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Preparation method of sulfur-doped nickel phosphide nano powder and application in electrolysis of water

A nano-powder and nickel phosphide technology, applied in chemical instruments and methods, catalyst activation/preparation, electrolysis process, etc., can solve problems such as large band gap width, large electron transfer resistance, and few active sites

Inactive Publication Date: 2019-09-10
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, transition metals generally have shortcomings such as large band gap width, high electron transfer resistance, and few active sites, making them still face major challenges on the road to becoming an ideal electrocatalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. 40 mL of deionized water was added to a 50 mL polytetrafluoroethylene liner, nickel nitrate (91.3 mg, 0.5 mmol) was added under stirring, and then 2.4 mg of sodium bicarbonate was added to adjust the pH of the reaction solution to 8. Stir rapidly for 10 min. The hydrothermal autoclave was sealed and placed in an oven at 130 °C for 30 h. After natural cooling, deionized water and ethanol were used to centrifugally wash and dry in vacuum to obtain nickel source precursor powder.

[0020] The second step: 50 mg nickel source precursor and 1 g sodium hypophosphite were placed in a tube furnace under N 2 Under gas protection with 2 o C / min heating rate, 300 o C was incubated for 2 h, then cooled naturally, and the product was washed by centrifugation with deionized water, and collected by vacuum drying to ...

Embodiment 2

[0028] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. 40 mL of deionized water was added to a 50 mL polytetrafluoroethylene liner, nickel chloride (64.7 mg, 0.5 mmol) was added under stirring, and then 2.6 mg of sodium bicarbonate was added to adjust the pH of the reaction solution to 8.5. Stir rapidly for 10 min. The hydrothermal autoclave was sealed and placed in an oven at 150 °C for 24 h. After natural cooling, deionized water and ethanol were used to centrifugally wash and dry in vacuum to obtain nickel source precursor powder.

[0029] The second step: 50 mg nickel source precursor and 1 g sodium hypophosphite were placed in a tube furnace under N2 Under gas protection with 2 o C / min heating rate, 400 o C was kept for 3 h, then cooled naturally, the product was centrifuged and washed with deionized water, and collected by vacuum drying to obtain bla...

Embodiment 3

[0037] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. 40 mL of deionized water was added to a 50 mL polytetrafluoroethylene liner, nickel nitrate (137 mg, 0.75 mmol) was added under stirring, and then 2.5 mg of sodium bicarbonate was added to adjust the pH of the reaction solution to 8. Stir rapidly for 10 min. The hydrothermal autoclave was sealed and placed in an oven at 180 °C for 10 h. After natural cooling, deionized water and ethanol were used to centrifugally wash and dry in vacuum to obtain nickel source precursor powder.

[0038] The second step: 50 mg nickel source precursor and 1 g sodium hypophosphite were placed in a tube furnace under N 2 Under gas protection with 2 o C / min heating rate, 500 o C for 4 h, then naturally cooled, the product was centrifuged and washed with deionized water, dried in vacuum and collected to obtain black nickel p...

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Abstract

The invention provides sulfur-doped nickel phosphide nano powder and an application in electrolysis of water. A method of preparing the sulfur-doped nickel phosphide nano powder comprises the following steps: (1) performing pretreatment on a nickel-containing aqueous solution, adjusting pH of the solution, adding an alkali regulating agent to prepare an alkaline pre-reaction solution, performing areaction under heating, after the reaction is completed, performing washing, performing centrifugation, and performing collection to obtain nickel source precursor powder; (2) performing calcinationtreatment on the nickel source precursor and a phosphating reagent according to a ratio under the protection of an inert gas to obtain nickel phosphide; and (3) performing calcination treatment on thenickel phosphide and a sulfur source under the protection of an inert gas, and performing collection to obtain the black sulphur-doped nickel phosphide powder. The sulfur-doped nickel phosphide provided by the invention has excellent catalytic performance when used for electrocatalysis of an oxygen evolution reaction (OER), has overpotential as low as 0.294 V (relative to a standard hydrogen electrode) and a Tafel slope as low as 58 mV / dec.

Description

technical field [0001] The invention relates to the field of preparation and application of inorganic nano powders, in particular to a calcination method for preparing sulfur-doped nickel phosphide nano powders and its application in electrolyzing water. Background technique [0002] Energy is very important to promote national development and improve people's living standards. The most widely used energy is carbon-containing traditional fossil fuels, which provide most of the world's energy. However, the use of fossil fuels will cause energy waste and even lead to There is an energy crisis phenomenon; at the same time, the combustion of fossil fuels can produce some pollutants and cause serious pollution to the environment on which human beings depend. With the enhancement of people's awareness of environmental protection, the development of clean, efficient and renewable new energy has become the focus of current research. Due to the intermittent, unstable, regional and o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/00B01J37/10B01J37/20C25B1/04C25B11/06
CPCB01J27/1853B01J37/20B01J37/10C25B1/04C25B11/075B01J35/23B01J35/33Y02E60/36
Inventor 孙旭马晓晶高令峰郭成英魏琴
Owner UNIV OF JINAN
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