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Preparation method of nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material

A nitrogen-doped carbon and composite material technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, electrodes, etc., can solve the problems of exhaust gas pollution, many by-products, cumbersome production process, etc. , to achieve the effect of high safety factor, less environmental pollution and simple operation

Inactive Publication Date: 2018-06-15
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation methods of nitrogen-doped carbon nanotube-wrapped metal composites mainly include: 1) Chemical Vaporous Deposition (CVD), but the preparation cost of this method is high, there are many by-products, and the nitrogen content cannot be controlled. , and the tail gas is easy to pollute the environment; 2) Electrochemical Deposition method (Electrochemical Deposition), this method needs to be carried out under certain electrolyte and operating conditions, and is greatly affected by the composition of the electrolyte and the pH and temperature of the environment
3) Impregnation method (Impregnation), this method is often affected by material properties and metal particle size, and the prepared material has low metal content and uneven dispersion; 4) Arc Discharge method (Arc Discharge), the preparation method has relatively high requirements, and the production process It is cumbersome, the raw materials are restricted, the production cannot be scaled and continuous, and the product purity and quality are not very high

Method used

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  • Preparation method of nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material
  • Preparation method of nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material
  • Preparation method of nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Preparation of nitrogen-doped carbon nanotube-wrapped iron-cobalt alloy composite (FeCo-NCNTs)

[0029] Dissolve the metal salt and dicyandiamide with a molar ratio of 1:30 in deionized water, wherein the metal salt only contains iron nitrate and cobalt nitrate and the molar ratio of the two is 1:10, ultrasonically mix evenly, and then dry and grind to prepare have to The precursor is placed in a high-temperature tube furnace under a nitrogen atmosphere, and the temperature is raised and roasted in programmed stages. The temperature of the first stage of roasting is 500°C, the roasting time is 3h, and the heating rate is 2°C / min; the temperature of the second stage of roasting is 700°C ℃, the calcination time is 4h, and the heating rate is 5℃ / min. After the temperature of the tube furnace dropped to room temperature, the sample was taken out for grinding to obtain a black powder.

[0030] The obtained samples were placed in a beaker with dilute sulfuric ac...

Embodiment 2

[0031] Example 2 Preparation of nitrogen-doped carbon nanotube-wrapped iron-cobalt alloy composite (FeCo-NCNTs)

[0032] Dissolve metal salt and urea with a molar ratio of 1:3 in deionized water, wherein the metal salt only contains ferric chloride and cobalt chloride and the molar ratio of the two is 10:1, ultrasonically mix evenly, and then dry and grind to prepare have to The precursor is placed in a high-temperature tube furnace under a nitrogen atmosphere, and the temperature is raised and roasted in programmed stages. The temperature of the first stage of roasting is 600°C, the roasting time is 2h, the heating rate is 5°C / min, and the temperature of the second stage of roasting is 900°C. ℃, the calcination time is 2h, and the heating rate is 10℃ / min. After the temperature of the tube furnace dropped to room temperature, the sample was taken out for grinding to obtain a black powder.

[0033] The obtained samples were placed in a beaker with dilute sulfuric acid The s...

Embodiment 3

[0034] Example 3 Preparation of nitrogen-doped carbon nanotube-wrapped iron-cobalt alloy composite (FeCo-NCNTs)

[0035] Dissolve metal salt and cyanamide with a molar ratio of 1:10 in deionized water, wherein the metal salt only contains iron nitrate and cobalt nitrate and the molar ratio of the two is 1:10, ultrasonically mix evenly, and then dry and grind to prepare have to The precursor is placed in a high-temperature tube furnace under a nitrogen atmosphere, and the temperature is raised and roasted in programmed stages. The temperature of the first stage of roasting is 600°C, the roasting time is 3h, the heating rate is 5°C / min, and the temperature of the second stage of roasting is 900°C. ℃, the calcination time is 4h, and the heating rate is 10℃ / min. After the temperature of the tube furnace dropped to room temperature, the sample was taken out for grinding to obtain a black powder.

[0036] The obtained samples were placed in a beaker with dilute sulfuric acid The...

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Abstract

Belonging to the technical field of material preparation, the invention relates to a preparation method of a nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material (FeCo-NCNTs). The technical scheme includes: firstly, dissolving a metal salt and a carbon-nitrogen source in water, ethanol or ethylene glycol, mixing the substances evenly, and then performing drying and grinding to obtain a precursor; then putting the precursor in a tubular furnace, in a nitrogen atmosphere, conducting programmed heating to a roasting temperature, and conducting high temperature roasting and grinding to obtain a black powder sample; and then subjecting the black sample to pickling treatment until the pH value of the solution is neutral, and conducting pumping filtration and naturaldrying, thus obtaining the nitrogen-doped carbon nanotube wrapped metal iron-cobalt alloy composite material (FeCo-NCNTs). The obtained composite material can be used as a good electrocatalytic hydrogen evolution catalyst. The composite material prepared by the method provided by the invention has the characteristics of easily available raw materials and low cost, and has important significance inelectrochemical application.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a preparation method of nitrogen-doped carbon nanotube-wrapped iron-cobalt alloy composite material (FeCo-NCNTs). technical background [0002] Carbon nanotubes are one-dimensional quantum materials with a special structure (the radial dimension is on the order of nanometers, the axial dimension is on the order of microns, and both ends of the tube are basically sealed). The novel structure and many potential application values ​​in the future high-tech field quickly become a research hotspot in the field of material science worldwide, and become one of the most typical and representative nanomaterials. When carbon nanotubes are doped, substituted and modified, their functions and application range will be greatly improved. In the periodic table of elements, nitrogen is adjacent to carbon, so nitrogen atoms are easier to dope into carbon nanotubes without causing too ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J27/24C25B1/04C25B11/06
CPCC25B1/04B01J23/75B01J27/24C25B11/091B01J35/33Y02E60/36
Inventor 吕晓萌张素云刘军谢吉民邵守言
Owner JIANGSU UNIV
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