CN112064060A - Nickel selenide/nickel iron substrate material and preparation method and application thereof - Google Patents
Nickel selenide/nickel iron substrate material and preparation method and application thereof Download PDFInfo
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- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 99
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000000758 substrate Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000006260 foam Substances 0.000 claims description 28
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 18
- 239000012498 ultrapure water Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 15
- 230000007935 neutral effect Effects 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 11
- 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 9
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 22
- 239000000047 product Substances 0.000 description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000002904 solvent Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000003346 selenoethers Chemical class 0.000 description 3
- 238000004729 solvothermal method Methods 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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- 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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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a nickel selenide/nickel-iron substrate material and a preparation method and application thereof, which are applied to the field of electrocatalysis.
Description
Technical Field
The invention belongs to the field of electrocatalytic materials, and particularly relates to a nickel selenide/nickel iron substrate material and a preparation method and application thereof.
Background
Hydrogen energy is considered a sustainable clean energy source to replace ever-diminishing fossil fuels. Electrochemical water splitting is a mature commercial technology, converts electric energy generated by intermittent renewable energy sources (such as solar energy, wind energy and the like) into chemical energy stored in hydrogen fuel, and solves the problems of effective storage and transportation. Currently, Ir-based and Ru-based compounds have high oxygen evolution performance (OER), and Pt group metals are the most effective Hydrogen Evolution (HER) catalysts, but their lack of resources and high cost greatly limit their wide application. Therefore, the design of OER and HER catalysts composed of elements rich in earth reserves is imminent. The water splitting is performed in a harsh solution to minimize its overpotential. However, the development of highly efficient and simultaneously bifunctional OER and HER catalysts in different electrolytes has the advantages of simplified system and reduced cost, which is a great challenge.
The metal alloy material has attracted great interest in electronics, optics and magnetism as a promising functional material, especially in catalysis. NiFe alloys are one of the promising candidates for accelerating catalytic kinetics due to their low cost and inherent catalytic activity. For better performance, compounding with other materials to obtain better electrocatalytic activity is often employed. In view of the fact that Ni-based selenides have similar physicochemical properties to the corresponding sulfides, it was concluded that high activity and stability of electrocatalysts of nickel-based selenides could be obtained by adjusting the crystal structure or microstructure. In the related technology, N-doped C-coated NiFe alloy particles are prepared by a solvent method and a solid phase method, and the N-doped C-coated NiFe alloy particles are used for OER under an alkaline condition, and show lower over potential and excellent stability. Also in the related art, uniform NiSe nanowire electrodes were prepared in situ on Nickel Foam (NF) by means of a solvothermal method, and showed excellent HER and OER in alkaline electrolytes. However, prepared byIt is rare that nickel selenide has good catalytic properties under both alkaline and neutral conditions. Thus, Ni-based selenide and NiFe alloy (NiSe/NiFe) are realized3) The combination of (a) and (b) and the subsequent exploration of their electrochemical properties as electrocatalytic materials are very urgent.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a nickel selenide/nickel iron base material and a preparation method and application thereof, wherein the preparation method adopts a final product directly synthesized by a one-step solvothermal strategy, has the characteristics of low reaction temperature, simple synthesis path, no need of large-scale equipment and harsh conditions, vanadium-doped nickel selenide is grown in situ on foamed nickel iron, and the prepared nickel selenide/nickel iron base material is applied to the field of electrocatalysis and has excellent HER and OER performances under alkaline and neutral conditions.
In order to achieve the above object, the present invention provides a method for preparing a nickel selenide/nickel iron base material, comprising the steps of:
the method comprises the following steps: pretreating the foamed nickel iron;
step two: pouring 75-80 mg of selenium powder into 2-3 mL of 50% hydrazine hydrate solution, and uniformly stirring until the transparent wine red solution A appears;
step three: pouring 5.77-17.42 mg of sodium dodecyl sulfate and 36.18-44.04 mg of vanadium trichloride into a container filled with absolute ethyl alcohol, stirring to obtain a solution B, pouring the solution A into the solution B, mixing to obtain a mixed solution C, then putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 158-162 ℃ for 10-14 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled to room temperature, taking out the foamed nickel iron cooled after the reaction, cleaning, collecting and drying to obtain the nickel selenide/nickel iron substrate material.
Preferably, the pretreatment in the first step comprises: firstly, ultrasonically cleaning foamed nickel iron cut into 1.5cm multiplied by 4cm in an acetone solution for 10-15 min, then placing the foamed nickel iron in a proper amount of hydrochloric acid solution with the concentration of 1-2 mol/L for ultrasonic cleaning for 10-15 s, then respectively and alternately washing the foamed nickel iron with absolute ethyl alcohol and ultrapure water for 2-3 times, and finally, drying the foamed nickel iron in vacuum at the temperature of 30-40 ℃ for 8-10 h for later use.
