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Method for preparing bimetallic carbide composite material through thermolysis approach

A technology of bimetallic carbides and composite materials, applied in the direction of carbides, carbon oxides/sulfur carbides, nanotechnology for materials and surface science, etc., can solve the problems of complex synthesis conditions and difficult control, and achieve preparation The process is simple, the operation is convenient, and the effect of relatively high reaction temperature requirements

Active Publication Date: 2019-08-09
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Transition metal carbides have attracted widespread attention due to their platinum-like catalytic behavior, while multi-metal carbides that utilize the synergistic effect and alloy effect between different metals are considered to have better electrocatalytic hydrogen evolution performance, but their synthesis conditions are complex and difficult to control
At present, the research on metal carbides at home and abroad is mainly focused on doping single metals into various carbides, but by mixing heteropolyacids with organic amines and then calcining them to prepare double metal carbides containing atomically premixed cubic phases. material composite materials and has electrolysis of water hydrogen production reaction, there is no such report

Method used

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  • Method for preparing bimetallic carbide composite material through thermolysis approach
  • Method for preparing bimetallic carbide composite material through thermolysis approach
  • Method for preparing bimetallic carbide composite material through thermolysis approach

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Heterotungstate Na 10 [Co 4 (H 2 O) 2 (PW 9 o 34 ) 2 ]·27H 2 O (0.54g, 0.1mmol) was dissolved in deionized water (30mL) to obtain heterotungstic acid solution; octadecyltrimethylammonium chloride (0.7g, 2.01mmol) was dissolved in deionized water (10mL), Obtain an organic amine solution; under the condition of stirring, add the heterotungstic acid solution dropwise to the organic amine solution, continue stirring for 1 hour after dropping, then centrifuge, wash with deionized water, and dry to obtain a solid precursor powder, which is stored in a dry place after grinding spare in the device;

[0037] Spread the precursor solid powder in a porcelain boat, place the porcelain boat in a quartz boat, place the quartz boat in a tube furnace for temperature-programmed calcination, and the calcination procedure is as follows: first, in N 2 Under the atmosphere, the temperature was raised from room temperature to 410 °C at a rate of 2 °C / min and kept for 1 h; 2 :H 2 =8...

Embodiment 2

[0039] Heterotungstate Na 10 [Co 4 (H 2 O) 2 (PW 9 o 34 ) 2 ]·27H 2 O (0.54g, 0.1mmol) was dissolved in deionized water (30mL) to obtain heterotungstic acid solution; octadecyltrimethylammonium chloride (0.7g, 2.01mmol) was dissolved in deionized water (10mL), Obtain an organic amine solution; under the condition of stirring, add the heterotungstic acid solution dropwise to the organic amine solution, continue stirring for 1 hour after dropping, then centrifuge, wash with deionized water, and dry to obtain a solid precursor powder, which is stored in a dry place after grinding spare in the device;

[0040] Spread the precursor solid powder in a porcelain boat, place the porcelain boat in a quartz boat, place the quartz boat in a tube furnace for temperature-programmed calcination, and the calcination procedure is as follows: first, in N 2 Under the atmosphere, the temperature was raised from room temperature to 410 °C at a rate of 2 °C / min and kept for 1 h; 2 :H 2 =9...

Embodiment 3

[0042] Heterotungstate Na 10 [Co 4 (H 2 O) 2 (PW 9 o34 ) 2 ]·27H 2 O (1.08g, 0.2mmol) was dissolved in deionized water (40mL) to obtain heterotungstic acid solution; octadecyltrimethylammonium chloride (1.4g, 4.02mol) was dissolved in deionized water (20mL), Obtain an organic amine solution; under the condition of stirring, add the heterotungstic acid solution dropwise to the organic amine solution, continue stirring for 1 hour after dropping, then centrifuge, wash with deionized water, and dry to obtain a solid precursor powder, which is stored in a dry place after grinding spare in the device;

[0043] Spread the precursor solid powder in a porcelain boat, place the porcelain boat in a quartz boat, place the quartz boat in a tube furnace for temperature-programmed calcination, and the calcination procedure is as follows: first, in N 2 Under the atmosphere, the temperature was raised from room temperature to 410 °C at a rate of 2 °C / min and kept for 1 h; 2 :H 2 =95:5...

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Abstract

The invention relates to a method for preparing a bimetallic carbide composite material. The method comprises the steps of dripping a hetero-tungstic acid solution Na10[Co4(H2O)2(PW9O34)2] 27H2O intoan organic amine solution during stirring, continuing stirring for 1 hour after dripping, performing centrifuging, conducting washing with deionized water, performing drying to obtain precursor solidpowder, and calcining the precursor solid powder to obtain the bimetallic carbide composite material. According to the method for preparing the bimetallic carbide for efficient electrolyzation of water for hydrogen evolution, prepared bimetallic carbide nanoparticles are uniform in size and high in dispersibility, wherein the molar ratio of Co6W6C is controlled within a range from 50% to 60%, andthe nanoparticles are coated with carbon in the thickness of 3-5 nm so that a corrosion effect of an electrolyte on a catalyst in a hydrogen evolution process can be effectively prevented. The methodhas the advantages of simple preparation process, convenient operation, lower requirement for reaction temperature and high efficiency and achieves a broad application prospect in the aspect of industrial application.

Description

[0001] (1) Technical field [0002] The invention relates to a method for preparing a double metal carbide composite material by a thermal decomposition method. [0003] (2) Background technology [0004] Among all the current artificial energy sources, hydrogen energy is a clean energy source with great potential for development because its reaction product is water and has no pollution to the environment. However, most of hydrogen energy is still produced from traditional fossil fuels, so how to efficiently and continuously produce hydrogen has become the focus of scientific research. Researching out efficient and stable catalysts to reduce the overpotential of hydrogen evolution will have great guiding significance for solving the energy crisis mentioned above. [0005] The thermal decomposition method is a method of decomposing metal compounds to form metal elements and other compounds at high temperature. In the reaction, only need to control the temperature, time, and ga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/907C25B1/04C25B11/06B82Y30/00
CPCB82Y30/00C01B32/907C01P2004/80C25B1/04C25B11/04Y02E60/36
Inventor 高静杨佳兴金秋阳刘书杰佟明兴李国华
Owner ZHEJIANG UNIV OF TECH
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