CN114774975B - Preparation method of two-phase nickel selenide compound - Google Patents
Preparation method of two-phase nickel selenide compound Download PDFInfo
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- CN114774975B CN114774975B CN202210477024.0A CN202210477024A CN114774975B CN 114774975 B CN114774975 B CN 114774975B CN 202210477024 A CN202210477024 A CN 202210477024A CN 114774975 B CN114774975 B CN 114774975B
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a preparation method of a two-phase nickel selenide compound, which comprises the steps of preparing a precursor by adopting a hydrothermal method, performing controllable phosphating treatment and the like. The preparation method of the two-phase nickel selenide compound has excellent electrocatalytic hydrogen evolution performance.
Description
Technical Field
The invention relates to a preparation method of a two-phase nickel selenide compound.
Technical Field
The vast majority of hydrogen production today relies on coal to produce hydrogen and natural gas to produce hydrogen. In the current situation of global fossil resource reduction, the most widespread water resource on earth is a desirable strategy for producing hydrogen. In the prior art, electrocatalytic decomposition of water to produce hydrogen is an effective method in large-scale hydrogen production. The electrolysis of water requires the use of an electrocatalyst. From the point of view of electrocatalyst, noble metal Pt is the most efficient electrocatalyst for hydrogen production by water electrolysis. However, it is costly, making it impractical for large scale applications. Thus, the current research is mainly focused on developing low-cost electrocatalysts with high catalytic activity.
Single-component electrocatalysts tend to have limited activity, whereas constructing two-component electrocatalysts can combine the properties of the different components and thus have attracted much research attention. The existing preparation of two-component electrocatalysts, especially two-component electrocatalysts of the same molecular formula and different crystal structures, still has a great chance. It was often unexpectedly found during the course of the experiment that the product was a two-component electrocatalyst. There is therefore a need to provide more cases of preparation methods that provide a hint to the preparation of two-component electrocatalysts.
Disclosure of Invention
The invention aims to provide a preparation method of a two-phase nickel selenide compound.
The preparation method of the two-phase nickel selenide compound is characterized by comprising the following steps: 4mmol Se powder and 5mmol NaBH 4 Dissolving in 65mL of DMF solution, and stirring for 60 minutes to obtain a mixed solution A; 3.4mmol of NiCl was then added 2 ×6H 2 Adding O into the mixed solution A, and stirring for 30 minutes to obtain a mixed solution B; transferring the mixed solution B into a reaction kettle with the volume of 100 mL; tightly sealing the reaction kettle and preserving heat for 24 hours at 160 ℃; natural coolingAfter reaching room temperature, collecting the precipitate therein and centrifugally cleaning the precipitate with deionized water for 3 times; centrifuging and cleaning with absolute ethyl alcohol for 2 times; the product is put into a baking oven at 60 ℃ to be dried for 6 hours, and the precursor Ni is obtained 0.85 Se; weighing 100mg of the precursor, dispersing the precursor in a quartz boat A, and placing the quartz boat A at a downstream position of the airflow in a tube furnace; weigh 1g of NaH 2 PO 2 Placing the quartz boat B in an upstream position of the air flow in the tube furnace; the gas flow is argon; the heating rate of the tube furnace is 2 ℃/min, and the heat is preserved for 1h after the temperature is increased to 350 ℃; and after naturally cooling to room temperature, closing the air flow and taking out the product in the quartz boat A to obtain the two-phase nickel selenide compound.
Compared with the prior art, the sample provided by the invention has the following advantages: the prepared electrocatalyst has excellent performance and simple preparation process.
Drawings
FIG. 1 is an X-ray diffraction pattern of a sample of an example.
FIG. 2 is a linear voltammogram of a sample of the example.
Detailed Description
The implementation of the present invention will be described in detail below with reference to specific embodiments.
The preparation method of the two-phase nickel selenide compound is characterized by comprising the following steps: 4mmol Se powder and 5mmol NaBH 4 Dissolving in 65mL of DMF solution, and stirring for 60 minutes to obtain a mixed solution A; 3.4mmol of NiCl was then added 2 ×6H 2 Adding O into the mixed solution A, and stirring for 30 minutes to obtain a mixed solution B; transferring the mixed solution B into a reaction kettle with the volume of 100 mL; tightly sealing the reaction kettle and preserving heat for 24 hours at 160 ℃; naturally cooling to room temperature, collecting precipitate, and centrifugally cleaning with deionized water for 3 times; centrifuging and cleaning with absolute ethyl alcohol for 2 times; the product is put into a baking oven at 60 ℃ to be dried for 6 hours, and the precursor Ni is obtained 0.85 Se; weighing 100mg of the precursor, dispersing the precursor in a quartz boat A, and placing the quartz boat A at a downstream position of the airflow in a tube furnace; weigh 1g of NaH 2 PO 2 Placing the quartz boat B in a tubeAn upstream location of the gas flow in the furnace; the gas flow is argon; the heating rate of the tube furnace is 2 ℃/min, and the heat is preserved for 1h after the temperature is increased to 350 ℃; and after naturally cooling to room temperature, closing the air flow and taking out the product in the quartz boat A to obtain the two-phase nickel selenide compound.
