CN110227496B - Microspherical Fe-doped trinickel disulfide nano-structure material composed of nanosheets, and preparation method and application thereof - Google Patents
Microspherical Fe-doped trinickel disulfide nano-structure material composed of nanosheets, and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
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- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
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- 239000000203 mixture Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/33—
-
- B01J35/61—
-
- 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
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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
Abstract
The invention discloses a microspherical Fe-doped trinickel disulfide nano-structure material consisting of nanosheets, and a preparation method and application thereof. Dissolving nickel salt, ferric salt and thiourea in ethylene glycol, transferring the solution to a reaction kettle, obliquely placing foamed nickel in the solution, carrying out solvothermal reaction, cooling to room temperature after the reaction is finished, washing and drying the product to obtain the microspherical Fe-doped Ni nano-sheet3S2A nanostructured material. Compared with the prior art, the invention designs and synthesizes the microspherical Fe-doped Ni consisting of the nano sheets on the conductive foam nickel substrate3S2A nanostructure. The electrochemical active area and the conductivity of the material are improved by utilizing Fe doping. The microspherical Fe doped Ni consisting of the nano-sheets provided by the invention3S2The nano-structure material is used as an electro-catalyst for oxygen evolution reaction, hydrogen evolution reaction and total water decomposition reaction, and has the advantages of high catalytic activity, excellent stability, simple preparation process and low cost.
Description
Technical Field
The invention belongs to the field of nano material preparation methods and electrocatalysis application, and particularly relates to a microspherical Fe-doped Ni formed by nanosheets3S2Nanostructure material, preparation method and application.
Background
Electrocatalytic decomposition of water into hydrogen and oxygen provides a prospective and competitive technology to produce sustainable and renewable energy sources. However, the high overpotential of Oxygen Evolution Reaction (OER) and Hydrogen Evolution Reaction (HER) half-cell reactions severely limits the practical application of total water splitting. Advances in this technology require highly active, stable and low cost electrocatalytic materials to lower the energy barrier and improve the overall energy efficiency of OER and HER processes.
In recent years, a great deal of research has been devoted to OER and HER electrocatalysts, which are abundant in global resources and cost-effective. 3d transition metal compound by adjusting group thereofThe composite structure can obtain high catalytic performance, and attracts wide attention. Among these catalysts, a nickel-based compound, such as nickel sulfide, has a unique structure and high electrical conductivity, and is a promising water decomposition electrocatalyst. Ni3S2The Ni-Ni bonds in (1) have more covalent bonds than other Ni-based compounds and have corrosion resistance under similar operating conditions. Controlling morphology or doping other elements into Ni3S2The crystal lattice can improve the electrocatalytic water decomposition performance. A nickel sulfide nano-structure material doped with heterogeneous atoms is elaborately constructed, the appearance and the electronic structure are simultaneously regulated and controlled, high conductivity and unique surface chemistry are obtained, the water dissociation is facilitated, the electrocatalytic water dissociation behavior is further improved, the method is very important for practical application, and still is a great challenge.
Disclosure of Invention
The invention aims to provide microspherical Fe-doped Ni consisting of nanosheets3S2A nano-structured material is prepared through direct design and synthesis of microspherical Fe doped Ni on the base of conductive foam Ni by low-temp chemical liquid-phase method3S2Nano structure, simple synthesis process and low cost.
The invention also provides a microspherical Fe-doped Ni composed of the nanosheets3S2Application of the nanostructure material as an electrocatalyst for Oxygen Evolution Reaction (OER), Hydrogen Evolution Reaction (HER) or total moisture decomposition reaction.
The invention provides a microspherical Fe-doped Ni consisting of nanosheets3S2A method of preparing a nanostructured material comprising the steps of:
microspherical Fe-doped Ni composed of nanosheets3S2A method for preparing a structural material, the method comprising the steps of:
dissolving nickel salt, ferric salt and thiourea in ethylene glycol, transferring the solution to a reaction kettle, obliquely placing foamed nickel in the solution, carrying out solvothermal reaction, cooling to room temperature after the reaction is finished, washing and drying the product to obtain the microspherical Fe-doped Ni nano-sheet3S2Nano-junctionA structural material.
