CN117779089A - Iron-doped trinickel disulfide material and preparation method and application thereof - Google Patents
Iron-doped trinickel disulfide material and preparation method and application thereof Download PDFInfo
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- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000013535 sea water Substances 0.000 claims abstract description 48
- 239000002135 nanosheet Substances 0.000 claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 150000002815 nickel Chemical class 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 69
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 53
- 239000006260 foam Substances 0.000 claims description 28
- 229910052742 iron Inorganic materials 0.000 claims description 27
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 24
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- -1 iron ions Chemical class 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 241000237852 Mollusca Species 0.000 claims description 3
- 241000080590 Niso Species 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000003575 carbonaceous material Substances 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 125000004434 sulfur atom Chemical group 0.000 claims description 3
- 239000010411 electrocatalyst Substances 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000011065 in-situ storage Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 76
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 27
- 238000000354 decomposition reaction Methods 0.000 description 25
- 239000003054 catalyst Substances 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 239000003792 electrolyte Substances 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000004809 Teflon Substances 0.000 description 6
- 229920006362 Teflon® Polymers 0.000 description 6
- 229910000474 mercury oxide Inorganic materials 0.000 description 6
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229960002089 ferrous chloride Drugs 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 229910018553 Ni—O Inorganic materials 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Catalysts (AREA)
Abstract
The invention is suitable for the technical field of electrocatalysts, and provides an iron-doped trinickel disulfide material, a preparation method and application thereof, wherein the iron-doped trinickel disulfide material has a nano-sheet structure, grows on a conductive substrate and is formed by stacking light and thin nano-sheets with different sizes; the preparation method comprises the following steps: the preparation method comprises the steps of taking a material with better conductivity as a substrate, taking ferric salt, nickel salt, N-dimethyl imidazole and thioacetamide as precursors, and carrying out hydrothermal reaction in a high-temperature environment to obtain the iron-doped trinickel disulfide nano-sheet. The method utilizes the one-step hydrothermal method to grow the iron-doped trinickel disulfide nano-sheet on the conductive substrate in situ, and is simple and efficient; and the iron-doped trinickel disulfide is used as an alkaline water and alkaline seawater oxidation electrode, has rich active sites, and shows excellent alkaline seawater oxidation catalytic activity and stability.
Description
Technical Field
The invention belongs to the technical field of electrocatalysts, and particularly relates to an iron-doped trinickel disulfide material, and a preparation method and application thereof.
Background
Among the many new energy sources, hydrogen energy (H 2 ) The novel energy carrier is considered to be a promising new energy carrier because of the characteristics of high energy, cleanness and no pollution, and is expected to become one of the main energy sources in the future. The traditional hydrogen production method mainly comprises methane reforming, water gas and electrolyzed water. Compared with the other two choices, the hydrogen production by water electrolysis has no pollution in the preparation process, and the products only comprise hydrogen and oxygen, so that the hydrogen production by water electrolysis is highly focused by researchers. However, the industrialization of the electrocatalytic decomposition of water is severely hindered due to the slow kinetics of the electrolytic water oxygen evolution half reaction (oxygen reduction reaction), the high price of commercial electrocatalysts ruthenium dioxide and iridium dioxide, and the large energy consumption, poor activity and instability of the traditional catalyst preparation process. Therefore, development of an electrocatalyst which is cost-effective, has good catalytic activity and can be widely applied to the commercial field is imperative, in particular to an electrolytic water anode catalyst. Another concern is the limited total amount of fresh water resources in the world, which is scarce in some countries. If a route for producing hydrogen by electrolyzing fresh water is adopted on a large scale, the method can bring great pressure to scarce fresh water resources. In contrast, seawater resources account for about 96.5% of the total amount of terrestrial water resources, so we can utilize electrocatalytic seawater decomposition to realize clean and sustainable energy technologies. However, the high concentration of chloride ions in seawater not only competes with Oxygen Evolution Reaction (OER) of electrolyzed water on the anode catalyst, but also severely corrodes most catalysts containing metal elements, which also puts high demands on the resistance of the electrocatalyst to chloride ion corrosion.
