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Preparation method of chromium-doped cobalt phosphide nanorod array growing on carbon cloth in situ

A nanorod array and in-situ growth technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the difficulty of increasing high-performance electrodes, cannot meet large-scale production, low efficiency, etc. problems, to achieve the effect of regular arrangement, easy control of reaction conditions, and avoidance of pollution

Pending Publication Date: 2021-04-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional electrode preparation method is affected by factors such as the dispersion effect of cobalt phosphide particles in the solvent, the addition ratio of ionic polymers, and the uniformity of cobalt phosphide particles loaded on the electrode, which increases the difficulty of preparing high-performance electrodes, and The operation is cumbersome and inefficient, which cannot meet the needs of mass production

Method used

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  • Preparation method of chromium-doped cobalt phosphide nanorod array growing on carbon cloth in situ
  • Preparation method of chromium-doped cobalt phosphide nanorod array growing on carbon cloth in situ
  • Preparation method of chromium-doped cobalt phosphide nanorod array growing on carbon cloth in situ

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] (01) Cut the carbon cloth into a size of 1cm-3cm, soak it in a 6mol / L nitric acid solution, and heat it in an oil bath at 90°C for 6h.

[0067] (02) Stop heating and cool to room temperature, take out the carbon cloth, and sonicate in 60 mL of acetone, 80 mL of ultrapure water, and 60 mL of ethanol for 30 mins.

[0068] (03) Take out the sonicated carbon cloth and place it in an oven at 65°C for 4 hours to obtain a clean, dry carbon cloth with enhanced hydrophilicity.

[0069] (04) 0.565g of Co(NO 3 ) 2 ·6H 2 O, 0.024g of Cr(NO 3 ) 3 9H 2 O, 0.6g of CO(NH 2 ) 2 , 0.186g of NH 4 F was dissolved in 20mL ultrapure water and stirred at room temperature for 1.5h to obtain a pale pink transparent solution.

[0070] (05) Transfer the light pink transparent solution obtained in step (04) to the polytetrafluoroethylene reactor lining, put a piece of clean, dry, and hydrophilic carbon cloth obtained in step (03) vertically, cover The lid is put into the steel pressure j...

Embodiment 2

[0081] (01) Cut the carbon cloth into a size of 1cm-3cm, soak it in 8mol / L nitric acid solution, and heat it in an oil bath at 85°C for 6h.

[0082] (02) Stop heating and cool to room temperature, take out the carbon cloth, and sonicate in 60 mL of acetone, 80 mL of ultrapure water, and 60 mL of ethanol for 30 mins.

[0083] (03) Take out the sonicated carbon cloth and place it in an oven at 65°C for 4 hours to obtain a clean, dry carbon cloth with enhanced hydrophilicity.

[0084] (04) 0.553g of Co(NO 3 ) 2 ·6H 2 O, 0.040g of Cr(NO 3 ) 3 9H 2 O, 0.6g of CO(NH 2 ) 2 , 0.186g of NH 4 F was dissolved in 20mL ultrapure water and stirred at room temperature for 1.5h to obtain a pink transparent solution.

[0085] (05) Transfer the pink transparent solution obtained in step (04) to the inner lining of the polytetrafluoroethylene reactor, put a piece of clean, dry, and hydrophilic carbon cloth obtained in step (03) vertically, and cover it The lid is placed into the steel ...

Embodiment 3

[0096] (01) Cut the carbon cloth into a size of 1cm-3cm, soak it in a 6mol / L nitric acid solution, and heat it in an oil bath at 90°C for 8h.

[0097] (02) Stop heating and cool to room temperature, take out the carbon cloth, and sonicate in 70 mL of acetone, 100 mL of ultrapure water, and 70 mL of ethanol for 50 mins.

[0098] (03) Take out the sonicated carbon cloth and place it in an oven at 65°C for 4 hours to obtain a clean, dry carbon cloth with enhanced hydrophilicity.

[0099] (04) 0.541g of Co(NO 3 ) 2 ·6H 2 O, 0.056g of Cr(NO 3 ) 3 9H 2 O, 0.6g of CO(NH 2 ) 2 , 0.186g of NH 4 F was dissolved in 20 mL of ultrapure water and stirred at room temperature for 2 h to obtain a dark pink transparent solution.

[0100] (05) Transfer the dark pink transparent solution obtained in step (04) to the polytetrafluoroethylene reactor liner, put a piece of clean, dry, hydrophilic carbon cloth obtained in step (03) vertically, cover The lid is put into the steel pressure jac...

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Abstract

The invention aims to provide a preparation method of a chromium-doped cobalt phosphide nanorod array growing on carbon cloth in situ, which comprises the following specific steps of oxidizing the carbon cloth in nitric acid to enhance the hydrophilicity of the carbon cloth, and growing a layer of precursor CrxCo1-x(OH)F / CC on the carbon cloth in situ by a hydrothermal method, finally, converting the precursor growing on the carbon cloth into chromium-doped cobalt phosphide CrxCo1-x(OH)F / CC through a high-temperature gas-phase phosphating method. The preparation process is simple to operate, easy to control and low in cost and can be used for large-scale production, the chromium-doped cobalt phosphide nanorod array which grows on the carbon cloth in situ and is prepared by adopting the method is uniform in distribution and close in arrangement, the rod-like particle size reaches the nanoscale and is uniform in particle size, and the CoP crystal form is reserved while the free energy of hydrogen adsorption is reduced by chromium doping; the hydrogen evolution reaction can be efficiently, continuously and stably catalyzed.

Description

technical field [0001] The invention belongs to the technical field of preparation of micro-nano materials, and in particular relates to the preparation of a chromium-doped cobalt phosphide nanorod array grown on carbon cloth in situ. Background technique [0002] The traditional energy structure dominated by fossil fuels is experiencing the double crisis of resource depletion and environmental pollution. Human development urgently needs to solve the two major challenges of energy and environmental problems, forcing people to develop efficient, clean and sustainable green energy. As a clean energy with high energy density, wide sources, easy storage, and only water as a combustion product, hydrogen energy is expected to replace fossil fuels. Among various hydrogen production methods, hydrogen production by electrocatalytic water splitting has the advantages of wide sources of raw materials and various forms of energy utilization, and has gradually become a hot spot in curren...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J35/06C25B1/04C25B11/054C25B11/056C25B11/065C25B11/091
CPCY02E60/36
Inventor 庄仲滨张立鹏张俊涛
Owner BEIJING UNIV OF CHEM TECH
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