CN112479274A - Ni3S4-NiS2-FeS2Preparation method of nanosheet - Google Patents
Ni3S4-NiS2-FeS2Preparation method of nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 8
- 229910052960 marcasite Inorganic materials 0.000 claims abstract description 24
- 229910052683 pyrite Inorganic materials 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 241000080590 Niso Species 0.000 claims description 5
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 20
- 239000000203 mixture Substances 0.000 description 9
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 239000004201 L-cysteine Substances 0.000 description 1
- 235000013878 L-cysteine Nutrition 0.000 description 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- 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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Abstract
The invention relates to Ni3S4‑NiS2‑FeS2Preparation method of nano-sheet, in particular to NiSO4·6H2O、FeCl3·6H2O, copper reagent C5H10NS2Na·3H2O is used as a precursor, and Ni is synthesized by hydrothermal synthesis3S4‑NiS2‑FeS2Nanosheets, the Ni3S4‑NiS2‑FeS2The nano-sheet can efficiently catalyze the water oxidation reaction at room temperature.
Description
Technical Field
The invention relates to Ni3S4-NiS2-FeS2A preparation method of a nano-sheet, belonging to the field of material preparation.
Background
Transition metal sulfides are hot spots of research due to their complex structural types and valence states. Nickel sulfide, FeS2The content of the catalyst in the crust is rich, and the catalyst has excellent catalytic performance. Because of different Ni and S metering ratio, different synthesis method and different nickel sulfide composition, at present, Ni is mainly used3S2、NiS、Ni7S6、Ni3S4、NiS2And (c) a compound such as a quaternary ammonium compound. FeS2Low conductivity is highly desirableModulate the surface composition and change the performance. Modulation of FeS by nickel sulfide2The method has important significance in exploring the synthetic route.
The solvothermal method and the high-temperature roasting method become modulation and construction of nickel sulfide-FeS due to simple and convenient operation and easy control2Important methods of materials. For example: chen et al react with Ni2FeO4/FeNi3The nitrogen-doped carbon hybrid and the S powder are roasted for 1h at 350 ℃ to obtain NiS2/FeS2Nitrogen-doped carbon nanorods (Journal of Power Sources,2019,436,226857). Sun et al use NiCl2·6H2O、FeCl2·4H2O、Na2S2O3·5H2O, PVP takes the raw material as the raw material, and synthesizes NiS doped with Fe by hydrothermal for 12h at 150 DEG C2Octahedron (Electrochimica Acta,2018,284, 24-29). Xi et al use NiFe2O4The nanocrystalline and the S powder are used as precursors to be roasted for 2h at 500 ℃, and the obtained product is centrifugally separated at different rotating speeds to obtain FeS2/NiS2Nanocrystals (Chinese Journal of Catalysis,2019,40, 43-51). Currently constructed nickel sulfide/FeS2Relatively few reports of materials are reported, while there is more literature on constructing different nickel sulfide composites or heterojunctions. For example: jiano et al utilize Ni (CH)3COO)2·4H2Performing hydrothermal reaction on O, CTAB and L-cysteine serving as precursors at 220 ℃ for 24h to obtain Ni3S2/NiS@Ni3S4Hollow microspheres (Electrochimica Acta,2018,283, 664) 675). Therefore, different nickel sulfide and FeS are synthesized by using a new path2It is very important to compound and modulate the composition of the transition metal sulfide.
The electrocatalytic oxidation of water to produce oxygen is an important half reaction for decomposing water, and has wide application prospect due to the advantages of mild conditions, high efficiency of atoms and the like. Modulation of different nickel sulfide and FeS2The composite catalyst has important research prospect for high-efficiency catalytic water oxidation.
The invention content is as follows:
the invention aims to provide Ni3S4-NiS2-FeS2A preparation method of the nano-sheet and application thereof in electrocatalytic water oxidation reaction.
Based on the above purpose, the technical scheme of the invention is as follows:
1)Ni3S4-NiS2-FeS2the preparation process of the nanosheet comprises the following steps: adding 50-270 mg of NiSO into a beaker4·6H2O，0.4～0.6g FeCl3·6H2O, 0.4-0.6g of copper reagent (C)5H10NS2Na·3H2O) and 40-80mL of water are stirred until the solution is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at the temperature of 220-260 ℃ for 6-24 h, then the solution is naturally cooled to room temperature, and the product is centrifugally washed and dried to obtain Ni3S4-NiS2-FeS2Nanosheets.