Among the numerous electrocatalysts, transition metal sulfides have attracted wide attention in the field of electrocatalytic pure water and seawater decomposition due to their good electron transport ability and electrocatalytic properties. However, the defects of poor stability, less exposure of active sites, complicated preparation process and the like are still to be improved, and the activity of the material is also to be improved. Therefore, we propose an iron-doped trinickel disulfide material, and a preparation method and application thereof.
Disclosure of Invention
The invention aims to provide an iron-doped trinickel disulfide material, a preparation method and application thereof, and aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
an iron-doped trinickel disulfide material which exhibits a nano-sheet structure grown on a conductive substrate and formed by stacking nano-sheets of different sizes, wherein the iron-doped trinickel disulfide material has a nickel atom content of 40.37% -58.49%, an iron atom content of 0.20% -1.40% and a sulfur atom content of 30.21% -40.23%.
The preparation method of the iron-doped trinickel disulfide material comprises the following steps:
s1, adding ferric salt and nickel salt into deionized water, and stirring to form a solution A;
s2, mixing and stirring the N, N-dimethyl imidazole aqueous solution and deionized water to form a solution B;
step S3, rapidly mixing the solution A and the solution B, adding thioacetamide solid, and stirring until the thioacetamide solid is completely dissolved to form a mixed solution C;
and S4, carrying out hydrothermal reaction on the conductive substrate and the mixed solution C, washing the conductive substrate and the mixed solution C after the reaction is finished, and drying the conductive substrate and the mixed solution C in an oven to obtain the iron-doped trinickel disulfide nano-sheet growing on the conductive substrate.
Further, in the step S1, the iron salt is Fe (NO 3 ) 3 、Fe 2 (SO 4 ) 3 、FeCl 2 And FeCl 3 Any one of them; the nickel salt is Ni (NO) 3 ) 2 、NiSO 4 And NiCl 2 Any one of the following.
Further, in the step S1, the concentration range of nickel or iron ions in the solution A is 10-60 mmol/L; the concentration range of the N, N-dimethyl imidazole in the solution B is 100-600 mmol/L.
Further, in the step S4, the conductive substrate is any one of metal nickel foam, metal nickel mesh, metal nickel felt, stainless steel felt, metal nickel iron foam, metal copper foil, metal copper foam, metal iron foam, metal titanium mesh, carbon cloth, carbon paper, graphite felt, carbon fiber, and carbon material after calcining various shells and mollusk shells.
In the step S4, the hydrothermal temperature is 100-200 ℃, and the hydrothermal reaction time is 4-14 h.
The iron-doped trinickel disulfide material is applied to the oxidation reaction of alkaline water or alkaline seawater.
Further, the specific application method comprises the following steps: the iron-doped trinickel disulfide material is placed in an alkaline system to be used as an oxygen evolution electrode for the oxidation reaction of alkaline water and alkaline seawater.
Compared with the prior art, the invention has the beneficial effects that:
1. the electrode material is prepared by adopting a one-step hydrothermal method. Directly adding the conductive substrate washed by hydrochloric acid into a mixed solution containing Thioacetamide (TAA), N-dimethyl imidazole and ferronickel ions, and carrying out hydrothermal treatment at the hydrothermal temperature of 100-200 ℃ for 4-14 h to obtain the nano flaky micro iron doped trinickel disulfide material. The three-dimensional nano-sheet array structure formed by the micro-iron doped trinickel disulfide effectively increases the electrochemical active surface area of the three-dimensional nano-sheet array structure and provides a large number of reactive centers; the doping of trace iron improves the intrinsic activity of the electrocatalyst and enhances the conductivity and the chloride ion corrosion resistance of the electrocatalyst.
