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Method for preparing hafnium boride powder by using boron/carbothermic method

A reduction method, hafnium boride technology, applied in the direction of boron/boride, metal boride, etc., can solve the problems of low purity and poor uniformity of powder, and achieve the effect of simple process, short time consumption and low raw material cost

Active Publication Date: 2014-04-30
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, carbon black, boron carbide and hafnium oxide are mixed in a solid state, and the uniformity is poor, resulting in the synthesis of HfB 2 Powder purity is not high

Method used

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  • Method for preparing hafnium boride powder by using boron/carbothermic method
  • Method for preparing hafnium boride powder by using boron/carbothermic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Hafnium oxide (HfO 2 ) as hafnium source, with boron carbide (B 4 C) as a boron source, with sucrose as a carbon source;

[0032] (1) Weigh 100g HfO 2 Powder, its purity is 99.9wt%, and average particle size is 50nm, weighs 16.4g boron carbide (B 4 C) powder, the purity is 96wt%, and the average particle size is 0.8μm. Put the two powders together into a ball mill tank, add absolute ethanol, add zirconia ball mill media, and ball mill for 24 hours. Move the mixed mixture to In a vessel containing 250ml of absolute ethanol, disperse by ultrasonic oscillation for 0.5h;

[0033] (2) Weigh 13.5g of sucrose and add it to 200ml of water, stir to make it evenly mixed, then add it to the solution obtained in step (1), and stir magnetically while heating. The heating temperature is 100°C and the heating time is 8h, and the mixture uniform reactants;

[0034] (3) Put the reactant obtained in step (2) into a graphite crucible, and then put the graphite crucible into a high-puri...

Embodiment 2

[0036] Hafnium oxide (HfO 2 ) as hafnium source, with boron carbide (B 4 C) as a boron source, with sucrose as a carbon source;

[0037] (1) Weigh 100g HfO 2 Powder, its purity is 99.9wt%, and average particle diameter is 100nm, weighs 15.7g boron carbide (B 4 C) powder, the purity is 96.0wt%, and the average particle size is 1 μm. Put the two powders together into a ball mill jar, add absolute ethanol, add zirconia ball mill media, and ball mill for 12 hours. Move the mixed mixture to In a vessel containing 300ml of absolute ethanol, disperse by ultrasonic oscillation for 1h;

[0038] (2) Weigh 27.0g of sucrose and add it to 200ml of water, stir to make it evenly mixed, then add it to the solution obtained in step 1), and stir magnetically while heating. reactant;

[0039] (3) Put the reactant obtained in step (2) into a graphite crucible, and then put the graphite crucible into a high-purity argon-protected heat treatment furnace for heating. The heating program is to h...

Embodiment 3

[0041] Hafnium oxide (HfO 2 ) as hafnium source, with boron carbide (B 4 C) as a boron source, with sucrose as a carbon source;

[0042] (1) Weigh 100g HfO 2 Powder, its purity is 99.9wt%, and average particle diameter is 80nm, weighs 13.1g boron carbide (B 4 C) powder, the purity is 97wt%, and the average particle size is 1.5 μm. Put the two powders together into a ball mill jar, add absolute ethanol, add zirconia ball milling media, and ball mill for 24 hours. Move the mixed mixture to In a vessel containing 300ml of absolute ethanol, disperse by ultrasonic oscillation for 0.5h;

[0043] (2) Weigh 22.5g of sucrose and add it to 200ml of water, stir to make it evenly mixed, then add it to the solution obtained in step (1), and heat it with magnetic stirring at the same time. uniform reactants;

[0044] (3) Put the reactant obtained in step (2) into a graphite crucible, and then put the graphite crucible into a high-purity argon-protected heat treatment furnace for heatin...

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Abstract

The invention relates to a method for preparing hafnium boride powder by using a boron / carbothermic method. The method comprises the following steps: (1) dissolving hafnium oxide and boron carbide in absolute ethyl alcohol or deionized water to mix up uniformly, and ultrasonically dispersing for 0.5-4 hours, wherein the concentration of a hafnium oxide solution is 0.3-3mol / L, and the concentration of a boron carbide solution is 0.3-3mol / L; (2) dissolving a carbon source into a solvent, subsequently pouring into a mixed suspension, heating and stirring to obtain a reactant which is uniformly mixed; and (3) adding the reactant into a graphite crucible, putting the graphite crucible into a thermal treatment furnace or a vacuum furnace for heating in the presence of flowing argon, subsequently cooling down to room temperature along with the furnace, further grinding to obtain HfB2 powder with the particle size of 100-500nm. According to the method, a hafnium source, a boron source and a carbon source are mixed in a wet mixing manner, and are uniformly mixed and not easy to agglomerate, the synthesis process is performed in high-purity Ar or vacuum, and the HfB2 powder can be synthesized through reduction reaction at low temperature, and is low in cost of raw materials.

Description

technical field [0001] The invention relates to a method for preparing hafnium boride powder at low temperature by a boron / carbothermal reduction method, and belongs to the technical field of ultra-high temperature functional / structural ceramics. Background technique [0002] HfB 2 Ceramics have a high melting point (3380°C), high hardness (28GPa), high strength, and good thermal conductivity (104W·(m·K) -1 ) and conductivity (9.1×10 6 S / m), excellent ablation resistance and thermal shock resistance, etc., have been widely used in the fields of aerospace high-temperature structural materials, superhard tool materials, composite materials, refractory materials and electrode materials, and become a A very promising ultra-high temperature structural ceramic material. But since the commercial HfB 2 Oxygen pollution on powder surface (by amorphous B 2 o 3 and crystalline HfO 2 Composition) makes it difficult to sinter and densify, and only when these oxygen contaminations ...

Claims

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Application Information

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IPC IPC(8): C01B35/04
Inventor 赵彦伟周延春李军平刘宏瑞
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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