To illustrate the technical effect of this example, the example samples were characterized. Figure 1 is an XRD pattern of a sample of the example. For the example samples, it can be seen that the diffraction peaks of the samples are compared with the cubic phase NiSe 2 (PDF # 65-1843) and orthorhombic NiSe 2 Standard data matching for (PDF # 18-0886) indicated that the resulting product was a two-phase nickel selenide complex. It is particularly pointed out that the use of NaH for precursors is reported in the literature 2 PO 2 The products obtained by phosphating the starting materials are generally single phosphides (see hongcao Yanget alNano Lett.2015, 15, 7616-7620) or a complex of several phosphides (see Qian Zhouet alSmall 2021, 2105642) as well as a few as the inventors in the literature (Shijie Shenet alReported in adv. Mate. 2022, 34, 2110631) are selenide and phosphide complexes. No document reports that a two-phase selenide complex is obtained by such a treatment, and thus the present invention achieves unexpected technical effects.
The electrocatalytic hydrogen evolution overpotential of the example samples was tested with a 0.5M sulfuric acid solution as electrolyte. FIG. 2 is a linear voltammogram of a sample of the example from which it can be seen that the electrocatalytic hydrogen evolution overpotential (10 mA/cm 2 At) was 161mV. And literature (InHye Kwaket alACS appl. Mater. Interfaces 2016, 8, 5327-5334) of NiSe of single composition 2 Compared (10 mA/cm) 2 The overpotential at 190 mV) the overpotential for the sample of this example is significantly smaller. Furthermore, and literature (Bo Yuet alNi reported in Electrochimica Acta 242 (2017) 25-30) 0.85 Se phase (10 mA/cm) 2 The overpotential is between about 240mV and 280 mV), the overpotential for the sample of this example is also significantly smaller. Thus, the excellent electrocatalytic hydrogen evolution performance of the samples of this example was demonstrated.
It should be noted that what has been described above is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It will be appreciated that other modifications and variations, which may be directly derived or contemplated by those skilled in the art, are deemed to be within the scope of the present invention without departing from the essential concept thereof.
Claims (3)
1. The preparation method of the two-phase nickel selenide compound is characterized by comprising the following steps: 4mmol Se powder and 5mmol NaBH 4 Dissolving in 65mL of DMF solution, and stirring for 60 minutes to obtain a mixed solution A; 3.4mmol of NiCl was then added 2 ·6H 2 Adding O into the mixed solution A, and stirring for 30 minutes to obtain a mixed solution B; transferring the mixed solution B into a reaction kettle with the volume of 100 mL; tightly sealing the reaction kettle and preserving heat for 24 hours at 160 ℃; naturally cooling to room temperature, collecting precipitate, and centrifugally cleaning with deionized water for 3 times; centrifuging and cleaning with absolute ethyl alcohol for 2 times; the product is put into a baking oven at 60 ℃ to be dried for 6 hours, and the precursor Ni is obtained 0.85 Se; weighing 100mg of the precursor, dispersing the precursor in a quartz boat A, and placing the quartz boat A at a downstream position of the airflow in a tube furnace; weigh 1g of NaH 2 PO 2 Placing the quartz boat B in an upstream position of the air flow in the tube furnace; the gas flow is argon; the heating rate of the tube furnace is 2 ℃/min, and the heat is preserved for 1h after the temperature is increased to 350 ℃; and after naturally cooling to room temperature, closing the air flow and taking out the product in the quartz boat A to obtain the two-phase nickel selenide compound.
2. A two-phase nickel selenide composite prepared according to the method of claim 1.
3. Use of a two-phase nickel selenide compound according to claim 2 in the field of electrocatalytic hydrogen evolution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112138701A (en) * | 2020-10-20 | 2020-12-29 | 中国石油大学(华东) | Ni0.85Preparation method of Se @ NC electro-catalytic material |
| CN112456473B (en) * | 2020-12-21 | 2022-06-03 | 台州学院 | Preparation method of two-phase NiSe 2/carbon nanotube composite |
| CN112619670B (en) * | 2020-12-22 | 2021-11-16 | 台州学院 | Preparation method of Ni85Se 100/carbon nanotube composite |
| CN113201753A (en) * | 2021-04-23 | 2021-08-03 | 江苏大学 | Preparation method of phosphorus-doped nickel selenide and application of phosphorus-doped nickel selenide in water electrolysis catalyst |
| CN113604830B (en) * | 2021-06-22 | 2022-12-20 | 西安航空学院 | NiSe with micro-nano double-stage holes and high structural stability 2 -CoSe 2 /CFs composite material and preparation thereof |
| CN113846352B (en) * | 2021-11-29 | 2022-08-30 | 台州学院 | Preparation method of crystalline orthorhombic phase cobalt diselenide amorphous cobalt phosphide heterojunction |
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Non-Patent Citations (2)
| Title |
|---|
| "Nanocrystalline Ni0.85Se as Efficient Non-noble-metal Electrocatalyst for Hydrogen Evolution Reaction";Yu, Bo 等;《ELECTROCHIMICA ACTA》;第242卷;第25-30页 * |
| "硫化镍复合碳纳米纤维的制备及其电催化析氢性能";韦悦 等;《现代纺织技术》;第81-88、128页 * |
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