2. The nano flaky trace iron doped trinickel disulfide material provided by the invention is used as a working electrode for electrocatalytic decomposition of alkaline pure water and alkaline seawater, and has excellent catalytic activity. In an alkaline pure water solution (1 mol/L potassium hydroxide pure water), when the current densities were 10mA/cm, respectively 2 And 100mA/cm 2 At the time, the minimum potential required for the reversible hydrogen electrode was 1.433V (. Eta.) 10mA =203 mV) and 1.516V (η 100mA =286 mV), far lower than the trinickel disulfide electrocatalyst without trace iron additions and the commercial ruthenium dioxide electrocatalyst;in an alkaline seawater solution (1 mol/L potassium hydroxide seawater), when the current densities were 10mA/cm, respectively 2 And 100mA/cm 2 At the same time, the minimum potential required for the reversible hydrogen electrode was 1.456V (. Eta 10mA =226 mV) and 1.539V (η 100mA =309 mV). In an alkaline seawater solution (1 mol/L potassium hydroxide seawater), the current density was 100mA/cm 2 When the catalyst was stable for 2000 hours, the performance did not significantly decay after long-term stability testing.
Drawings
FIG. 1 is a trace amount of iron doped trinickel disulfide (noted as Fe-Ni) grown on a nickel foam substrate 3 S 2 /NF).
In FIG. 2, (A) to (D) are nano-sheet active materials Fe-Ni 3 S 2 SEM image of/NF; (E) And (F) is Fe-Ni 3 S 2 SEM image after electro-activation of the reconstructed NF.
FIG. 3 is a diagram of Fe-Ni 3 S 2 X-ray spectroscopy (EDX) elemental profile of NF.
In FIG. 4, (A) is Fe-Ni 3 S 2 /NF、Ni 3 S 2 X-ray diffraction (XRD) patterns of NF (trinickel disulfide material without trace iron doping regulation) and FeS/IF (ferrous sulfide supported on foam iron); (B) Is Fe-Ni 3 S 2 /NF、Ni 3 S 2 Raman spectra of/NF and FeS/IF; (C) is XRD pattern of Fe-Ni3S2/NF before and after electrochemical activation; (D) Is Fe-Ni 3 S 2 Raman spectra before and after NF electrochemical activation; (E) XRD patterns of samples prepared at different hydrothermal times when the hydrothermal temperature is 120 ℃; (F) XRD patterns of samples prepared at different hydrothermal temperatures were obtained at a hydrothermal time of 12 h.
In FIG. 5, (A) Fe-Ni was measured at a scanning rate of 5mV/s in a 1mol/L potassium hydroxide pure water solution 3 S 2 /NF、Ni 3 S 2 /NF, feS/IF and commercial catalyst RuO 2 Is a polarization diagram of the oxygen reduction reaction; (B) To determine Fe-Ni in 1mol/L potassium hydroxide pure water solution 3 S 2 /NF、Ni 3 S 2 Electric double layer capacitance diagrams of/NF and FeS/IF; (C) To 1mol/L potassium hydroxide pure waterFe-Ni in solution 3 S 2 /NF、Ni 3 S 2 Normalized oxygen reduction polarization curves for NF and FeS/IF; (D is Fe-Ni 3 S 2 /NF、Ni 3 S 2 /NF, feS/IF and commercial catalyst RuO 2 The corresponding current density in 1mol/L potassium hydroxide solution is 10mA/cm 2 、100mA/cm 2 Is used for the overvoltage map of (1); (E) For Fe-Ni in 1mol/L potassium hydroxide pure water solution 3 S 2 /NF、Ni 3 S 2 /NF, feS/IF and commercial catalyst RuO 2 A corresponding tafel slope map; (F) For Fe-Ni in 1mol/L potassium hydroxide pure water solution 3 S 2 /NF、Ni 3 S 2 Corresponding electrochemical impedance diagrams of/NF and FeS/IF; (G) Is Fe-Ni 3 S 2 The oxygen reduction polarization curve graph is measured by NF in 1mol/L potassium hydroxide pure water solution, 1mol/L potassium hydroxide+0.5 mol/L NaCl pure water solution and 1mol/L potassium hydroxide seawater solution at a scanning rate of 5 mV/s; (H) The current density of the prepared sample and the sample reported in the literature of contemporaneous related electrolytic alkaline pure water and seawater is 10mA/cm 2 Overpotential versus current density.
