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Method for preparing nitrogen-doped three-dimensional porous carbon microsphere-supported molybdenum carbide/molybdenum nitride and iron nanoparticle composite material

A technology of three-dimensional porous and composite materials, applied in chemical instruments and methods, nanotechnology, chemical/physical processes, etc., can solve the problems of complicated process, difficult to realize, high production cost, etc., and achieve simple and controllable preparation process and equipment Good performance and cost-saving effect

Inactive Publication Date: 2021-03-16
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, hydrothermal and solvothermal combined template technology has high production cost, complicated process and low output, which is not suitable for large-scale industrial production.
At the same time, it is difficult to co-support multiple metal-based materials on nitrogen-doped porous carbon microspheres.
These have severely limited its practical application and performance improvement in the field of electrochemistry.

Method used

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  • Method for preparing nitrogen-doped three-dimensional porous carbon microsphere-supported molybdenum carbide/molybdenum nitride and iron nanoparticle composite material
  • Method for preparing nitrogen-doped three-dimensional porous carbon microsphere-supported molybdenum carbide/molybdenum nitride and iron nanoparticle composite material
  • Method for preparing nitrogen-doped three-dimensional porous carbon microsphere-supported molybdenum carbide/molybdenum nitride and iron nanoparticle composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] According to Fe 3+ :Mo:C:Na + The ratio of the amount of material is 0.5:2:30:100, and 0.19g of FeCl 3 , 2.9 g of C 6 h 5 o 7 (NH 4 ) 3 , 0.842g of (NH4) 6 Mo 7 o 24 4H 2 O and 15g of NaCl were dissolved in 115mL of deionized water and stirred at room temperature for 8h to ensure that C 6 h 5 o 7 (NH 4 ) 3 Fully complexed with metal salts. The resulting homogeneous solution was spray-dried by a spray dryer. In the process, being burdened (NH4) 6 Mo 7 o 24 .4H 2 O, C 6 h 5 o 7 (NH 4 ) 3 and FeCl 3 The NaCl self-assembled to form a hollow sphere, and the size of the sphere was normally distributed. Due to the rapid volatilization of water on the surface of the droplet at high temperature, the water inside the droplet migrates to the surface with NaCl, which leads to its self-assembly in a very short time to form a hollow sphere precursor NaCl@FeCl 3 -C 6 h 5 o 7 (NH 4 ) 3 -(NH4) 6 Mo 7 o 24 4H 2 O. Put the precursor in a tube furnace, ...

Embodiment 2

[0025] According to Fe 3+ :Mo:C:Na + The ratio of the amount of material is 0.25:2.5:30:100, the FeCl of 0.097g 3 , 2.9 g of C 6 h 5 o 7 (NH 4 ) 3 , 1.053g of (NH4) 6 Mo 7 o 24 4H 2O and 15g of NaCl were dissolved in 115mL deionized water and stirred at room temperature for 12h to ensure that C 6 h 5 o 7 (NH 4 ) 3 Fully complexed with metal salts. The resulting homogeneous solution was spray-dried by a spray dryer. In the process, being burdened (NH4) 6 Mo 7 o 24 .4H 2 O, C 6 h 5 o 7 (NH 4 ) 3 and FeCl 3 The NaCl self-assembled to form a hollow sphere, and the size of the sphere was normally distributed. Due to the rapid volatilization of water on the surface of the droplet at high temperature, the water inside the droplet migrates to the surface with NaCl, which leads to its self-assembly in a very short time to form a hollow sphere precursor NaCl@FeCl 3 -C 6 h 5 o 7 (NH 4 ) 3 -(NH4) 6 Mo 7 o 24 4H 2 O. Put the precursor in a tube furnace,...

Embodiment 3

[0027] According to Fe 3+ :Mo:C:Na + The ratio of the amount of material is 0.21:1.4:21:100, the FeCl of 0.116g 3 , 2.9 g of C 6 h 5 o 7 (NH 4 ) 3 , 0.842g of (NH4) 6 Mo 7 o 24 4H 2 O and 20g of NaCl were dissolved in 115mL of deionized water and stirred at room temperature for 6h to ensure that C 6 h 5 o 7 (NH 4 ) 3 Fully complexed with metal salts. The resulting homogeneous solution was spray-dried by a spray dryer. In the process, being burdened (NH4) 6 Mo 7 o 24 .4H 2 O, C 6 h 5 o 7 (NH 4 ) 3 and FeCl 3 The NaCl self-assembled to form a hollow sphere, and the size of the sphere was normally distributed. Due to the rapid volatilization of water on the surface of the droplet at high temperature, the water inside the droplet migrates to the surface with NaCl, which leads to its self-assembly in a very short time to form a hollow sphere precursor NaCl@FeCl 3 -C 6 h 5 o 7 (NH 4 ) 3 -(NH4) 6 Mo 7 o 24 4H 2 O. Put the precursor in a tube furna...

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Abstract

The invention provides a method for preparing nitrogen-doped three-dimensional porous carbon microspheres loaded with molybdenum carbide / molybdenum nitride and iron nanoparticle composite materials, which includes the following steps: 1) Preparing precursors: selecting ferric chloride, ammonium heptamolybdate, Ammonium citrate and sodium chloride are used as raw materials. The above raw materials are mixed and dissolved in deionized water, and the resulting uniform mixed solution is sprayed into balls using a spray dryer to prepare the precursor; 2) Preparation of nitrogen-doped three-dimensional porous carbon microstructures Ball-loaded molybdenum carbide / molybdenum nitride and iron nanoparticle composite material: Calculate the precursor prepared in step 1 in a tube furnace and then cool it to room temperature to obtain the calcined product. Remove NaCl to obtain nitrogen-doped three-dimensional porous carbon microspheres. Loaded molybdenum carbide / molybdenum nitride and iron nanoparticle composites.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped three-dimensional porous carbon microspheres loaded with molybdenum carbide / molybdenum nitride and iron nanoparticles by using industrial production technology (spray drying method), and belongs to the technical field of nanomaterial preparation. Background technique [0002] Nitrogen-doped three-dimensional porous carbon microspheres have excellent physical and chemical properties, such as: large specific surface area, high mechanical strength, excellent electrical conductivity and thermal conductivity, etc., so they can be used in many fields, especially in electrochemical In the field, the rich pore structure and doped nitrogen atoms make the porous carbon microspheres can be used as a supporting matrix to load a variety of nano-metal particles or metal-based nanomaterials. The prepared composite material can be used as a high-performance electrode material in many applications. Various ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/24H01G11/30H01G11/36H01M4/36H01M4/38H01M4/58H01M4/62B01J27/24B82Y40/00
CPCH01M4/362H01M4/58H01M4/38H01M4/62H01G11/24H01G11/30H01G11/36B01J27/24B01J37/0018B82Y40/00B01J35/33Y02E60/10
Inventor 何春年陈伯超赵乃勤师春生马丽颖何芳刘恩佐
Owner TIANJIN UNIV