Preferably, magnetic stirring is adopted for stirring in the second step, the temperature is 60-65 ℃, the time is 30-40 min, and the rotating speed is 400-500 r/min.
Preferably, in the third step, sodium dodecyl sulfate is poured into the p-polyphenyl lining, and the mixture is stirred for 15-20 min at normal temperature to obtain a solution B.
Preferably, the hydrothermal reaction in the third step is carried out in a p-polyphenyl hydrothermal reaction kettle.
Preferably, the filling ratio of the p-polyphenyl hydrothermal reaction kettle in the hydrothermal reaction is 50-60%.
Preferably, the cleaning in the fourth step adopts 2-5 times of ultrapure water and 2-5 times of absolute ethyl alcohol for alternate cleaning.
Preferably, the drying temperature in the fourth step is 60-65 ℃, and the drying time is 5-6 h.
The invention also provides a nickel selenide/nickel iron base material prepared by the preparation method.
The invention also provides the application of the nickel selenide/nickel-iron base material as a nickel selenide/nickel-iron base self-supporting electrode in electrocatalytic reaction under alkaline or neutral conditions.
Compared with the prior art, the preparation method provided by the invention can be used for obtaining the tremella-shaped nickel selenide/nickel iron base material which is applied to the field of electrocatalysis, and can have excellent HER and OER performances under alkaline and neutral conditions, and compared with the prior art, the preparation method provided by the invention has the following beneficial effects:
1) the invention adopts the final product directly synthesized by the one-step solvothermal strategy, so the method has the characteristics of low reaction temperature, simple synthesis path, no need of large-scale equipment and harsh conditions and the like;
2) the selenium source used in the invention is selenium powder, the morphology regulator is sodium dodecyl sulfate, and the two raw materials are common materials, are easy to obtain and have low cost;
3) the invention adopts absolute ethyl alcohol as a solvent, is a common solvent, and has no toxicity and corrosiveness; compared with the common inorganic solvent, the organic solvent has lower boiling point, lower viscosity and surface tension, and low ionic strength, and has better place than water for certain reactions;
4) the foam nickel-iron adopted in the invention is used as a nickel source, because the construction of a three-dimensional multilevel structure usually needs a substrate with better conductivity as a support, and the foam nickel-iron has high conductivity, vanadium-doped nickel selenide is grown in situ on the foam nickel-iron by adopting solvothermal reaction, and the in-situ vanadium, the nickel selenide and the foam nickel-iron of the conductive substrate are compounded, so that the contact resistance can be effectively reduced, the distribution of a catalyst is improved, electrons can be rapidly transmitted to the surface of the catalyst and participate in the reaction, and the electro-catalytic activity and the stability of the catalyst are improved;
5) when the nickel selenide/nickel-iron base material prepared by the invention is applied to alkaline and neutral conditions, the nickel selenide/nickel-iron base material shows good electrochemical activity. NiSe/NiFe for the invention3The electrode was subjected to HER and OER tests in alkaline solution, when the current density reached 100mA/cm2The required overpotential is 240-257 mV and 270-280 mV respectively, and meanwhile, the NiSe/NiFe of the invention3The electrode was subjected to HER and OER tests in neutral solution, when the current density reached 100mA/cm2The required overpotential is 460-474 mV and 280-291 mV respectively, and the result shows that the NiSe/NiFe3The electrode shows excellent electrocatalytic performance under high current density under both alkaline and neutral media.
Drawings
FIG. 1 is a scheme for preparing NiSe/NiFe in example 1 of the invention3An X-ray diffraction (XRD) pattern of the electrode;
FIG. 2 is a schematic representation of the preparation of NiSe/NiFe in example 1 of the present invention3Low power Scanning Electron Microscope (SEM) photographs of the electrodes;
FIG. 3 is the preparation of NiSe/NiFe in example 1 of the invention3High power Scanning Electron Microscope (SEM) photographs of the electrodes;
FIG. 4 is a schematic representation of the preparation of NiSe/NiFe in example 1 of the present invention3A hydrogen production performance diagram (HER) and an oxygen production performance diagram (OER) of a Linear Sweep Voltammetry (LSV) curve of the electrode under an alkaline environment;
FIG. 5 is a schematic representation of the preparation of NiSe/NiFe in example 1 of the present invention3And (3) a hydrogen production performance graph (HER) and an oxygen production performance graph (OER) of the electrode in a neutral environment by Linear Sweep Voltammetry (LSV) curve.