Further, the nickel salt is nickel nitrate hexahydrate; the iron salt is ferric nitrate nonahydrate.
The ratio of the amounts of the nickel salt, the iron salt and the thiourea is 0.75-1.25: 0.2-0.5: 0.75, preferably 0.75-1.25: 0.3: 0.75.
The concentration of the thiourea in ethylene glycol was 0.0375M.
The solvent thermal reaction condition is that the reaction is carried out for 6 to 10 hours at 140 ℃, and the reaction is preferably carried out for 8 hours at 140 ℃.
The foam Nickel (NF) needs to be cleaned before use, and the specific cleaning steps are as follows: soaking in 6M hydrochloric acid for 15min to remove the outer oxide film, and cleaning with deionized water and anhydrous ethanol for 3-5 times; when in use, the foam nickel is cut into the size of 2 multiplied by 3 cm.
The washing is 3-5 times by using deionized water and absolute ethyl alcohol respectively.
The drying is carried out in a vacuum drying oven at 55-60 ℃ for 6-12 h.
The invention also provides a microspherical Fe-doped Ni formed by the nanosheets prepared by the preparation method3S2Nanostructured materials, said microspheroidal Fe doped Ni3S2The morphology of the nano-structure material is a microspherical structure which is composed of nano sheets and has an average size of 250-350 nm.
The invention also provides microspherical Fe-doped Ni consisting of the nanosheets3S2The application of the nanostructure material as an electro-catalyst for oxygen evolution reaction or hydrogen evolution reaction or total water decomposition reaction.
Fe doped Ni composed of nanosheets3S2When the nano-structure material is applied as an electrocatalyst of an Oxygen Evolution Reaction (OER) or a Hydrogen Evolution Reaction (HER), the specific method comprises the following steps: the microspherical Fe composed of the nano-sheets prepared on the foamed nickel is doped with Ni3S2The nanostructured material was cut to 1 × 1cm size as a working electrode, and tested using a CHI760E electrochemical workstation with 1M KOH solution as electrolyte. Platinum wire (OER reaction) or carbon rod (HER reaction) and Ag/AgCl electrode were used as counter and reference electrodes, respectively. Linear Sweep Voltammetry (LSV) at 2.0mV·s-1The polarization curve is obtained at a scanning rate of 90% ohm compensation; stability was obtained by measuring the current density time curve at constant voltage. Electrochemically active area (ECSA) was determined by scanning (2, 4, 6, 8, 10, 12 and 14mV · s) at different scan rates without significant faraday region-1) Measurement of double layer capacitance (C) by Cyclic Voltammetry (CV)dl) Carrying out evaluation; electrochemical Impedance (EIS) open circuit voltage was tested in the frequency range of 100kHz to 0.1 Hz. In the commercial RuO2And Pt/C supported on nickel foam as electrodes, the performance of OER and HER were measured as a comparison, respectively.
The Fe is doped with Ni3S2When the nano-structure material is applied as an electrocatalyst of a full-water decomposition reaction, the specific method comprises the following steps: the microspherical Fe composed of the nano-sheets prepared on the foamed nickel is doped with Ni3S2The nanostructured material was cut into 2 pieces of 1 × 1cm size and assembled as cathode and anode in a two-electrode electrolytic cell, and the total water decomposition performance was tested by 90% iR compensated LSV polarization curve and current density time curve at constant voltage. As a comparison, the noble metal RuO supported on nickel foam in a two-electrode electrolyzer was investigated2LSV polarization curves as anode and Pt/C as cathode.
In the invention, the Fe doping realizes the adjustment of an electronic structure, improves the conductivity and increases the electrochemical active area. The overlap of the d-d orbitals between metal cations in the lattice delocalizes the charge, enhances lewis acidity, promotes the adsorption and activation of water, increases the electrophilicity of adsorbed oxygen, subsequently forms O-OH species by nucleophilic attack, further deprotonates the OOH species by an electron-withdrawing induction effect, producing oxygen. Furthermore, delocalization of the electrons between the cations provides donor-acceptor chemisorption sites for reversible adsorption of oxygen. In strong alkaline electrolyte, a thin surface oxide layer or surface hydroxide layer is formed on the surface of the catalyst in the electrolytic process and is the actual active site, and Fe doped Ni with higher conductivity is arranged below the surface3S2The electron transfer between the electrode and the metal oxide or metal hydroxide shell can be accelerated. Meanwhile, the thin oxide or hydroxide shell on the surface can reduce S-HadsFormation of a bond, and S-HadsThe bond is usually too stable to allow HadsConversion to H2It is difficult. The material shows excellent activity and excellent durability to oxygen evolution reaction, hydrogen evolution reaction and total hydrolysis reaction in alkaline electrolyte, and has great value for researching the practical application of water-decomposition electro-catalysis electrode material.
