Preparation method of zirconium diboride powder

A technology of zirconium diboride and zirconium dioxide powder is applied in the field of preparation of zirconium diboride ceramic powder, which can solve the problems of low production cost, low reaction efficiency, coarse product particles and the like, and achieves fast heating speed and high purity. High, complete product conversion effect

Active Publication Date: 2016-08-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The most commonly used method in industrial production is carboron thermal reduction: 3ZrO 2 +B 4 C+8C+B 2 o 3 →3ZrB 2 +9CO, the raw materials of this method are easy to obtain, the production cost is low, but the reaction efficiency is low, and a higher temperature is required to complete the reaction, which will cause the product particles to be coarse, and it is difficult to obtain fine-sized particles

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  • Preparation method of zirconium diboride powder
  • Preparation method of zirconium diboride powder
  • Preparation method of zirconium diboride powder

Examples

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Effect test

Embodiment 1

[0021] A preparation method of zirconium diboride powder, which comprises the steps of:

[0022] Zirconia powder (50nm), amorphous boron powder (1μm), amorphous carbon powder (50nm) and boron carbide powder (1μm) are selected as raw materials, x is 0.1, y is 0.1, and the total molar ratio is 0.4:1: 0.1:0.1, planetary ball milling for 6 hours, the ball milling balls are zirconia balls (diameter 5mm), the medium is ethanol, the ball milling speed is 200 rpm; after ball milling, filter, pour the filtered liquid into a pear-shaped bottle, and rotate at 60°C Evaporate for 0.5h, dry for 48h (dried at 60°C), grind and sieve (325 mesh) to get a uniformly mixed mixed powder (or called raw material powder); put the mixed powder in a graphite reactor, and the graphite reacts Put the device into a high-current reaction synthesis device, evacuate to below 10Pa, start heating (200K / min), heat up to 1400°C and keep warm for 3 minutes to obtain a powder sample; take out the synthesized powder...

Embodiment 2

[0024] A preparation method of zirconium diboride powder, which comprises the steps of:

[0025] Choose zirconia powder (50nm), amorphous boron powder (1μm), amorphous carbon powder (50nm) and boron carbide powder (1μm) as raw materials, x is 0.1, y is 0.5, and the total molar ratio is 0.9:1 : 0.1: 0.5, planetary ball milling for 6 hours, ball milling balls are zirconia balls (diameter 5mm), medium is ethanol, ball milling speed is 200 rpm; filter after ball milling, pour the filtered liquid into a pear-shaped bottle, and store at 60°C Rotary evaporation for 0.5h, drying for 48h (drying at 60°C), grinding and sieving (325 mesh) to obtain a uniformly mixed mixed powder; put the mixed powder in a graphite reactor, and put the graphite reactor into a high-current reaction In the synthesis device, evacuate to below 10Pa, start to heat up (300K / min), heat up to 1400°C and keep it warm for 5 minutes to obtain a powder sample; take out the synthesized powder sample, wash it in hot wa...

Embodiment 3

[0027] A preparation method of zirconium diboride powder, which comprises the steps of:

[0028] Zirconia powder (50nm), amorphous boron powder (1μm), amorphous carbon powder (50nm) and boron carbide powder (1μm) are selected as raw materials, x is 0.33, y is 0.1, and the total molar ratio is 0.46:1: 0.33:0.1, planetary ball milling for 6 hours, ball milling balls are zirconia balls (diameter 5mm), medium is ethanol, ball milling speed is 200 rpm; filter after ball milling, pour the filtered liquid into a pear-shaped bottle, and rotate at 60°C Evaporate for 0.5h, dry for 48h (dry at 60°C), grind and sieve (325 mesh) to get a uniform mixed powder; put the mixed powder in a graphite reactor, and put the graphite reactor into a high-current reaction synthesis In the device, evacuate to below 10Pa, start to heat up (500K / min), heat up to 1500°C and keep warm for 3 minutes to obtain a powder sample; take out the synthesized powder sample, wash it in 80°C hot water for 2h, filter an...

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Abstract

The invention relates to a preparation method of zirconium diboride powder and belongs to the field of nonoxide ceramic powder preparation. The preparation method is characterized by including following steps: 1), selecting zirconium dioxide powder, amorphous boron powder, amorphous carbon powder and boron carbide powder, and performing ball milling, rotary evaporating and grinding and sieving to obtain uniform mixed powder; 2), performing synthesis and aftertreatment on the mixed powder: placing the mixed powder in a large-current reaction synthetic device, quickly heating to 1300-1500 DEG C at a temperature rising speed of 50-500 DEG C / min, maintaining the temperature for 3-10 min, obtaining a powder sample, washing with water, and drying to obtain high-purity ZrB2 powder. By using the preparation method, the ZrB2 powder which is high in purity (> / =95 wt%) and small in grain size (< / =500 nm) can be obtained within several minutes.

Description

technical field [0001] The invention relates to a preparation method of zirconium diboride ceramic powder, which belongs to the field of preparation of non-oxide ceramic powder. Background technique [0002] Zirconium boride (ZrB 2 ) is a transition metal boride, its crystal structure is hexagonal C32 type, B atomic plane and Zr atomic plane appear alternately to form a two-dimensional network structure, this structure similar to graphite determines the ZrB 2 Has good electrical and thermal conductivity. The Zr-B bond and the B-B bond have strong covalent bonds and large bond energy, which determines that zirconium boride has an ultra-high melting point (3245°C), and its ceramic products have excellent mechanical properties and good chemical properties. stability. [0003] Preparation of ZrB 2 The methods of powder mainly include: elemental direct synthesis method, carbothermal / magnesian / borothermal reduction method, etc. The synthesis method of each element uses the di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626
CPCC04B35/58078C04B35/626C04B2235/3244C04B2235/3821C04B2235/421C04B2235/422
Inventor 傅正义顾俊峰王为民王皓张帆
Owner WUHAN UNIV OF TECH
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