In FIG. 6, (A) is Fe-Ni 3 S 2 NF was carried out at 100mA/cm in 1mol/L potassium hydroxide pure water solution 2 A voltage-time diagram for a steady operation of current density for 1000 hours; (B) Is Fe-Ni 3 S 2 NF is 1mol/L potassium hydroxide 100mA/cm in seawater solution 2 The current density was stable for 2000h of voltage versus time.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Specific implementations of the invention are described in detail below in connection with specific embodiments.
According to the iron-doped trinickel disulfide material provided by the embodiment of the invention, the iron-doped trinickel disulfide material has a nano-sheet structure, is grown on a conductive substrate and is formed by stacking nano-sheets with different sizes, and in the iron-doped trinickel disulfide material, the nickel atom content is 40.37% -58.49%, the iron atom content is 0.20% -1.40% and the sulfur atom content is 30.21% -40.23%.
The preparation method of the iron-doped trinickel disulfide material provided by the embodiment of the invention comprises the following steps of:
s1, adding ferric salt and nickel salt into deionized water, and stirring to form a solution A;
s2, mixing and stirring the N, N-dimethyl imidazole aqueous solution and deionized water to form a solution B;
step S3, rapidly mixing the solution A and the solution B, adding thioacetamide solid, and stirring until the thioacetamide solid is completely dissolved to form a mixed solution C;
and S4, carrying out a hydrothermal reaction on the conductive substrate and the mixed solution C, wherein the hydrothermal temperature is 100-200 ℃, the hydrothermal reaction time is 4-14 h, washing the conductive substrate after the reaction is finished, and drying the conductive substrate and the mixed solution C in an oven to obtain the iron-doped trinickel disulfide nano-sheet growing on the conductive substrate.
As a preferred embodiment of the present invention, in the step S1, the iron salt is Fe (NO 3 ) 3 、Fe 2 (SO 4 ) 3 、FeCl 2 And FeCl 3 Any one of them; the nickel salt is Ni (NO) 3 ) 2 、NiSO 4 And NiCl 2 Any one of the following.
As a preferred embodiment of the present invention, in the step S1, the concentration of nickel or iron ions in the solution A is in the range of 10 to 60mmol/L; the concentration range of the N, N-dimethyl imidazole in the solution B is 100-600 mmol/L.
In the step S4, the conductive substrate is any one of metallic nickel foam, metallic nickel mesh, metallic nickel felt, stainless steel felt, metallic nickel-iron foam, metallic copper foil, metallic copper foam, metallic iron foam, metallic titanium mesh, carbon cloth, carbon paper, graphite felt, carbon fiber, and carbon material after calcining various shells and mollusk shells.
An embodiment of the present invention provides an iron-doped trinickel disulfide material as described above for use in an oxidation reaction of alkaline water or alkaline seawater.
As a preferred embodiment of the invention, the specific application method is as follows: the iron-doped trinickel disulfide material is placed in an alkaline system to be used as an oxygen evolution electrode for the oxidation reaction of alkaline water and alkaline seawater.
Example 1, the method for preparing iron-doped trinickel disulfide nanosheets according to an embodiment of the present invention includes the following steps:
firstly, sequentially placing metal nickel foam with the size of 1 cm-2 cm-1 mm into hydrochloric acid solution with the concentration of 3mol/L, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 40mmol/L nickel nitrate and 20mmol/L ferrous chloride into deionized water, and stirring and dissolving to form a solution A; 400mmol/L N, N-dimethyl imidazole is added into deionized water, and stirred and dissolved to form solution B; rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the metal nickel foam and the mixed solution C into a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 120 ℃ for 12h, washing after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst (marked as Fe-Ni) growing on the nickel foam in situ 3 S 2 /NF”)。
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide material is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
In FIG. 2, it can be seen from A to D that the foam nickel substrate is supported with Fe-Ni 3 S 2 Rear watchThe surface becomes rough, the size of the nano-sheet composed of micro-iron doped trinickel disulfide/foam nickel is 1-10 mu m, and the thickness of the nano-sheet is about 10-100 nm; see E and F for Fe-Ni 3 S 2 After electrochemical cremation, the morphology is changed from nano-flake shape to ox horn shape.
