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Method and application of in-situ electrochemical growth of nano-carbide-based electrocatalytic film on the surface of self-supporting carbon substrate

An in-situ electrochemical, carbon-based technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, can solve problems such as being unsuitable for large-scale engineering applications, and achieve excellent electrocatalytic activity, Excellent electrochemical stability, low reaction temperature effect

Active Publication Date: 2020-08-07
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that powdered electrocatalysts are currently not suitable for large-scale engineering applications.

Method used

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  • Method and application of in-situ electrochemical growth of nano-carbide-based electrocatalytic film on the surface of self-supporting carbon substrate
  • Method and application of in-situ electrochemical growth of nano-carbide-based electrocatalytic film on the surface of self-supporting carbon substrate
  • Method and application of in-situ electrochemical growth of nano-carbide-based electrocatalytic film on the surface of self-supporting carbon substrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Put 300mg of molybdenum disulfide into 300mL of absolute ethanol and ultrasonically disperse for 6 hours with an ultrasonic power of 160W to form a uniform suspension. 2 carbon fiber cloth surface (geometric area is about 18cm 2 ), after drying, a carbon fiber cloth with molybdenum disulfide uniformly loaded on the surface is obtained, and the loading capacity is about 2mg / cm (geo) 2 ; will subsequently carry the MoS 2 The carbon fiber cloth was placed in a crucible, and the temperature was raised to 300 °C at a rate of 5 °C / min under the protection of an argon atmosphere in a tube furnace and maintained for 1 hour.

[0043] (2) After the carbon fiber cloth is cooled naturally, it is fixed on one end of a molybdenum rod (3mm in diameter) with a molybdenum wire as the cathode, and a graphite rod as the anode, and the NaCl-KCl (molar ratio 1:1) molten salt at 700°C In the middle, 2.7V constant tank pressure electrolysis for 1 hour, figure 1 Schematic diagram of th...

Embodiment 2

[0046] (1) Put 300mg of molybdenum disulfide into 150mL of absolute ethanol and ultrasonically disperse for 6 hours with an ultrasonic power of 180W to form a uniform suspension. 2 The surface of the square graphite sheet (excluding the side area, the geometric area of ​​the graphite sheet is about 16cm 2 ), after drying, a graphite sheet uniformly loaded with molybdenum disulfide on the surface is obtained, and the loading capacity is about 5mg / cm (geo) 2 ; will subsequently carry the MoS 2 The graphite sheet was placed in a crucible, and the temperature was raised to 150°C at a rate of 5°C / min under the protection of an argon atmosphere in a tube furnace and maintained for 3 hours.

[0047] (2) After the graphite sheet is cooled naturally, fix it on one end of a molybdenum rod (diameter 3mm) with a molybdenum wire as the cathode, and use the graphite rod as the anode, in NaCl-KCl (molar ratio 1:1) molten salt at 700°C , 2.9V constant tank pressure electrolysis for 45 minu...

Embodiment 3

[0050] (1) Put 300mg of molybdenum disulfide into 150mL of isopropanol and ultrasonically disperse for 6 hours with an ultrasonic power of 180W to form a uniform suspension. cm 3 On the grapefruit peel derived carbon foam (the geometric area of ​​the large grapefruit peel carbon foam is 40cm 2 ), after drying, the grapefruit peel-derived carbon foam with molybdenum disulfide uniformly loaded on the surface was obtained, and the loading capacity was about 1.5mg / cm (geo) 2 ; will subsequently carry the MoS 2 The grapefruit peel-derived carbon foam was placed in a crucible, and the temperature was raised to 260°C at a rate of 3°C / min under the protection of nitrogen atmosphere in a tube furnace and kept for 2h.

[0051] (2) To be loaded with MoS 2 The grapefruit peel-derived carbon foam was cooled naturally, and then fixed on one end of a nickel-chromium rod (5mm in diameter) with a molybdenum wire as the cathode, and a graphite rod as the anode, in 700°C NaCl-KCl (molar rati...

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Abstract

The invention belongs to the technical field of electrocatalytic material preparation, and relates to a method of in-situ electrochemical growth of a nano-carbide-based electrocatalytic film layer onthe surface of a self-supporting carbon matrix and application of the method. The method comprises the following preparation steps that (1), transition metal sulfide powder is dispersed in a solvent to obtain a uniform turbid liquid; (2), a self-supporting carbon matrix is selected, a certain amount of a turbid liquid is fetched and evenly coated on the surface of the selected self-supporting carbon matrix, and drying is carried out; (3), the step (2) carbon matrix is calcined under the protection of inert gases, and cooling is carried out after the calcining; (4), the step (3) treated carbonmatrix is used as a cathode, and an inert electrode is used as an anode, the cathode electrode and the anode electrode are both immersed in molten salt mediums for electrolysis; and (5), after the electrolysis is finished, cathode products are subjected to washing and drying. According to the method of the in-situ electrochemical growth of the nano-carbide-based electrocatalytic film layer on thesurface of the self-supporting carbon matrix and the application of the method, the transition metal sulfide is used as a metal source to transform the transition metal sulfide into uniformly distributed, highly adhering and granular metal carbide nano-particles on the surface of the self-supporting carbon matrix in an efficient and in-situ electrochemical mode.

Description

technical field [0001] The invention belongs to the technical field of electrocatalytic material preparation and also belongs to the field of material surface engineering, and relates to a method and application of in-situ electrochemical growth of nano carbide-based electrocatalytic film on the surface of a self-supporting carbon matrix. Background technique [0002] Transition metal carbides (such as dimolybdenum carbide, tungsten carbide, etc.) are widely used in industries such as machining, mineral mining, and temperature and wear resistance. Since transition metal carbides mostly have a d-band electronic structure similar to that of platinum group metals, they exhibit platinum-like electrocatalytic properties, and thus have been widely used in catalytic hydrogenation reactions, electrocatalytic hydrogen production, electrocatalytic oxygen reduction and electrocatalysis. catalytic CO 2 Restoration etc. [0003] However, although according to relevant reports, transiti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D5/54C25D9/08C25B11/12C25B11/06B82Y30/00
CPCB82Y30/00C25D5/54C25D9/08C25B11/051C25B11/073
Inventor 汪的华蒋睿熊欣朱华
Owner WUHAN UNIV
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