Compared with the prior art, the method utilizes the decomposition of thiourea on the conductive substrate nickel foam to generate S by a simple chemical liquid phase method2-Ions, with Ni2+Ion reaction to obtain Ni3S2Seed with a small amount of Fe3+Ion doping of Ni3S2A crystal lattice. Under the combined action of the inherent lamellar structure drive of the crystal and the coordination effect of ethylene glycol molecules, the crystal further grows to obtain the microspherical Fe-doped Ni consisting of nanosheets3S2A nanostructure. Prepared microspherical Fe-doped Ni consisting of nanosheets3S2The nano-structure material shows excellent catalytic activity and stability for oxygen evolution reaction, hydrogen evolution reaction and total water decomposition reaction, and the preparation process is environment-friendly, simple and low in cost.
Drawings
FIG. 1 is a microspherical Fe-doped Ni composition of nanosheets prepared in example 13S2An X-ray powder diffraction (XRD) pattern of the nanostructured material;
FIG. 2 is a microspherical Fe-doped Ni composition of nanosheets prepared in example 13S2An energy dispersive X-ray spectroscopy (EDX) map of the nanostructured material;
FIG. 3 is a microspherical Fe-doped Ni composition of nanosheets prepared in example 13S2A Scanning Electron Microscope (SEM) image of the nanostructured material;
FIG. 4 is a microspherical Fe-doped Ni composition of nanoplates prepared in example 13S2A Transmission Electron Microscope (TEM) image of the nanostructured material;
FIG. 5 is a microspherical Fe-doped Ni composition of nanoplates prepared in example 13S2Scanning transmission electron microscope pictures (STEM) and corresponding elemental profiles of the nanostructured material;
FIG. 6 shows microspherical Fe-doped Ni consisting of nanosheets with Fe doping amounts of 14.0% and 20.9% prepared in example 23S2An X-ray powder diffraction (XRD) pattern of the nanostructured material;
FIG. 7 shows microspherical Fe-doped Ni consisting of nanosheets with Fe doping amounts of 14.0% and 20.9% prepared in example 23S2An energy dispersive X-ray spectroscopy (EDX) map of the nanostructured material;
FIG. 8 shows microspherical Fe-doped Ni consisting of nanosheets with Fe doping amount of 14.0% prepared in example 23S2A Scanning Electron Microscope (SEM) image of the nanostructured material;
FIG. 9 shows microspherical Fe-doped Ni consisting of nanosheets with 20.9% Fe doping prepared in example 23S2A Scanning Electron Microscope (SEM) image of the nanostructured material;
FIG. 10 shows Fe-doped Ni with different Fe contents (14.0%, 16.9% and 20.9%) prepared in examples 1 and 23S2LSV profile of Oxygen Evolution Reaction (OER) of the product;
FIG. 11 shows Fe-doped Ni with different Fe contents (14.0%, 16.9% and 20.9%) prepared in examples 1 and 23S2LSV profile of Hydrogen Evolution Reaction (HER) of the product.
