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Method for in-situ preparation of zirconium, hafnium or vanadium carbide powder by molten salt disproportionation reaction

A disproportionation reaction and in-situ preparation technology, which is applied in the field of HfC or VC powder to prepare ZrC, can solve the problems of complex preparation process and equipment, difficult control of shape and size, high synthesis temperature, etc., and achieve low raw material cost and process cost , product shape and size controllable, simple process effect

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 ZrC, HfC or VC powder synthesis temperature, complex preparation process and equipment, high cost, difficult to control shape and size, etc.

Method used

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  • Method for in-situ preparation of zirconium, hafnium or vanadium carbide powder by molten salt disproportionation reaction
  • Method for in-situ preparation of zirconium, hafnium or vanadium carbide powder by molten salt disproportionation reaction
  • Method for in-situ preparation of zirconium, hafnium or vanadium carbide powder by molten salt disproportionation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0049] In this embodiment, weigh 50 unit weight of LiCl-KCl eutectic salt, and mix with 3.0 unit weight of Zr powder (200 mesh), 0.4 unit weight of nano-scale acetylene black powder (average particle size 40nm), and place the mixture in 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 940°C at a rate of 10°C / min, keep it at this temperature for 2 hours, 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 ZrC nanometer powder.

[0050] 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 It can be seen that the obtained nano-powder is ZrC, and after further testing, the particle size of the Z...

Embodiment 2

[0052] In the present embodiment, weigh 20 unit weight of KF-KCl eutectic salt, and mix with 3.0 unit weight of Zr powder (325 mesh), 0.68 unit weight of NH 4 Cl, 0.4 unit weight of graphite flakes (average particle size 500nm) 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 880°C at a rate of 8°C / min, keep 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 120°C to obtain ZrC nanopowder. The ZrC nanopowder in the obtained product has a particle size of 500-700nm and a purity of 98.5wt%.

Embodiment 3

[0054] In this embodiment, weigh 30 unit weights of NaCl-KCl eutectic salt, mix with 4.3 unit weights of V powder (325 mesh), 1.0 unit weights of acetylene black (average particle size 40nm), and place the mixture 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 950°C at a rate of 5°C / min, keep it at this temperature for 4 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, then dried at 80°C, and detected by XRD and SEM as follows: Figure 4 and 5 As shown, the target product is VC nanopowder, and the particle size of VC nanopowder in the obtained product is 50-80nm, and the purity is 98wt%.

[0055] In addition, it has been tested that the obtained ZrC nanopowders and VC nanopowders have excellent hydrophilicity and dispers...

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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 ZrC, HfC or VC powder in situ through molten salt disproportionation reaction. The method comprises directly forming a raw material mixture according to the stoichiometric ratio, with the structural formula of transition metal carbide beingMC, M being a transition metal element zirconium or hafnium or vanadium, and C being a carbon element; reacting the raw material mixture in molten salt in an inert atmosphere, and cooling after the reaction is finished to obtain a product mixture; and removing the molten salt in the product mixture to obtain ZrC, HfC or VC powder. The method can solve one or more of the problems of high ZrC, HfC or VC powder synthesis temperatures, 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, a 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 ZrC, HfC or VC powder by using molten salt disproportionation reaction. Background technique [0002] Transition metal carbides ZrC, HfC and VC are a class of substances with high melting point, hardness, good electrical and thermal conductivity, chemical stability, and extremely high thermal and mechanical stability. It is these properties that make They are widely used in fields such as metallurgy, machinery, electronics, nuclear industry, biomaterials and aerospace. In addition, due to their unique electronic structure and excellent catalytic performance, transition metal carbides have attracted great attention as a new class of catalytic materials in the field of catalysis, which has expanded a new field for the research and development of transition metal carbides. In many reactions catalyz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/626
CPCC04B35/5607C04B35/5622C04B35/62645C04B2235/781C04B2235/785C04B2235/96
Inventor 刘会军杨凌旭曾潮流
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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