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Co-CoOx/NMC (nitrogen-doped mesoporous carbon supported cobalt-cobalt oxide) nanocomposite material and preparation method and application thereof

A nitrogen-doped mesoporous carbon and nanocomposite technology is applied in the preparation/purification of carbon, cobalt oxide/cobalt hydroxide, nanotechnology, etc. It can improve the performance of electrocatalytic oxygen reduction, easy operation and low cost.

Inactive Publication Date: 2017-09-19
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The impregnation method is the most traditional preparation method. This method is simple to operate, but the bonding force between the two phases of the composite material is poor, and the metal active components are easily agglomerated or lost; This method can obtain a stable structure, but the operation method is complicated, which is not conducive to large-scale production; the one-pot method refers to fully mixing the carbon source, template agent and metal precursor, and roasting at high temperature , Removing templates to obtain mesoporous carbon materials containing metal components, this method is simple to operate, short synthesis cycle, and easy for large-scale production

Method used

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  • Co-CoOx/NMC (nitrogen-doped mesoporous carbon supported cobalt-cobalt oxide) nanocomposite material and preparation method and application thereof
  • Co-CoOx/NMC (nitrogen-doped mesoporous carbon supported cobalt-cobalt oxide) nanocomposite material and preparation method and application thereof
  • Co-CoOx/NMC (nitrogen-doped mesoporous carbon supported cobalt-cobalt oxide) nanocomposite material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] At room temperature, fully dissolve 0.24mmol triblock copolymer F127, 10mmol 3-aminophenol, 5mmol urotropine and 19mmol ammonia water in 52ml of water, stir well, heat in an oil bath at 80°C, condense and reflux and stir for 24h to make it Fully polymerize; naturally cool down after polymerization, settle, wash with water to collect the product, and dry overnight in a vacuum oven at 40°C; after drying, heat up to 350°C at a heating rate of 1°C / min for calcination in a high-temperature tube furnace under an Ar gas atmosphere 1h, then raised to 600°C at the same heating rate and then calcined for 3h, and the mesoporous carbon was obtained after natural cooling, denoted as NMC-600 (see figure 1 with 2 ).

[0035] Depend on figure 1 with 2 It can be seen that the mesoporous carbon NMC-600 is an amorphous material with a spherical shape and a uniform mesoporous structure.

Embodiment 2

[0037] At room temperature, fully dissolve 0.24mmol triblock copolymer F127, 10mmol 3-aminophenol, 5mmol urotropine, 0.6mmol Co(NO 3 ) 2 ·6H 2O and 19 mmol of ammonia water, stirred thoroughly, heated in an oil bath at 80°C, condensed and refluxed and stirred for 24 hours to fully polymerize; after polymerization, the temperature was naturally lowered, the product was collected by sedimentation, washed with water, and dried overnight in a vacuum oven at 40°C; after drying In a high-temperature tube furnace under an Ar gas atmosphere, heat up to 350°C at a rate of 1°C / min for calcination for 1 hour, then raise the temperature to 600°C for 3 hours at the same rate, and then naturally cool down to obtain nitrogen-doped mesoporous carbon Loaded cobalt-cobalt oxide nanocomposites, denoted as Co-CoO x -1 / NMC-600 (see image 3 with 4 ).

[0038] Depend on image 3 It can be seen that the composite Co-CoO x The characteristic diffraction peaks of Co and CoO appeared in the XRD ...

Embodiment 3

[0040] At room temperature, fully dissolve 0.24mmol triblock copolymer F127, 10mmol 3-aminophenol, 5mmol urotropine, 1.2mmol Co(NO 3 ) 2 ·6H 2 O and 19 mmol of ammonia water, stirred thoroughly, heated in an oil bath at 80°C, condensed and refluxed and stirred for 24 hours to fully polymerize; after polymerization, the temperature was naturally lowered, the product was collected by sedimentation, washed with water, and dried overnight in a vacuum oven at 40°C; after drying In a high-temperature tube furnace under an Ar gas atmosphere, the temperature was raised to 350°C for 1 hour at a heating rate of 1°C / min, and then calcined for 3 hours at the same heating rate to 600°C, and nitrogen-doped mesoporous pores were obtained after natural cooling. Carbon-supported cobalt-cobalt oxide nanocomposites, denoted as Co-CoO x -2 / NMC-600 (see Figure 5 , 6 , 7, 8 and 9).

[0041] Depend on Figure 5 It can be seen that the composite Co-CoO x The characteristic diffraction peaks o...

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Abstract

The invention belongs to the field of electrode material preparation, and specifically relates to a preparation method and application of a Co-CoOx / NMC (nitrogen-doped mesoporous carbon supported cobalt-cobalt oxide) nanocomposite material. The composite material is prepared by utilization of a one-pot process and by means of the following steps of adding cobalt salt during a process of forming aminated mesoporous polymers and performing pyrolysis, wherein Co-CoOx particles are uniformly dispersed on a mesoporous carbon skeleton, and the particle diameter of the Co-CoOx particles is 10 to 20nm. The composite material disclosed by the invention has the advantages of higher electrocatalytic oxygen reduction performance, and wide application prospects in the fields of electrocatalysis, fuel cells and the like.

Description

technical field [0001] The invention belongs to the field of preparation of electrode materials, in particular to a nitrogen-doped mesoporous carbon-loaded cobalt-cobalt oxide nanocomposite material (Co-CoO x / NMC) preparation method and application. Background technique [0002] Mesoporous carbon is an important branch of porous carbon materials, which refers to carbon materials with a pore size between micropores and macropores and a mesoporous structure. Due to its unique mesoporous structure, chemical stability, high specific surface area, and electrical conductivity, mesoporous carbon has been widely used in catalysis, adsorption separation, and energy storage. Combination of mesoporous carbon materials with metal-based nanoparticles, non-metallic elements, etc. can further combine the dual advantages of mesoporous carbon materials and loaded substances, greatly enhance their performance in related fields, and further expand the application range of mesoporous carbon m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05C01G51/04B82Y30/00B01J27/24C25B11/06
CPCC01G51/04B01J27/24B82Y30/00C01P2002/72C01P2002/82C01P2002/85C01P2004/04C01P2004/64C25B11/04
Inventor 江河清刘真真焦成丽
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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