FIG. 12 is a microspherical Fe-doped Ni composition of nanoplatelets of example 33S2LSV profile of nanostructure material Oxygen Evolution Reaction (OER);
FIG. 13 shows microspherical Fe doped Ni composed of nanoplatelets of example 33S2A current density time profile of the nanostructure material Oxygen Evolution Reaction (OER);
FIG. 14 shows microspherical Fe doped Ni composed of nanoplatelets of example 33S2A capacitance current diagram of the nanostructure material at different scan rates;
FIG. 15 shows microspherical Fe doped Ni composed of nanoplatelets of example 33S2Impedance plot of the nanostructure material;
FIG. 16 shows microspherical Fe doped Ni composed of nanosheets of example 43S2Nanostructured materials hydrogen evolutionLSV plot of response (HER);
FIG. 17 shows microspherical Fe doped Ni composed of nanoplatelets of example 43S2Current density time profile of nanostructure material Hydrogen Evolution Reaction (HER);
FIG. 18 shows microspherical Fe doped Ni composed of nanoplatelets of example 53S2Polarization curve diagram of full water decomposition of nanostructure material in two-electrode system;
FIG. 19 is a microspherical Fe-doped Ni composition of nanoplatelets of example 53S2Current density time plot of total water decomposition of nanostructured materials in a two-electrode system.
Detailed Description
The invention is described in detail below with reference to the following examples and the accompanying drawings.
Example 1
Microspherical Fe-doped Ni consisting of nanosheets3S2A method of preparing a nanostructured material comprising the steps of:
soaking foamed nickel with the size of 2 multiplied by 3cm in 6M hydrochloric acid solution, washing the foamed nickel for 3 times by deionized water and absolute ethyl alcohol respectively after 15min, and drying to obtain the foamed nickel with a clean surface. Accurately measuring 40mL of ethylene glycol, adding the ethylene glycol into a clean small beaker, and then respectively weighing 2mmol of Ni (NO)3)2·6H2O，0.6mmol Fe(NO3)3·9H2O and 1.5mmol of thiourea are added into a small beaker and stirred to be dissolved for 20min, so as to obtain a uniform solution. Transferring the solution to a 50mL stainless steel reaction kettle with polytetrafluoroethylene as a lining, obliquely inserting the pretreated foamed nickel into the solution, sealing and reacting in a drying oven at 140 ℃ for 8 hours, naturally cooling to room temperature after the reaction is finished, respectively cleaning the foamed nickel covering the sample for 3 times by using deionized water and absolute ethyl alcohol, then drying the foamed nickel in a vacuum drying oven at 60 ℃ for 10 hours to obtain the microspherical Fe-doped Ni composite nano sheet3S2A nanostructured material.
The product obtained in example 1 was subjected to phase characterization by X-ray powder diffractometer, and the results are shown in FIG. 1, all diffraction peaks are similar to hexagonal phase N in JCPDS No.44-1418 cardi3S2The coincidence, compared with the standard card number, the diffraction peak is obviously shifted to the right, which shows that the Fe doping changes the electronic structure of the material.
Analysis of the product using energy dispersive X-ray spectroscopy (EDX), as shown in fig. 2, indicated successful coupling of Fe into the sample, with 0.38:1 atomic percent Fe and S, from which 16.9% Fe doping was calculated.
The sample prepared in example 1 is subjected to morphology analysis by using a Scanning Electron Microscope (SEM), and as shown in fig. 3, the sample is a microspherical nanostructure composed of nanosheets, and the average size of the microspheres is 250-350 nm.
The morphology of the sample was further observed using a Transmission Electron Microscope (TEM), and the result is shown in fig. 4, which indicates that the sample is a microspherical nanostructure composed of flexible nanosheets.
The scanning transmission electron microscope picture (STEM) of fig. 5 further illustrates that the sample is a spherical structure composed of nanosheets, and the corresponding elemental distribution diagram illustrates the uniform distribution of Ni, Fe, and S elements.
Example 2
Accurately measuring 40mL of ethylene glycol, adding the ethylene glycol into a clean small beaker, and then respectively weighing 2mmol of Ni (NO)3)2·6H2O, 0.4mmol or 0.8mmol of Fe (NO)3)3·9H2O and 1.5mmol of thiourea were added to a small beaker and stirred well. Obliquely inserting the dried foamed nickel into a stainless steel reaction kettle with a lining of 50mL polytetrafluoroethylene, transferring the solution into the reaction kettle after the solution is fully dissolved, and reacting for 8 hours in an oven at 140 ℃ after sealing. After the reaction is completed, naturally cooling to room temperature, washing the foam nickel covering the sample for several times by using deionized water and absolute ethyl alcohol, and then drying the foam nickel covering the sample in a vacuum drying oven at 60 ℃ for 12 hours to obtain Fe-doped Ni consisting of nanosheets with Fe doping amounts of 14.0% and 20.9%3S2A microspheroidal nanostructure.