Detailed Description
The present invention will be further explained with reference to the drawings and specific examples in the specification, and it should be understood that the examples described are only a part of the examples of the present application, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention discloses a preparation method of a nickel selenide/nickel iron substrate material, which comprises the following steps:
the method comprises the following steps: pretreating the foamed nickel iron; the pretreatment comprises the following steps: firstly, ultrasonically cleaning foamed nickel iron cut into 1.5cm multiplied by 4cm in an acetone solution for 10-15 min, then placing the foamed nickel iron in a proper amount of hydrochloric acid solution with the concentration of 1-2 mol/L for ultrasonic cleaning for 10-15 s, then respectively and alternately washing the foamed nickel iron with absolute ethyl alcohol and ultrapure water for 2-3 times, and finally, drying the foamed nickel iron in vacuum at the temperature of 30-40 ℃ for 8-10 h for later use;
step two: pouring 75-80 mg of selenium powder into 2-3 mL of 50% hydrazine hydrate solution, and uniformly stirring until the transparent wine red solution A appears; preferably, magnetic stirring is adopted for stirring, the temperature is 60-65 ℃, the time is 30-40 min, and the rotating speed is 400-500 r/min;
step three: pouring 5.77-17.42 mg of sodium dodecyl sulfate and 36.18-44.04 mg of vanadium trichloride into a container filled with absolute ethyl alcohol, stirring to obtain a solution B, pouring the solution A into the solution B, mixing to obtain a mixed solution C, then putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 158-162 ℃ for 10-14 hours; preferably, sodium dodecyl sulfate is poured into 50mL of p-polyphenyl lining, and the mixture is stirred for 15-20 min at normal temperature to obtain solution B; further preferably, the hydrothermal reaction is carried out in a p-polyphenyl hydrothermal reaction kettle, and the filling ratio of the p-polyphenyl hydrothermal reaction kettle in the thermal reaction is 50-60%;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled to room temperature, taking out the foamed nickel iron cooled after the reaction, cleaning, collecting and drying to obtain the nickel selenide/nickel iron substrate material. Preferably, the cleaning is carried out by alternately cleaning 2-5 times of ultrapure water and 2-5 times of absolute ethyl alcohol, the drying temperature is 60-65 ℃, and the time is 5-6 hours.
The invention also provides a nickel selenide/nickel iron base material prepared by the preparation method, which is in a silver ear shape and has a current density of 100mA/cm under an alkaline condition2During the process, the HER overpotential can reach 240-257 mV, and the OER overpotential can reach 270-280 mV; the current density under neutral conditions was 100mA/cm2In the process, the HER overpotential can reach 460-474 mV, and the OER overpotential can reach 280-291 mV.
The invention also provides the nickel selenide/nickel-iron substrate material which is used as a nickel selenide/nickel-iron substrate self-supporting electrode and applied to electrocatalytic reaction under alkaline or neutral conditions.
Example 1:
1) pretreatment of the foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 10min, then pouring the foam nickel iron into prepared 1mol/L hydrochloric acid for ultrasonic cleaning for 15s, then respectively and alternately washing for 2 times by using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 34 ℃ for 10h for later use;
2) pouring 75mg of selenium powder into 2mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the rotating speed of 400r/min for 40min at the temperature of 60 ℃ until the transparent solution A is wine red;
3) pouring 5.77mg of sodium dodecyl sulfate and 36.18mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring at normal temperature for 20min to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 158 ℃ for 14h, wherein the filling ratio is 50%;
4) after the hydrothermal reaction is finished, naturally cooling the kettle to room temperature, and then cooling the product after the reaction to obtain the foam nickel ironTaking out, alternately cleaning with 5 times of ultrapure water and 5 times of anhydrous ethanol, collecting, and drying at 60 deg.C for 6 hr to obtain Tremella-shaped nickel selenide/nickel-iron base (NiSe/NiFe)3) A self-supporting electrode.
NiSe/NiFe prepared in example 13The electrodes are respectively subjected to X-ray diffraction, low-power scanning and high-power scanning electron microscopes, referring to fig. 1, fig. 2 and fig. 3, wherein 1 in the figure can prove that the in-situ vanadium-doped NiSe phase is successfully prepared on the NiFe substrate, and the prepared NiSe/NiFe can be seen from fig. 2 and fig. 33The electrode presents a silver ear shape, and the porous structure is favorable for full contact of electrolyte and the electrode, so that the occurrence of catalytic reaction is accelerated, and the catalytic performance of the electrode is improved.
