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Method for preparing hafnium boride powder

A technology of hafnium boride and powder, which is applied in the field of polyethylene glycol-assisted preparation of hafnium boride powder, which can solve the problem of many steps, high requirements for preparation conditions, and unsatisfactory particle size, purity, and output of hafnium boride powder scientific research and production

Pending Publication Date: 2022-05-13
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these preparation methods have a long production cycle, many steps, and high preparation conditions, and the particle size, purity, and output of the produced hafnium boride powder cannot meet the needs of scientific research and production.
[0005] Saranya Venugopal et al proposed a gel-sol method using phenolic resin, hafnium chloride and boric acid to synthesize hafnium boride powder (J.Am.Ceram.Soc.,97[1]92–99(2014)), but The particle size of the hafnium boride powder prepared by this method is large and uneven, which further affects the quality of the powder and the performance of the subsequent ceramic block.
[0006] The applicant proposed a method (CN113816379A) ​​for synthesizing hafnium boride powder using boric acid, sorbitol, and hafnium chloride as raw materials. However, the hafnium boride powder prepared by this method still has the problem of wide particle size distribution. As a result, the bulk ceramic body formed by subsequent sintering is not dense

Method used

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  • Method for preparing hafnium boride powder
  • Method for preparing hafnium boride powder
  • Method for preparing hafnium boride powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Weigh 2g (32mmol) of boric acid and 3g (16mmol) of sorbitol, mix them in the same beaker, then pour 20mL of acetic acid (analytical grade, 21g) into it, and use an oil bath magnetic stirrer to gradually raise the temperature to 60°C , stirring at constant temperature, until boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining clear solution 1. Add 0.4 g of polyethylene glycol (molecular weight: 2000) to the clear solution 1, stop heating, keep stirring until cooled to room temperature, and then keep stirring.

[0074] Weigh 3.2g (10mmol) hafnium tetrachloride and put it into a beaker, pour 10ml of acetic acid (analytical grade, 10.5g) into it, and use a magnetic stirrer to stir at normal temperature until the hafnium tetrachloride is completely dissolved in acetic acid to obtain a solution 2. The solution is light yellow. Slowly drop the light yellow solution into solution 1 at a rate of 10 mL / min (1 m...

Embodiment 2

[0077] Weigh 2g (32mmol) of boric acid and 3g (16mmol) of sorbitol, mix them in the same beaker, then pour 20mL of acetic acid (analytical grade, 21g) into it, and use an oil bath magnetic stirrer to gradually raise the temperature to 60°C , stirring at constant temperature, until boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining clear solution 1. Add 0.8 g of polyethylene glycol (molecular weight: 2000) to the clear solution, stop heating, keep stirring until cooled to room temperature, and then continue to keep stirring.

[0078] Weigh 3.2g (10mmol) hafnium tetrachloride and put it into a beaker, pour 10ml of acetic acid (analytical grade, 10.5g) into it, and use a magnetic stirrer to stir at normal temperature until the hafnium tetrachloride is completely dissolved in acetic acid to obtain a solution 2. The solution is light yellow. Slowly drop the light yellow solution into solution 1 at a rate of 10 m...

Embodiment 3

[0081] Weigh 2g of boric acid (32mmol) and 3g of sorbitol (16mmol), mix them in the same beaker, then pour 20mL of acetic acid (analytical grade, 21g) into it, and use an oil bath magnetic stirrer to make it gradually warm up to 60°C , stirring at constant temperature, until boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining clear solution 1. Add 2 g of polyethylene glycol (molecular weight: 2000) to the clear solution, stop heating, keep stirring until cooled to room temperature, and then continue to keep stirring.

[0082] Weigh 3.2g (10mmol) hafnium tetrachloride and put it into a beaker, pour 10ml of acetic acid (analytical grade, 10.5g) into it, and use a magnetic stirrer to stir at normal temperature until the hafnium tetrachloride is completely dissolved in acetic acid to obtain a solution 2. The solution is light yellow. Slowly drop the light yellow solution into solution 1 at a rate of 10 mL / min (1...

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Abstract

The invention relates to a method for preparing hafnium boride powder. The method comprises the following steps: dissolving a hafnium source compound in a first solvent to form a first solution; dissolving a boron source compound and a carbon source compound in a second solvent, and adding polyethylene glycol to form a second solution; adding the first solution into the second solution, and collecting the generated precipitate; and drying the collected precipitate, grinding the dried precipitate into powder, and carrying out high-temperature calcination to prepare the hafnium boride powder. The preparation process is simple, the reaction process is easy to control, the production period is short, the cost is low, the prepared hafnium boride powder has high purity, small particle size, narrow particle size distribution and good microstructure, and the mechanical property and sintering driving force of a sintered body can be enhanced in the subsequent forming process.

Description

technical field [0001] The invention relates to the technical field of hafnium boride powder preparation, in particular to a method for preparing hafnium boride powder assisted by polyethylene glycol. Background technique [0002] With the continuous development of aviation, aerospace technology, and space vehicle technology, human beings can explore more vast outer space. However, in the extreme environment of outer space, the performance of many materials cannot meet the requirements. [0003] Hafnium boride (HfB 2 ), as an ultra-high temperature boride material, has high melting point, high hardness, high thermal shock resistance, high electrical conductivity and high thermal conductivity, etc. Candidate materials for components. However, HfB 2 The sintering performance of ceramic materials is severely restricted by the original powder characteristics such as purity and particle size. [0004] At present, the preparation methods of hafnium boride powder mainly include...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
CPCC01B35/04C01P2002/72C01P2004/03
Inventor 胡小晔王天旭王振胡晨光李昕扬黄竹林李越
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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