The product obtained in example 2 was subjected to phase characterization by X-ray powder diffractometer, and the results are shown in FIG. 6, wherein all diffraction peaks are similar to hexagonal phase Ni in JCPDS No.44-1418 card3S2Anastomosis of the two phasesThe diffraction peak is shifted to the right compared to the standard card number.
The product was analyzed using energy dispersive X-ray spectroscopy (EDX), as shown in fig. 7, in which the atomic percentages of Fe and S elements were 0.303:1 and 0.493:1, respectively, from which the Fe doping amounts were calculated to be 14.0% and 20.9%.
Morphology analysis was performed on the sample prepared in example 2 using a Scanning Electron Microscope (SEM), and fig. 8 and 9 are Fe-doped Ni having Fe doping amounts of 14.0% and 20.9%, respectively3S2The SEM image shows that the samples are all microspherical nanostructures consisting of nanosheets.
FIG. 10 Fe-doped Ni with different Fe contents of 14.0%, 16.9% and 20.9%3S2Oxygen Evolution Reaction (OER) polarization curve of the product. It is shown that the doping amount of Fe significantly affects the OER activity, and the samples with the doping amount of Fe of 16.9% are better than the samples with the doping amounts of 14.0% and 20.9%.
FIG. 11 is Fe-doped Ni with different Fe contents of 14.0%, 16.9% and 20.9%3S2Hydrogen Evolution Response (HER) polarization curve of the product. The Fe doping amount is also shown to significantly influence the HER activity of the catalyst, and the sample with the Fe doping amount of 16.9% achieves the best.
Example 3
Microspherical Fe-doped Ni consisting of nanosheets3S2Application of the nano material as an Oxygen Evolution Reaction (OER) catalyst.
The specific application method comprises the following steps: ni is doped with microspherical Fe consisting of nanosheets with the area of 1 multiplied by 1cm3S2The nanomaterial was used as the working electrode and platinum wire and Ag/AgCl electrode as the counter and reference electrodes, respectively, were tested in a 1.0M KOH electrolyte solution using the CHI760E electrochemical workstation. Linear Sweep Voltammetry (LSV) at 2.0mV · s-1And the polarization curve was obtained at 90% ohmic compensation. As shown in FIG. 12, Fe was doped with Ni3S2The nano structure can realize 50mA cm only by using low overpotential of 233mV-2Current density of (2) to Ni3S2And commercial RuO292mV and 57mV as small as Ni3S2Based on example 1, Fe (NO) in the raw material is omitted3)3·9H2O is prepared. The OER electrocatalytic stability was evaluated using a current density time curve at an overpotential of 248mV, with the results shown in figure 13. After 14 hours of continuous electrolytic reaction, the current density remained at the first 98.3%, showing excellent electrocatalytic stability. Evaluation of the electrochemically active area of the material by double layer capacitance, Fe doped with Ni, as shown in FIG. 143S2The electric double layer capacitance was 7.93 mF. cm-2Is greater than Ni3S23.87 mF. cm-2Indicating that the doping of Fe increases the electrochemically active area of the sample. FIG. 15 is an Electrochemical Impedance (EIS) diagram showing Fe doped Ni3S2The semi-circle diameter of the nano structure is small, the slope of the straight line is large, and the nano structure is proved to have small resistance and faster catalytic kinetics.
Example 4
Microspherical Fe-doped Ni consisting of nanosheets3S2Use of nanostructured materials as Hydrogen Evolution Reaction (HER) catalysts.