NiSe/NiFe prepared in example 13The electrodes were subjected to HER and OER tests in alkaline and neutral environments, respectively, see FIGS. 4 and 5, with current densities of 100mA/cm under alkaline conditions2Then HER overpotential can reach 240mV and OER overpotential can reach 270 mV; the current density reaches 100mA/cm under the neutral condition2When the overvoltage of HER reaches 460mV and the overvoltage of OER reaches 280mV, the result shows that NiSe/NiFe3The electrode shows excellent electrocatalytic performance under high current density under both alkaline and neutral media.
Example 2:
1) pretreating foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 11min, then pouring the foam nickel iron into prepared 2mol/L hydrochloric acid for ultrasonic cleaning for 12s, then respectively and alternately washing for 3 times by using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 40 ℃ for 8h for later use;
2) pouring 76mg of selenium powder into 3mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the temperature of 61 ℃ and the rotating speed of 450r/min for 35min until wine red transparent solution A appears;
3) pouring 8.1mg of sodium dodecyl sulfate and 37.75mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring at normal temperature for 19min to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at 159 ℃ for 13h, wherein the filling ratio is 52%;
4) after the hydrothermal reaction is finished, naturally cooling the kettle to room temperature, taking out the product foamed nickel iron cooled after the reaction, alternately cleaning by 4 times of ultrapure water and 4 times of absolute ethyl alcohol, collecting, and drying at the temperature of 61 ℃ for 6 hours to obtain the tremella-shaped nickel selenide/nickel iron substrate (NiSe/NiFe)3) A self-supporting electrode.
Example 3:
1) pretreating foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 12min, then pouring the foam nickel iron into prepared 1mol/L hydrochloric acid for ultrasonic cleaning for 14s, then respectively and alternately washing for 2 times by using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 38 ℃ for 8h for later use;
2) pouring 77mg of selenium powder into 2mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the rotating speed of 500r/min for 30min at the temperature of 62 ℃ until the transparent solution A is wine-red;
3) pouring 10.43mg of sodium dodecyl sulfate and 39.33mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring for 18min at normal temperature to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at 160 ℃ for 12h, wherein the filling ratio is 54%;
4) after the solvothermal reaction is finished, naturally cooling the kettle to room temperature, taking out the product foamed nickel iron cooled after the reaction, alternately cleaning the product foamed nickel iron by 5 times of ultrapure water and 5 times of absolute ethyl alcohol, collecting the product foamed nickel iron, and drying the product foamed nickel iron at the temperature of 62 ℃ for 6 hours to obtain the tremella-shaped nickel selenide/nickel iron substrate (NiSe/NiFe)3) A self-supporting electrode.
Example 4:
1) pretreating foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 13min, then pouring the foam nickel iron into prepared 2mol/L hydrochloric acid for ultrasonic cleaning for 11s, then respectively and alternately washing for 3 times by using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 35 ℃ for 9h for later use;
2) pouring 78mg of selenium powder into 3mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the temperature of 63 ℃ at the rotating speed of 400r/min for 40min until wine red transparent solution A appears;
3) pouring 12.76mg of sodium dodecyl sulfate and 40.90mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring for 17min at normal temperature to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 161 ℃ for 11h, wherein the filling ratio is 56%;
4) after the hydrothermal reaction is finished, naturally cooling the kettle to room temperature, taking out the product foamed nickel iron cooled after the reaction, alternately cleaning the foamed nickel iron by using ultrapure water and absolute ethyl alcohol for 3 times, collecting the product, and drying the product at 63 ℃ for 5 hours to obtain the silver ear-shaped nickel selenide/nickel iron substrate (NiSe/NiFe)3) A self-supporting electrode.
Example 5:
1) pretreating foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 14min, then pouring the foam nickel iron into prepared 1mol/L hydrochloric acid for ultrasonic cleaning for 13s, then respectively and alternately washing for 2 times by using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 32 ℃ for 10h for later use;
2) pouring 79mg of selenium powder into 2mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the rotating speed of 450r/min for 35min at the temperature of 64 ℃ until the transparent solution A is wine-red;
3) pouring 15.09mg of sodium dodecyl sulfate and 42.47mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring for 16min at normal temperature to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 158 ℃ for 14h, wherein the filling ratio is 58%;
4) after the hydrothermal reaction is finished, naturally cooling the kettle to room temperature, taking out the product foam ferronickel cooled after the reaction, passing through ultrapure water for 4 times and nickel-free for 4 timesAlternately cleaning with water and ethanol, collecting, and oven drying at 64 deg.C for 5 hr to obtain nickel selenide/nickel iron substrate (NiSe/NiFe)3) A self-supporting electrode.