The composition of Fe-Ni can be seen with reference to FIG. 3 3 S 2 The Ni, fe, C, O and S elements of/NF are uniformly distributed.
In FIG. 4, see A, a comparison of Jade database PDF#44-1418, shows XRD characteristic peaks of the synthesized samples versus Ni 3 S 2 To illustrate the successful synthesis of a trinickel disulfide/nickel foam material; see B for Fe-Ni 3 S 2 The Raman spectrum of the/NF has a characteristic peak of Fe-S, ni-S, which further indicates the successful synthesis of the material; see C for Ni before and after electrochemical activation 3 S 2 The characteristic peaks of (2) still exist, which indicates that the material is not completely reconstructed; see D for 400-600 cm -1 The characteristic peak of Ni-O/Ni-OH bond of wave number shows that amorphous nickel oxide/hydroxide is generated on the surface of the material after electrochemical activation; see E, it can be seen that the hydrothermal duration is longer than 6h, and the Ni appears in the prepared material 3 S 2 XRD characteristic peaks of (2); it can be seen from F that Ni appears only in the prepared material when the hydrothermal temperature is higher than 100 DEG C 3 S 2 Is an XRD characteristic peak of (C).
In FIG. 5, see A, fe-Ni can be seen as compared to the comparative sample 3 S 2 the/NF material has optimal performance of electrocatalytic decomposition of alkaline pure water when the current density is 10 and 100mA/cm 2 At the time, the minimum potential required for the reversible hydrogen electrode was 1.433V (. Eta.) 10mA =203 mV) and 1.516V (η 100mA =286 mV), which is superior to the commercial noble metal catalyst RuO 2 The method comprises the steps of carrying out a first treatment on the surface of the See B, comparing with the control, illustrate Fe-Ni 3 S 2 NF has the greatest electrochemically active surface area and the greatest number of active sites; see C, compared to the control, fe-Ni 3 S 2 NF has the strongest intrinsic activity; with reference to D, the Fe-Ni can be visually seen compared with the comparison sample 3 S 2 the/NF was 10mAcm 2 、100mA/cm 2 The overpotential at the time is the lowest; see E, compared to the control, fe-Ni 3 S 2 the/NF has the lowest Tafil slope, indicating Fe-Ni 3 S 2 NF has faster reaction kinetics; see F, compared with the control, fe-Ni 3 S 2 The NF has the smallest charge transfer resistance, which indicates that the doping of trace Fe improves the conductivity and mass transfer capacity of the original material; see G for Fe-Ni 3 S 2 The performance of the electro-catalytic decomposition of alkaline seawater of/NF is slightly lower than that of the electro-catalytic decomposition of alkaline pure water, because the pH value of alkaline seawater is slightly lower than that of alkaline pure water (pH (alkaline seawater) ≡13.8); referring to H, it can be seen that the electrocatalytic decomposition water properties of the material are at a moderate level.
In FIG. 6, see A for Fe-Ni 3 S 2 The NF has excellent stability; see B for Fe-Ni 3 S 2 The NF has excellent stability of the electrocatalytic decomposition seawater and stronger function of resisting chloride ion corrosion.
