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Method for in-situ preparation of NbC and/or TaC powder by molten salt disproportionation reaction

A disproportionation reaction, in-situ preparation technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, inorganic chemistry, etc., can solve the complex preparation process and equipment, difficult to control morphology and size, synthesis temperature Advanced problems, to achieve the effects of low raw material cost and process cost, controllable product shape and scale, and simple process flow

Inactive Publication Date: 2020-04-21
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, one of the objectives of the present invention is to solve one or more of the existing problems of high synthesis temperature of NbC and TaC, complex preparation process and equipment, high cost, and difficult control of shape and size.

Method used

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  • Method for in-situ preparation of NbC and/or TaC powder by molten salt disproportionation reaction
  • Method for in-situ preparation of NbC and/or TaC powder by molten salt disproportionation reaction
  • Method for in-situ preparation of NbC and/or TaC powder by molten salt disproportionation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] In this embodiment, weigh 20 units of weight (for example, kilograms) of NaCl-KCl eutectic salt, and mix with 2 units of weight of Nb powder (400 mesh), 0.34 units of weight of Nb 2 o 5 Powder (300 mesh), 1.0 unit weight of NaF, 0.36 unit weight of nano C powder (average particle size 50nm) were mixed, and the mixture was placed in a corundum crucible. The above crucible was placed in a stainless steel reactor, sealed and protected by Ar gas. Use a temperature controller to raise the temperature to 750°C at a rate of 5°C / min, keep it at this temperature for 6 hours, and then turn off the power and cool down to room temperature with the furnace. The obtained product was taken out, soaked and rinsed with deionized water to remove residual molten salt, and then dried at 80° C. to obtain the target product NbC.

[0051] The obtained target product is tested, and its XRD pattern and SEM photo are respectively as follows figure 2 and 3 shown. Depend on figure 2 and 3...

Embodiment 2

[0053] In this example, weigh 50 units of NaCl-KCl eutectic salt, and mix it with 2 units of Nb powder (325 mesh), 0.7 units of NbCl 5 powder, 0.32 unit weight carbon nanotubes (average tube diameter 50nm, tube length 5-10μm) were mixed, and the mixture was placed in a corundum crucible. The above crucible was placed in a stainless steel reactor, sealed and protected by Ar gas. Use a temperature controller to raise the temperature to 925°C at a rate of 8°C / min, keep it at this temperature for 5 hours, then turn off the power and cool down to room temperature with the furnace. The resulting product was taken out, rinsed with deionized water to remove residual molten salt, and then dried at 100°C to obtain NbC nanotubes. The TEM results were as follows: Figure 4 As shown, the size of the NbC nanotubes in the obtained product is equivalent to that of the carbon nanotubes in the raw material, and the purity is 95.5 wt%.

Embodiment 3

[0055] In this example, weigh 10 units of NaCl-CaCl 2 Eutectic salt, and with 2 unit weight of Nb powder (325 mesh), 1.8 unit weight of NH 4 Cl and 0.32 unit weight of acetylene black (average particle size 50nm) were mixed, and the mixture was placed in a corundum crucible. The above crucible was placed in a stainless steel reactor, sealed and protected by Ar gas. Use a temperature controller to raise the temperature to 850°C at a rate of 8°C / min, keep it at this temperature for 3 hours, and then turn off the power and cool down to room temperature with the furnace. The obtained product is taken out, soaked and rinsed with deionized water to remove residual molten salt, and then dried at 100°C to obtain NbC nanoparticles. The particle size of the NbC nanoparticles in the obtained product is 50-80nm, and the purity is 99.6wt%.

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Abstract

The invention relates to the technical field of preparation of transition metal carbide powder materials, in particular to a method for in-situ preparation of an NbC and / or TaC powder material throughmolten salt disproportionation reaction. The method comprises directly forming a raw material mixture according to a stoichiometric ratio; reacting the raw material mixture in molten salt in an inertatmosphere, and cooling after the reaction is finished to obtain a product mixture; and removing the molten salt in the product mixture to obtain the NbC and / or TaC powder material. The method can solve one or more of the problems of high NbC and / or TaC synthesis temperature, complex preparation processes and equipment, high costs, uncontrollable morphology and sizes and the like in the prior art, and has the advantages of rapidness, high efficiency, energy saving, environmental protection, low cost, easy realization of large-scale production and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of transition metal carbide powder materials, in particular to a method for in-situ preparation of NbC and / or TaC powder materials by utilizing molten salt disproportionation reaction. Background technique [0002] Both niobium carbide and tantalum carbide have high melting point, hardness, good electrical and thermal conductivity, chemical stability, high thermal stability and mechanical stability, etc. It is these properties that make them widely used in metallurgy, machinery, Electronics, nuclear industry, biomaterials and aerospace and other fields. In addition, the unique electronic structure and excellent catalytic performance of niobium carbide and tantalum carbide have attracted great attention as a new type of catalytic material in the field of catalysis, which has expanded a new field for the research and development of niobium carbide and tantalum carbide. In many reactions catalyz...

Claims

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Application Information

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IPC IPC(8): C01B32/914B82Y30/00
CPCB82Y30/00C01P2002/01C01P2002/72C01P2004/03C01P2004/64C01P2006/80C01B32/914
Inventor 刘会军杨凌旭曾潮流
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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