Example 6:
1) pretreating foamed nickel iron: firstly, ultrasonically cleaning cut foam nickel iron with the size of 1.5cm multiplied by 4cm in an acetone solution for 15min, then pouring the foam nickel iron into prepared 2mol/L hydrochloric acid for ultrasonic cleaning for 10s, then alternately washing for 3 times by respectively using absolute ethyl alcohol and ultrapure water, and finally, drying in vacuum at 30 ℃ for 10h for later use;
2) pouring 80mg of selenium powder into 3mL of hydrazine hydrate solution with the mass concentration of 50%, and magnetically stirring at the rotating speed of 500r/min for 30min at the temperature of 65 ℃ until the transparent solution A is wine red;
3) pouring 17.42mg of sodium dodecyl sulfate and 44.04mg of vanadium trichloride into 50mL of p-polyphenyl lining filled with an absolute ethyl alcohol solvent, stirring for 15min at normal temperature to obtain a solution B, pouring the solution A into the solution B, putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 162 ℃ for 10h, wherein the filling ratio is 60%;
4) after the hydrothermal reaction is finished, naturally cooling the kettle to room temperature, taking out the product foamed nickel iron cooled after the reaction, alternately cleaning the product foamed nickel iron by 5 times of ultrapure water and 5 times of absolute ethyl alcohol, collecting the product foamed nickel iron, and drying the product foamed nickel iron at the temperature of 65 ℃ for 5 hours to obtain the silver ear-shaped nickel selenide/nickel iron substrate (NiSe/NiFe)3) A self-supporting electrode.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a nickel selenide/nickel iron base material is characterized by comprising the following steps:
the method comprises the following steps: pretreating the foamed nickel iron;
step two: pouring 75-80 mg of selenium powder into 2-3 mL of 50% hydrazine hydrate solution, and uniformly stirring until the transparent wine red solution A appears;
step three: pouring 5.77-17.42 mg of sodium dodecyl sulfate and 36.18-44.04 mg of vanadium trichloride into a container filled with absolute ethyl alcohol, stirring to obtain a solution B, pouring the solution A into the solution B, mixing to obtain a mixed solution C, then putting the pretreated foam nickel iron into the mixed solution C, and carrying out hydrothermal reaction at the temperature of 158-162 ℃ for 10-14 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled to room temperature, taking out the foamed nickel iron cooled after the reaction, cleaning, collecting and drying to obtain the nickel selenide/nickel iron substrate material.
2. The method for preparing a nickel selenide/nickel iron base material according to claim 1, wherein the pretreatment in the first step comprises: firstly, ultrasonically cleaning foamed nickel iron cut into 1.5cm multiplied by 4cm in an acetone solution for 10-15 min, then placing the foamed nickel iron in a proper amount of hydrochloric acid solution with the concentration of 1-2 mol/L for ultrasonic cleaning for 10-15 s, then respectively and alternately washing the foamed nickel iron with absolute ethyl alcohol and ultrapure water for 2-3 times, and finally, drying the foamed nickel iron in vacuum at the temperature of 30-40 ℃ for 8-10 h for later use.
3. The method for preparing a nickel selenide/nickel iron base material according to claim 1, wherein the stirring in the second step is magnetic stirring at 60-65 ℃ for 30-40 min at a rotation speed of 400-500 r/min.
4. The method for preparing the nickel selenide/nickel iron base material according to claim 1, wherein in the third step, sodium dodecyl sulfate is poured into the p-polyphenyl lining, and the mixture is stirred at normal temperature for 15-20 min to obtain solution B.
5. The method for preparing a nickel selenide/nickel iron base material according to the claim 1, wherein the hydrothermal reaction in the third step is carried out in a p-polyphenyl hydrothermal reaction kettle.
6. The method for preparing a nickel selenide/nickel iron base material according to claim 5, wherein the filling ratio of a p-polyphenyl hydrothermal reaction kettle in the hydrothermal reaction is 50-60%.
7. The method for preparing a nickel selenide/nickel iron base material according to claim 1, wherein the cleaning in the fourth step is performed by alternately cleaning 2-5 times of ultrapure water and 2-5 times of absolute ethyl alcohol.
8. The method for preparing a nickel selenide/nickel iron base material according to claim 7, wherein the drying temperature in the fourth step is 60-65 ℃ and the drying time is 5-6 h.
9. A nickel selenide/nickel-iron base material, which is prepared by the preparation method of the nickel selenide/nickel-iron base material as claimed in any one of claims 1 to 8.
10. Use of a nickel selenide/nickel iron base material according to claim 9 as a nickel selenide/nickel iron base self-supporting electrode in electrocatalytic reactions under alkaline or neutral conditions.
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