2-4 and anodic deposition there is into iridium
Co0.8Fe0.2Se2- NF two-dimensional nano thin slice, that is, Ir/Co0.8Fe0.2Se2The performance of the monatomic catalyst of-NF also carries out above-mentioned respectively
It is assessed, equally also shows brilliant catalytic activity and catalytic stability.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art within the technical scope of the present invention, according to the technique and scheme of the present invention and its invents
It is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of Ir/Co0.8Fe0.2Se2The monatomic catalyst of-NF, which is characterized in that the catalyst is by monodisperse Ir atom
Equably it is supported on Co0.8Fe0.2Se2- NF two-dimensional nano sheet surface is constituted, Co0.8Fe0.2Se2- NF two-dimensional nano thin slice is
Co0.8Fe0.2Se2Nano flake is carried on the complex carrier in nickel foam.
2. Ir/Co according to claim 10.8Fe0.2Se2The monatomic catalyst of-NF, which is characterized in that Ir atom with
Co0.8Fe0.2Se2The mass ratio of-NF two-dimensional nano thin slice is 2-4:95-105.
3. a kind of Ir/Co according to claim 1 or claim 20.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, feature exist
In, comprising: in the electrolyte solution comprising iridium salt, electrochemical deposition is carried out using three-electrode system, with Co0.8Fe0.2Se2-
NF two-dimensional nano thin slice carries out linear voltammetric scan as working electrode, makes iridium atom monodisperse, equably deposits to
Co0.8Fe0.2Se2On-NF two-dimensional nano thin slice, the Ir/Co is obtained0.8Fe0.2Se2The monatomic catalyst of-NF.
4. Ir/Co according to claim 30.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, which is characterized in that described
Iridium salt is iridic chloride, and also includes potassium hydroxide, the quality volume of potassium hydroxide and deionized water in the electrolyte solution
Than for 56-57mg:0.8-1.2mL, the mass ratio of potassium hydroxide and iridic chloride is 56-57:0.03-0.04.
5. according to the Ir/Co of claim 3 or 40.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, which is characterized in that
Prepare the Co0.8Fe0.2Se2The method of-NF two-dimensional nano thin slice includes: under room temperature
3-4mmol:0.15-0.25mmol:9.5-10.5mmol:11.5-12.5mmol:15-25mL: 150-200mL cobalt chloride, chlorine
Change iron, sodium chloride, hexa, ethyl alcohol, deionized water mixing, after mixing evenly the hydrolysis 1.5- at 80-100 DEG C
3h is cooled to room temperature, filters, and washs, dry, obtains Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice；It will be described
Co0.8Fe0.2(OH)2- NF two-dimensional nano thin slice and molal volume are than for 3-4mmol:7-8mmol:0.1-0.2mL:20-30mL's
Selenium powder, sodium hydroxide, hydrazine hydrate, n,N-Dimethylformamide mix, after mixing evenly the hydro-thermal reaction 1- at 160-200 DEG C
2h is cooled to room temperature, filters, and washs, dry, obtains Co0.8Fe0.2Se2- NF two-dimensional nano thin slice；Preferably, sheet-formed foam
The size specification of nickel is 0.8-1.2cm*2.6-3.5cm.
6. according to any one of the claim 3-5 Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, feature
It is, the electrochemical deposition is cathodic electrochemical deposition, and the scanning current potential of cathodic electrochemical deposition is relative to reversible hydrogen electrode
For -0.3-0.1V, scanning speed 4.8-5.2mV/s, scanning times are 8-12 times.
7. according to any one of the claim 3-5 Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, feature
It is, the electrochemical deposition is anode electrochemical deposition, and the scanning current potential of anode electrochemical deposition is relative to reversible hydrogen electrode
For 1.3-1.8V, scanning speed 4.8-5.2mV/s, scanning times are 8-12 times.
8. according to any one of the claim 3-7 Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, feature
It is, when carrying out electrochemical deposition, electrolyte solution, stirring rate 1300-1500r/ is stirred by the way of magnetic agitation
min。
9. according to any one of the claim 3-9 Ir/Co0.8Fe0.2Se2The preparation method of the monatomic catalyst of-NF, feature
It is, the preparation method further include: after the completion of linear voltammetric scan, take out working electrode, rinsed with polar solvent, in repetition
State flushing process 4-6 times；Preferably, washing time 1-2min, it is highly preferred that polar solvent is deionized water.
10. a kind of Ir/Co according to claim 1 or claim 20.8Fe0.2Se2The monatomic catalyst of-NF answering in the reaction of complete solution water
With.
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