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A two-step method for preparing refractory metal borides

A technology of refractory metal and boride, which is applied in the field of preparation of refractory metal boride, can solve the problems of economy, reliability and high product quality, and achieve the effect of flexible and convenient method and low raw material cost

Active Publication Date: 2022-02-25
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods often cannot balance economy, reliability and high product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) A refractory metal oxide powder (TiO 2 , ZrO 2 , HfO 2 , V 2 o 3 , Nb 2 o 5 、 Ta 2 o 5 and Cr 2 o 3 ) and graphite are weighed and proportioned according to the reaction metering ratio of carbon excess 20%, and mixed uniformly.

[0020] (2) Under an argon protective atmosphere, the mixture obtained in (1) was placed in a crucible for vacuum treatment at 1800° C. for 4 hours.

[0021] (3) the reaction product in (2) and B 4 C mixes uniformly by reaction stoichiometric ratio, and adds the calcium metal of excessive 20% reaction stoichiometric ratio;

[0022] (4) Under an argon protective atmosphere, the mixture obtained in (3) was placed in a crucible and treated at 1300° C. for 4 hours.

[0023] (5) After the heat preservation is completed, the reaction product is cooled to room temperature in an argon atmosphere, and the reaction product is filtered by acid leaching, rinsed and dried to obtain a refractory metal boride.

Embodiment 2

[0025] (1) A refractory metal oxide powder (TiO 2 , ZrO 2 , HfO 2 , V 2 o 3 , Nb 2 o 5 、 Ta 2 o 5 and Cr 2 o 3 ) and carbon black are weighed and proportioned according to the reaction metering ratio of carbon excess of 20%, and mixed uniformly.

[0026] (2) Under an argon protective atmosphere, the mixture obtained in (1) was placed in a crucible for vacuum treatment at 1500° C. for 4 hours.

[0027] (3) the reaction product in (2) and B 4 C mixes uniformly by reaction stoichiometric ratio, and adds the calcium metal of excessive 20% reaction stoichiometric ratio;

[0028] (4) Under an argon protective atmosphere, the mixture obtained in (3) was placed in a crucible and treated at 1300° C. for 4 hours.

[0029] (5) After the heat preservation is completed, the reaction product is cooled to room temperature in an argon atmosphere, and the reaction product is filtered by acid leaching, rinsed and dried to obtain a refractory metal boride.

Embodiment 3

[0031] (1) A certain nanometer refractory metal oxide powder (TiO 2 or ZrO 2 ) and carbon black are weighed and proportioned according to the reaction metering ratio of carbon excess of 20%, and mixed uniformly.

[0032] (2) Under an argon protective atmosphere, the mixture obtained in (1) was placed in a crucible for vacuum treatment at 1500° C. for 4 hours.

[0033] (3) the reaction product in (2) and B 4 C mixes uniformly by reaction stoichiometric ratio, and adds the calcium metal of excessive 20% reaction stoichiometric ratio;

[0034] (4) Under an argon protective atmosphere, the mixture obtained in (3) was placed in a crucible and treated at 1200° C. for 4 hours.

[0035] (5) After the heat preservation is completed, the reaction product is cooled to room temperature in an argon atmosphere, and the reaction product is filtered by acid leaching, rinsed, and dried to obtain ultrafine refractory metal borides.

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Abstract

A method for preparing refractory metal boride in two steps belongs to the field of inorganic non-metallic materials. Refractory metal borides usually have the characteristics of high melting point, high hardness, good wear resistance and good oxidation resistance. The current industrial methods for preparing refractory metal borides have the problems of low product purity, large particle size and high preparation cost. Usually, the preparation of elemental powders of such metals is difficult and expensive. The method uses refractory metal oxides, carbonaceous reducing agents, boron carbide and metal calcium as raw materials, first undergoes a high-temperature carbothermic reduction reaction, and then undergoes a high-temperature boride reaction under certain conditions to generate corresponding refractory metal borides, and the final reaction The product is acid leached to remove soluble impurities, and then filtered, rinsed and dried to obtain high-purity refractory metal boride. The invention is a new method for synthesizing refractory metal boride powder, which has the advantages that the method has universal applicability, the reaction product has high purity, low cost, controllable product particle size, and is easy to scale production.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and discloses a two-step method for preparing refractory metal borides, especially relates to the preparation of refractory metals using refractory metal oxides, carbonaceous reducing agents, boron carbide and metal calcium as raw materials boride method. Background technique [0002] Due to their special chemical bond structure, refractory metal borides usually have high melting point, high hardness, good electrical and thermal conductivity, and high corrosion resistance. They are a class of materials that can be used in extreme service conditions. Refractory metal borides can be used as heat shielding materials, ceramic armor, special knives, wear-resistant ceramics, etc. A large number of preparation methods of refractory metal boride powders have been proposed, such as direct elemental synthesis, borothermic reduction, carbothermal reduction, magnesothermic reduction, electrol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/04
CPCC01B35/04
Inventor 张国华汪宇
Owner UNIV OF SCI & TECH BEIJING
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