Example 2, the method for preparing iron-doped trinickel disulfide nanosheets according to an embodiment of the present invention includes the following steps:
firstly, sequentially placing metal iron foam with the size of 1 cm-2 cm-1 mm into hydrochloric acid solution with the concentration of 3mol/L, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 60mmol/L nickel nitrate and 10mmol/L ferric chloride into deionized water, and stirring and dissolving to form solution A; adding 500mmol/L N, N-dimethyl imidazole into deionized water, and stirring for dissolving to form a solution B; and (3) rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the metal iron foam and the mixed solution C into a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 100 ℃ for 14h, washing after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst growing on the iron foam in situ.
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
The sample was at 10mA/cm 2 And 100mA/cm 2 The overpotential for alkaline seawater oxidation at current density is shown in table 1.
Example 3, the method for preparing the iron-doped trinickel disulfide nanosheets according to the embodiment of the invention comprises the following steps:
firstly, sequentially placing metal copper foam with the size of 1 cm-2 cm-1 mm in a hydrochloric acid solution with the concentration of 3mol/L, absolute ethyl alcohol and deionized water, performing ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 50mmol/L nickel nitrate and 30mmol/L ferric sulfate into deionized water, and stirring and dissolving to form a solution A; adding 500mmol/L N, N-dimethyl imidazole into deionized water, and stirring for dissolving to form a solution B; and (3) rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the metal copper foam and the mixed solution C into a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 140 ℃ for 10h, washing after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst growing on the copper foam in situ.
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
The sample was at 10mA/cm 2 And 100mA/cm 2 The overpotential for alkaline seawater oxidation at current density is shown in table 1.
Example 4, the method for preparing iron-doped trinickel disulfide nanosheets according to an embodiment of the present invention includes the following steps:
firstly, sequentially placing 1cm x 2cm x 1mm carbon cloth in a hydrochloric acid solution of 3mol/L, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 30mmol/L nickel nitrate and 40mmol/L ferric nitrate into deionized water, and stirring and dissolving to form a solution A; adding 300mmol/L N, N-dimethyl imidazole into deionized water, and stirring and dissolving to form a solution B; and (3) rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the carbon cloth and the mixed solution C in a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 160 ℃ for 8h, washing cleanly after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst growing on the carbon cloth in situ.
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
The sample was at 10mA/cm 2 And 100mA/cm 2 The overpotential for alkaline seawater oxidation at current density is shown in table 1.
Example 5, a method for preparing an iron-doped trinickel disulfide nanosheet according to an embodiment of the present invention includes the following steps:
firstly, placing a stainless steel felt with the size of 1cm x 2cm x 1mm in a hydrochloric acid solution with the concentration of 3mol/L, absolute ethyl alcohol and deionized water in sequence, performing ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 20mmol/L nickel sulfate and 50mmol/L ferrous chloride into deionized water, and stirring and dissolving to form a solution A; 200mmol/L N, N-dimethyl imidazole is added into deionized water, and stirred and dissolved to form solution B; and (3) rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the stainless steel felt and the mixed solution C into a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 180 ℃ for 6h, washing after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst growing on the stainless steel felt in situ.
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
The sample was at 10mA/cm 2 And 100mA/cm 2 The overpotential for alkaline seawater oxidation at current density is shown in table 1.
Example 6, the method for preparing an iron-doped trinickel disulfide nanosheet according to an embodiment of the present invention includes the following steps:
firstly, sequentially placing 1 cm-2 cm-1 mm metal titanium foam in a hydrochloric acid solution with the concentration of 3mol/L, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 15min, and drying for later use;
step 2, adding 10mmol/L nickel chloride and 60mmol/L ferrous chloride into deionized water, and stirring and dissolving to form a solution A; adding 100mmol/L N, N-dimethyl imidazole into deionized water, and stirring and dissolving to form a solution B; and (3) rapidly mixing the solution A and the solution B, adding 1mol/L thioacetamide, stirring for 10min to form a mixed solution C, placing the metal titanium foam and the mixed solution C into a Teflon reaction kettle, performing hydrothermal reaction at a high temperature of 200 ℃ for 4h, washing after the reaction is finished, and then drying in an oven set at 40 ℃ for 6h to obtain the iron-doped trinickel disulfide nano-sheet catalyst growing on the titanium foam in situ.
