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Preparation method of WC/WO3 core-shell structure electrocatalyst

An electrocatalyst, core-shell structure technology, applied in structural parts, circuits, electrical components, etc., can solve the problems of tungsten carbide surface area carbon, catalytic ability impact, catalytic performance instability, etc., to reduce surface area carbon and increase carbon defects , Catalytic effect and stable effect

Active Publication Date: 2018-02-16
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Publication No. CN102070143B "A Preparation Method for Mesoporous Hollow Spherical Tungsten Carbide" discloses a one-step solid-phase preparation process of tungsten carbide directly from ammonium metatungstate, and the prepared tungsten carbide has good acid and alkali resistance and good Catalytic performance, but the one-step preparation method is likely to lead to severe carbon on the surface of tungsten carbide, which has a relatively large impact on the subsequent catalytic ability, resulting in unstable catalytic performance

Method used

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  • Preparation method of WC/WO3 core-shell structure electrocatalyst
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  • Preparation method of WC/WO3 core-shell structure electrocatalyst

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Embodiment 1

[0026] A WC / WO of the present invention 3The method for preparing an electrocatalyst with a core-shell structure comprises the following steps: (1) preparing a 10wt% aqueous solution and introducing it into a spray dryer, the flow rate of hot air for spray drying is 600L / h, the feed temperature is 120°C, and the discharge temperature is 70°C , the feeding rate was 10ml / min, and sample A was obtained; put sample A into a muffle furnace for sintering, the sintering temperature was 1100°C, the heating rate was 2°C / min, and the sintering time was 4h, and a hollow mesoporous structure was obtained. WO 3 Microspheres; (2) WO 3 The microspheres were placed in a tubular muffle furnace under CO / H 2 Under the atmosphere, raise the temperature to 750°C at 3°C / min, keep it for 1.5h, and blow the cold air at 10°C on the outside of the tube furnace; let the temperature in the muffle furnace drop to room temperature; then take out the obtained Things are WC / WO 3 intermediate; the CO / H 2...

Embodiment 2

[0034] A WC / WO of the present invention 3 The method for preparing an electrocatalyst with a core-shell structure comprises the following steps: (1) preparing a 40wt% aqueous solution and introducing it into a spray dryer, the flow rate of hot air for spray drying is 1300L / h, the feed temperature is 240°C, and the discharge temperature is 120°C , the feeding rate was 45ml / min, and sample A was obtained; put sample A into a muffle furnace for sintering, the sintering temperature was 1300°C, the heating rate was 4°C / min, and the sintering time was 6h, and a hollow mesoporous structure was obtained. WO 3 Microspheres; (2) WO 3 The microspheres were placed in a tubular muffle furnace under CO / H 2 Under the atmosphere, raise the temperature to 850°C at 5°C / min, keep it for 1.5~2h, and blow the cold air at 15°C on the outside of the tube furnace; let the temperature inside the muffle furnace drop to room temperature; then take it out The result is WC / WO 3 intermediate; the CO / H ...

Embodiment 3

[0042] A WC / WO of the present invention 3 The preparation method of the core-shell structure electrocatalyst comprises the following steps: (1) preparing a 25wt% aqueous solution, and introducing it into a spray dryer, the hot air flow rate of the spray drying is 900L / h, the feed temperature is 180°C, and the discharge temperature is 90°C , the feeding rate was 28ml / min, and sample A was obtained; put sample A into a muffle furnace for sintering, the sintering temperature was 1100-1300°C, the heating rate was 3°C / min, and the sintering time was 5h, and the hollow mesopore was obtained. Structured WO 3 Microspheres; (2) WO 3 The microspheres were placed in a tubular muffle furnace under CO / H 2 Under atmosphere, raise the temperature to 750-850°C at 3-5°C / min, keep it for 2 hours, and blow the cold air at 12°C on the outside of the tube furnace to blow the tube furnace; let the temperature inside the muffle furnace drop to room temperature; Then take out the result is WC / WO ...

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Abstract

The invention provides a WC / WO3 core-shell structure electrocatalyst and a preparation method thereof. The method comprises the following steps: (1) preparing an ammonium metatungstate water solutionto carry out spray granulation so as to obtain a sample A; and sintering the sample A to obtain WO3 microspheres of hollow mesoporous structures; (2) after sintering the WO3 microspheres in a CO2 / H2 atmosphere, cooling with cold wind; and then taking out an obtained product which is a WC / WO3 intermediate; and (3) after putting the WC / WO3 intermediate into vacuum high-purity oxygen for sintering, naturally cooling to obtain the WC / WO3 core-shell structure electrocatalyst. By adopting the ammonium metatungstate precursor, tungsten oxide is firstly prepared at high temperature, and then the particle surface of tungsten oxide is reduced into tungsten carbide to form a core-shell structure, so that the surface is oxidized to remove accumulated carbon on the surface, and the WC / WO3 core-shell structure electrocatalyst of a hollow mesoporous structure is prepared. The catalyst provided by the invention is simple in technology, and the electro-catalytic property for methanol oxidation and oxygen reduction reactions is further improved.

Description

【Technical field】 [0001] The invention belongs to the technical field of electrochemical catalyst synthesis, in particular to a WC / WO 3 Preparation method of core-shell structure electrocatalyst. 【Background technique】 [0002] With the depletion of oil resources and the deterioration of the ecological environment, the development of new energy vehicles to replace traditional fuel vehicles has become a hot research and development field in all countries in the world. Since Toyota Mirai and Hyundai ix30 fuel cell vehicles were introduced to the market in 2016, proton exchange membrane fuel cell (PEMFC) technology has attracted widespread attention. Poisoning and easy oxidation of carbon supports, etc. Therefore, the development of cheap and high-performance fuel cell catalysts has important scientific significance and practical application value. Tungsten carbide (WC) has been extensively studied as a potential alternative catalytic material for Pt-group noble metals. Howe...

Claims

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Application Information

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IPC IPC(8): H01M4/86H01M4/88H01M4/90
CPCH01M4/8657H01M4/88H01M4/90H01M4/9016Y02E60/50
Inventor 周阳
Owner JIANGXI UNIV OF SCI & TECH
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