2) Mixing Ni3S4-NiS2-FeS2The nano-sheet is used for electrocatalysis water oxidation reaction at room temperature. The current density is 10mA/cm at a voltage of 1.48V2。
The invention has the following advantages:
1) by using NiSO4·6H2O，FeCl3·6H2O, copper reagent (C)5H10NS2Na·3H2O) as precursor, hydrothermally synthesizing Ni3S4-NiS2-FeS2The nano sheet effectively expands Ni3S4-NiS2-FeS2A method for preparing nano material.
2) The method has the characteristics of simplicity, high efficiency and low cost.
Description of the drawings:
FIG. 1 is Ni3S4-NiS2-FeS2Characterization results of the nanosheets, (a) XRD and (b-c) electron microscope pictures.
Detailed Description
The following examples are intended to further illustrate the invention but are not intended to limit the invention thereto.
Example 1
Ni3S4-NiS2-FeS2The specific preparation process of the nanosheet is as follows: adding 120mg of NiSO into a beaker4·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 2
Adding 56mg of NiSO into a beaker4·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 3
Adding 270mg NiSO into a beaker4·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 4
80 μ L of the homogeneous slurry from example 1 was applied dropwise to a thickness of 1X 1cm2On a foamed Nickel (NF) electrode, after being dried, the water oxidation performance of the electrode is measured on a CHI760E electrochemical workstation, and the electrolyte is 1.0mol/L KOH solution. The current density is 10mA/cm at a voltage of 1.48V2。
Claims (2)
1. Ni3S4-NiS2-FeS2Preparation method of nano-sheet, in particular to NiSO4·6H2O、FeCl3·6H2O, copper reagent C5H10NS2Na·3H2O is used as a precursor, and Ni is synthesized by hydrothermal synthesis3S4-NiS2-FeS2Nanosheets, the Ni3S4-NiS2-FeS2The nano-sheet can efficiently catalyze the water oxidation reaction at room temperature; ni3S4-NiS2-FeS2The nanosheet is prepared by the following steps: adding 50-270 mg of NiSO into a beaker4·6H2O，0.4～0.6g FeCl3·6H2O, 0.4-0.6g of copper reagent C5H10NS2Na·3H2Stirring O and 40-80mL of water until the O and the water are dissolved, transferring the obtained liquid into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at the temperature of 220-260 ℃ for 6-24 h, then naturally cooling to room temperature, centrifugally washing the product, and drying to obtain Ni3S4-NiS2-FeS2Nanosheets.
2. The method of claim 1, wherein:
mixing Ni3S4-NiS2-FeS2The nano-sheet is used for electrocatalysis water oxidation reaction at room temperature. The current density is 10mA/cm at a voltage of 1.48V2。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113830837A (en) * | 2021-09-26 | 2021-12-24 | 青岛科技大学 | FeS with defect sites on surface2/Fe7S8Method for preparing heterojunction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261491A (en) * | 2014-10-10 | 2015-01-07 | 湘潭大学 | Method for synthesizing high-purity nickel disulfide |
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN110918103A (en) * | 2019-12-24 | 2020-03-27 | 济南大学 | Composite electrocatalyst and preparation method and application thereof |
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- 2020-08-26 CN CN202010868507.4A patent/CN112479274B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261491A (en) * | 2014-10-10 | 2015-01-07 | 湘潭大学 | Method for synthesizing high-purity nickel disulfide |
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN110918103A (en) * | 2019-12-24 | 2020-03-27 | 济南大学 | Composite electrocatalyst and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| WENPIN WANG ET. AL.: "Novel (Ni, Fe)S2/(Ni, Fe)3S4 solid solution hybrid: an efficient electrocatalyst with robust oxygen-evolving performance", 《SCIENCE CHINA CHEMISTRY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113830837A (en) * | 2021-09-26 | 2021-12-24 | 青岛科技大学 | FeS with defect sites on surface2/Fe7S8Method for preparing heterojunction |
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