The application of the iron-doped trinickel disulfide nanosheets provided by the embodiment of the invention comprises the following specific steps: the nano flaky trace iron doped trinickel disulfide is used as a working electrode, a carbon rod is used as a counter electrode, mercury oxide is used as a reference electrode, and the electrocatalytic decomposition of alkaline pure water and the reaction of alkaline seawater are carried out in an alkaline three-electrode system. Wherein, the electrolyte ratio of the electrocatalytic decomposition alkaline pure water is 1mol/L potassium hydroxide pure water solution, and the electrolyte ratio of the electrocatalytic decomposition alkaline seawater is 1mol/L potassium hydroxide seawater.
The sample was at 10mA/cm 2 And 100mA/cm 2 The overpotential for alkaline seawater oxidation at current density is shown in table 1.
TABLE 1 Fe-Ni prepared by different examples 3 S 2 Alkaline seawater oxidation performance summary of samples
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and improvements can be made by those skilled in the art without departing from the spirit of the present invention, and these should also be considered as the scope of the present invention, which does not affect the effect of the implementation of the present invention and the utility of the patent.
Claims (8)
1. An iron-doped trinickel disulfide material, characterized in that the iron-doped trinickel disulfide material has a nano-sheet structure, is grown on a conductive substrate and is formed by stacking nano-sheets of different sizes, and the iron-doped trinickel disulfide material has a nickel atom content of 40.37% -58.49%, an iron atom content of 0.20% -1.40% and a sulfur atom content of 30.21% -40.23%.
2. A method for preparing the iron-doped trinickel disulfide material according to claim 1, comprising the steps of:
s1, adding ferric salt and nickel salt into deionized water, and stirring to form a solution A;
s2, mixing and stirring the N, N-dimethyl imidazole aqueous solution and deionized water to form a solution B;
step S3, rapidly mixing the solution A and the solution B, adding thioacetamide solid, and stirring until the thioacetamide solid is completely dissolved to form a mixed solution C;
and S4, carrying out hydrothermal reaction on the conductive substrate and the mixed solution C, washing the conductive substrate and the mixed solution C after the reaction is finished, and drying the conductive substrate and the mixed solution C in an oven to obtain the iron-doped trinickel disulfide nano-sheet growing on the conductive substrate.
3. The method for preparing iron-doped trinickel disulfide material according to claim 2, wherein in step S1, the iron salt is Fe (NO 3 ) 3 、Fe 2 (SO 4 ) 3 、FeCl 2 And FeCl 3 Any one of them; the nickel salt is Ni (NO) 3 ) 2 、NiSO 4 And NiCl 2 Any one of the following.
4. The method for preparing iron-doped trinickel disulfide material according to claim 2, wherein in the step S1, the concentration of nickel or iron ions in the solution a ranges from 10 to 60mmol/L; the concentration range of the N, N-dimethyl imidazole in the solution B is 100-600 mmol/L.
5. The method for preparing the iron-doped trinickel disulfide material according to claim 2, wherein in the step S4, the conductive substrate is any one of metal nickel foam, metal nickel mesh, metal nickel felt, stainless steel felt, metal nickel iron foam, metal copper foil, metal copper foam, metal iron foam, metal titanium mesh, carbon cloth, carbon paper, graphite felt, carbon fiber, and carbon material after calcination of various shells and mollusk shells.
6. The method for preparing iron-doped trinickel disulfide material according to claim 2, wherein in the step S4, the hydrothermal temperature is 100-200 ℃ and the hydrothermal reaction time is 4-14 h.
7. An iron-doped trinickel disulfide material according to claim 1 for use in an oxidation reaction of alkaline water or alkaline seawater.
8. The application according to claim 7, wherein the specific application method is: the iron-doped trinickel disulfide material is placed in an alkaline system to be used as an oxygen evolution electrode for the oxidation reaction of alkaline water and alkaline seawater.
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