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Method for preparing boron-and-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound/carbon composite material

A technology of sulfur-oxygen compounds and carbon composite materials, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve unseen problems

Active Publication Date: 2020-08-07
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for preparing boron-and-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound/carbon composite material
  • Method for preparing boron-and-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound/carbon composite material
  • Method for preparing boron-and-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound/carbon composite material

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Embodiment 1

[0024] CoCl 2 ∙ 6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. The carbon paper with basic cobalt salt arrays was placed in the air at 500 °C for 0.5 h, and then in an Ar+S atmosphere at 500 °C for 1 h, cooled naturally and taken out for use. Soak the above-mentioned carbon paper with cobalt sulfide arrays grown in 400 mM molybdenum chloride solution, which is composed of 50 mg bipyridyl, 0.1 g glucose and 3 mL N, N-dimethylformamide, soak for about 1 min, and dried on a hot table at 80°C for 10 min after taking it out. The coated substrate was placed in a tube furnace with Ar as the protective gas and boric acid ...

Embodiment 2

[0027] CoCl 2 ∙ 6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2 The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. The carbon paper with basic cobalt salt arrays was placed in the air at 500 °C for 0.5 h, and then in an Ar+S atmosphere at 500 °C for 1 h, cooled naturally and taken out for use. Soak the above-mentioned carbon paper with cobalt sulfide arrays grown in 400 mM molybdenum chloride solution, which is composed of 50 mg o-phenanthroline, 0.1 g glucose and 3 mL N, N-dimethylformamide, soak After about 1 min, take it out and dry it on a hot table at 80°C for 10 min. Put the coated substrate into a tube furnace, use Ar as the protective gas, and use a solid ...

Embodiment 3

[0030] CoCl 2 ∙ 6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2 The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. The carbon paper with basic cobalt salt arrays was placed in the air at 500 °C for 0.5 h, and then in an Ar+S atmosphere at 500 °C for 1 h, cooled naturally and taken out for use. Soak the above-mentioned carbon paper grown with cobalt sulfide arrays in 400 mM molybdenum chloride solution, which is composed of 50 mg o-phenanthroline, 0.05 g glucose and 3 mL N, N-dimethylformamide, soak After about 1 min, take it out and dry it on a hot table at 80°C for 10 min. Put the coated substrate into a tube furnace, use Ar as the protective gas, and use a solid...

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Abstract

The invention provides a method for preparing a boron-and-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound / carbon composite material. The method comprises the following steps: dissolving a molybdenum salt and a nitrogen carbon source in a volatile non-aqueous solvent to obtain a Mo-N-C precursor solution, coating a substrate, on which a cobalt sulfide array structure grows, with the precursor solution, and carrying out drying; and with Ar or N2 as a shielding gas and a carrier gas and mixed powder of sublimed sulfur element and boric acid as a solid evaporation source, carrying out a chemical vapor deposition reaction to obtain the composite material. According to the invention, sulfur steam formed by evaporation of elemental sulfur and oxygen introduced by decomposition of boric acid react with cobalt sulfide and molybdenum ions to generate a cobalt-molybdenum-sulfur-oxygen compound; nitrogen and carbon are gradually carbonized in a protective atmosphere to form a carbon material; and meanwhile, boron atoms and nitrogen atoms can be respectively doped into the cobalt-molybdenum-sulfur-oxygen compound and the carbon material in a form of replacing sulfur-oxygen atoms or carbon atoms in the CVD reaction process. The boron-nitrogen-doped cobalt-molybdenum-sulfur-oxygen compound / carbon composite material obtained according to a technical scheme of the invention has excellent multifunctional electrocatalytic performance.

Description

technical field [0001] The invention relates to the preparation of composite and doped multi-component multifunctional materials, and its application belongs to the field of energy storage and conversion materials and devices. Background technique [0002] The whole world is actively and urgently looking for and researching renewable clean energy and energy conversion and storage methods. Among them, because the combustion product of hydrogen is water, its new preparation methods (such as: electrocatalytic water splitting to produce hydrogen) have attracted extensive attention. Similarly, Zn-air batteries and fuel cells, as new energy conversion and storage devices, are also eagerly concerned by researchers from various countries due to their many advantages such as rich metal Zn or biofuels, and aqueous electrolytes. However, there is still a long way to go to develop electrocatalysts with high catalytic activity, economical feasibility, and high stability for these device...

Claims

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Application Information

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IPC IPC(8): B01J27/24C25B1/04C25B11/06
CPCB01J27/24C25B1/04C25B11/091B01J35/33Y02E60/36
Inventor 黄妞骆禅闫术芳杨柳孙小华孙盼盼
Owner CHINA THREE GORGES UNIV
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