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Method for in-situ preparation of Cr3C2 and/or Mo2C powder by using molten salt

A technology for in-situ preparation and molten salt, applied in the field of preparing Cr3C2 and/or Mo2C powder, can solve the problems of high synthesis temperature, difficult control of morphology and size, complicated preparation process and equipment, etc. The effect of low mass production, raw material cost and process cost

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

AI Technical Summary

Problems solved by technology

For example, one of the purposes of the present invention is to solve the problem of existing Cr 3 C 2 and / or Mo 2 One or more of the problems of high synthesis temperature, 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 Cr3C2 and/or Mo2C powder by using molten salt
  • Method for in-situ preparation of Cr3C2 and/or Mo2C powder by using molten salt
  • Method for in-situ preparation of Cr3C2 and/or Mo2C powder by using molten salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] In this embodiment, weigh 20 units of LiCl-KCl eutectic salt, and mix with 1.3 units of Cr powder (325 mesh), 0.34 units of NH 4 Cl and 0.2 unit weight of graphite (average particle size 1 μm) 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 920°C at a rate of 8°C / min, keep at this temperature for 3 hours, 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 80°C to obtain Cr 3 C 2 , Cr in the resulting product 3 C 2 The particle size of the powder is 1-2 μm, and the purity is 98wt%.

[0050] As detected by XRD figure 2 As shown, the target product is Cr 3 C 2 . The obtained target product is characterized by SEM, and its SEM is as follows image 3 shown....

Embodiment 2

[0052] In the present embodiment, weigh 30 unit weights of NaCl-KCl eutectic salt, and mix with 2.6 unit weights of Cr powder (325 mesh), 2.1 unit weights of CrCl 3 , 0.4 unit weight of carbon black (average particle size 200nm) was 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 860°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 obtained product is taken out, soaked and rinsed with deionized water to remove residual molten salt, and then dried at 120°C to obtain Cr 3 C 2 , Cr in the resulting product 3 C 2 The particle size of the powder is 300-500nm, and the purity is 99wt%.

Embodiment 3

[0054] In the present embodiment, weigh 40 unit weight of KF-KCl eutectic salt, and mix with 2.6 unit weight of Cr powder (325 mesh), 1.08 unit weight of Cr powder 2 o 3 , 0.25 unit weight flake graphite (average particle size 500nm) was 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 980°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 is taken out, soaked and rinsed with deionized water to remove residual molten salt, and then dried at 80°C to obtain Cr 3 C 2 , Cr in the resulting product 3 C 2 The particle size of the powder is 1-2 μm, and the purity is 99.5 wt%.

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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 Cr3C2 and / or Mo2C powder in 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 being MxCy, M being a transition metal element Cr and / or Mo, and C being carbon; reacting the raw material mixture in molten salt in an inert atmosphere, and cooling after the reaction is finished to obtain aproduct mixture; and removing the molten salt in the product mixture to obtain the Cr3C2 and / or Mo2C powder material. The method can solve one or more of the problems of high synthesis temperature, complex preparation process and equipment, high cost, uncontrollable morphology and size and the like of the existing transition metal carbide, and has the advantages of rapidness, high efficiency, energy conservation, environmental protection, low cost, easiness in realizing 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 Cr by using molten salt disproportionation reaction 3 C 2 and / or Mo 2 C powder method. Background technique [0002] Transition metal carbide Cr 3 C 2 and / or Mo 2 C is 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 them widely used in metallurgy, machinery, etc. , electronics, nuclear industry, biomaterials and aerospace and other fields. 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 carbi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/626
CPCC04B35/5607C04B35/62675C04B2235/786C04B2235/96C04B2235/95
Inventor 刘会军杨凌旭曾潮流
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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