The specific application method comprises the following steps: ni is doped with microspherical Fe consisting of nanosheets with the area of 1 multiplied by 1cm3S2The nanostructured material was used as a working electrode, a carbon rod and an Ag/AgCl electrode as a counter electrode and a reference electrode, respectively, and tested in a 1.0M KOH electrolyte solution using the CHI760E electrochemical workstation. Linear Sweep Voltammetry (LSV) at 2.0mV · s-1And the polarization curve was obtained at 90% ohmic compensation. As shown in FIG. 16, Fe was doped with Ni3S2The nano structure can reach 10mA cm under the overpotential of 130mV-2Current density much less than Ni3S2193mV of catalyst. Although Pt/C electrodes show outstanding HER activity at low current densities, the overpotential increases very rapidly at high current densities. Because the Pt/C is loaded on the foamed nickel through the adhesive, the Pt/C is easy to fall off. The HER electrocatalytic stability was evaluated using the current density time curve at a constant overpotential of 167mV, and as shown in fig. 17, the current density remained at the initial 93.9% over 14 hours of continuous electrolysis, indicating good HER electrocatalytic stability.
Example 5
Microspherical Fe-doped Ni consisting of nanosheets3S2The application of the nano-structure material as a catalyst for the total-moisture decomposition reaction.
The specific application method comprises the following steps: 2 Fe areas of 1X 1cm are doped with Ni3S2The nanostructures were assembled as anodes and cathodes, respectively, in a two-electrode electrolyzer and tested for full water splitting performance in a 1.0M KOH electrolyte solution by a 90% iR compensated LSV polarization curve (fig. 18) and a current density time curve at constant voltage (fig. 19). Fe doped Ni3S2The nano structure can reach 10mA cm under the voltage of 1.58V-2Current density, albeit slightly higher than Pt/C// RuO2The voltage of the couple is 1.50V, but the couple is electrolyzed continuously for 14 hours under the constant voltage of 1.627V without obvious attenuation, and the current density is kept to be 98.6 percent of the initial value, which shows that the couple has excellent durability in a double-electrode electrolytic cell.
The above detailed description of the microspherical Fe-doped trinickel disulfide nanostructured material composed of nanosheets, the preparation method and the application thereof with reference to the embodiments are illustrative and not restrictive, and several embodiments can be enumerated according to the limited scope, so that variations and modifications thereof without departing from the general concept of the present invention shall fall within the protection scope of the present invention.
Claims (7)
1. Microspherical Fe-doped Ni consisting of nanosheets3S2A method for preparing a nanostructured material, the method comprising the steps of:
dissolving nickel salt, ferric salt and thiourea in ethylene glycol, transferring the solution to a reaction kettle, obliquely placing foamed nickel in the solution, carrying out solvothermal reaction, cooling to room temperature after the reaction is finished, washing and drying the product to obtain the microspherical Fe-doped Ni nano sheet3S2A nanostructured material;
the solvothermal reaction condition is that the reaction is carried out for 6 to 10 hours at the temperature of 140 ℃;
the ratio of the nickel salt, the iron salt and the thiourea is 0.75-1.25: 0.2-0.5: 0.75.
2. The method according to claim 1, wherein the nickel salt is nickel nitrate hexahydrate; the iron salt is ferric nitrate nonahydrate.
3. The method according to claim 1 or 2, wherein the concentration of thiourea in the ethylene glycol is 0.0375M.
4. Microspherical Fe-doped Ni consisting of nanosheets prepared by the preparation method of any one of claims 1-33S2A nanostructured material.
5. Nanobule Fe-doped Ni made of nanoplatelets according to claim 43S2Use of nanostructured materials as Oxygen Evolution Reaction (OER) electrocatalysts.
6. Nanobule Fe-doped Ni made of nanoplatelets according to claim 43S2Use of nanostructured materials as Hydrogen Evolution Reaction (HER) electrocatalysts.
7. Nanobule Fe-doped Ni made of nanoplatelets according to claim 43S2Application of the nanostructure material as an electrocatalyst of a total hydrolysis reaction.
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| CN113897636B (en) * | 2021-10-20 | 2022-10-11 | 中国科学院金属研究所 | FeS 2 /NiS 2 Preparation method of core-shell electrocatalyst |
| CN114016073B (en) * | 2021-10-25 | 2023-12-19 | 吉林师范大学 | Fe doped Ni 0.85 Preparation method of Se nano sheet array electrocatalyst |
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| CN115094472A (en) * | 2022-06-21 | 2022-09-23 | 上海嘉氢源科技有限公司 | Iron-doped Ni 3 S 2 Nano material, preparation method and application |
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