Preparation method and application of nickel-doped pyrrhotite FeS nanoparticles

A nanoparticle and pyrrhotite technology, applied in chemical instruments and methods, physical/chemical process catalysts, structural parts, etc., can solve the problems of increasing synthesis cost and time, and achieve controllable shape, simple operation, and size uniform effect

Pending Publication Date: 2020-12-15
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the synthesis of iron-sulfur compounds requires purified fin

Method used

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  • Preparation method and application of nickel-doped pyrrhotite FeS nanoparticles
  • Preparation method and application of nickel-doped pyrrhotite FeS nanoparticles
  • Preparation method and application of nickel-doped pyrrhotite FeS nanoparticles

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preparation example Construction

[0035] Such as figure 1 As shown, the preparation method of the nickel-doped pyrrhotite FeS nanoparticles provided by the invention comprises the following steps:

[0036] S101: Dissolving sulfur powder and nickel acetate in an organic solvent under nitrogen protection, stirring for several minutes, adding iron pentacarbonyl dropwise;

[0037] S102: After continuing to stir the mixture at room temperature for a period of time, the mixture is transferred to a stainless steel high-pressure reactor, and the reactor is placed in an oven to keep warm for a period of time and then cooled;

[0038] S103: After the reactor was cooled to room temperature, the mixture was centrifuged and washed to obtain a black precipitate, which was ultrasonically treated and washed several times with absolute ethanol and water; dried in a freeze dryer to obtain nickel-doped pyrrhotite FeS nanoparticles.

[0039] The preparation method of nickel-doped FeS nanoparticles provided in the embodiments of t...

Embodiment 1

[0050] The preparation method of the nickel-doped FeS nanoparticle provided by the embodiment of the present invention comprises the following steps: firstly, 0.33 g of sublimed sulfur powder is dissolved in 35 mL of organic solvent with 40 mg; 80 mg; 160 mg of nickel acetate under nitrogen protection, And stir well. Then, 1 mL of iron pentacarbonyl was added dropwise under nitrogen protection. Then, the mixture was magnetically stirred rapidly at room temperature for 20 min, and then the mixture was transferred to a stainless steel autoclave, and the autoclave was placed in an oven at 210 ° C. Keep it for 16 hours; finally, after the temperature of the autoclave is cooled to room temperature, the mixture is centrifuged and washed to obtain a black precipitate. The above black precipitate is ultrasonically dispersed, washed alternately with absolute ethanol and water several times, and finally collected by centrifugation. , and dried in a vacuum freeze dryer for 2 hours to obt...

Embodiment 2

[0052] The preparation method of the nickel-doped FeS nanoparticle that the example of the present invention provides comprises the following steps: first the sublimation sulfur powder of 0.5g is respectively mixed with 40mg under nitrogen protection; 80mg; 160mg of nickel acetate is dissolved in 35mL organic solvent, and Stir well. Then, 1 mL of iron pentacarbonyl was added dropwise under nitrogen protection. Then, the mixture was magnetically stirred rapidly at room temperature for 20 min, and then the mixture was transferred to a stainless steel autoclave, and the autoclave was placed in an oven at 210 ° C. Keep it for 16 hours; finally, after the temperature of the autoclave is cooled to room temperature, the mixture is centrifuged and washed to obtain a black precipitate. The above black precipitate is ultrasonically dispersed, washed alternately with absolute ethanol and water several times, and finally collected by centrifugation. , and dried in a vacuum freeze dryer fo...

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Abstract

The invention belongs to the technical field of electrocatalytic decomposition of water, and discloses a preparation method and application of nickel-doped pyrrhotite FeS nanoparticles. The compound is synthesized by adopting a one-pot method and is applied to the field of electrocatalytic decomposition of water. The preparation method comprises the following steps: dissolving pentacarbonyl iron,sublimed sulfur powder and nickel acetate in a certain amount of organic solvent under the protection of nitrogen, stirring at room temperature for a period of time to fully dissolve pentacarbonyl iron, sublimed sulfur powder and nickel acetate, transferring the solution into a stainless steel high-pressure reaction kettle, putting the reaction kettle into a drying oven, keeping the temperature for a period of time, and cooling; after the reaction kettle is cooled to room temperature, carrying out centrifugal operation on the reaction solution to obtain a black precipitate, carrying out ultrasonic treatment on the obtained black precipitate, and washing the black precipitate with absolute ethyl alcohol and water for multiple times; performing centrifugal collection; and finally, performingvacuum freeze drying to obtain the nickel-doped pyrrhotite FeS nano-catalyst. The required raw materials are cheap and easy to obtain, the preparation method is simple, the cost is low, and the method is expected to play an important role in wider emerging fields.

Description

technical field [0001] The invention belongs to the technical field of electrocatalytic water splitting, and in particular relates to a preparation method and application of nickel-doped pyrrhotite FeS nanoparticles. Background technique [0002] Present: Global energy problems and environmental pollution have prompted intensive research on the development of renewable and clean energy. Electrochemical water splitting is a promising technology for the production of hydrogen, a renewable, safe and environmentally friendly energy source. Electrochemical water splitting offers a feasible route to generate hydrogen, involving two half-reactions, the hydrogen evolution reaction (HER) at the cathode and the oxygen evolution reaction (OER) at the anode. The oxygen evolution reaction (OER) has attracted particular interest. However, the overall efficiency is severely limited by the sluggish kinetics of the four-electron transfer process of OER, resulting in a driving cell voltage ...

Claims

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Application Information

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IPC IPC(8): B01J27/043B01J35/10C25B11/06C25B1/04H01M4/58H01M10/054
CPCB01J27/043B01J35/0033B01J35/1004C25B11/04C25B1/04H01M4/5815H01M10/054Y02E60/36Y02E60/10
Inventor 林健健郑德华荆忠鑫孙蕾周倩男许慧忠
Owner QINGDAO UNIV OF SCI & TECH
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