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A kind of oleic acid assists the method for preparing zirconium boride powder

A technology of zirconium boride and oleic acid, which is applied in the field of oleic acid-assisted preparation of zirconium boride powder, can solve the problems that the particle size, purity and output of zirconium boride powder cannot meet scientific research and production, and the production cycle is long. Enhanced sintering driving force, short production cycle, high purity effect

Active Publication Date: 2022-04-29
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these preparation methods are generally completed under relatively harsh conditions, and the production cycle is long, and the particle size, purity, and output of the zirconium boride powder produced cannot meet the needs of scientific research and production.

Method used

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  • A kind of oleic acid assists the method for preparing zirconium boride powder
  • A kind of oleic acid assists the method for preparing zirconium boride powder
  • A kind of oleic acid assists the method for preparing zirconium boride powder

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0031] (1) In step A, the amount of oleic acid is 1%-20% of the total volume of the clear solution. The morphology of the final zirconium boride powder can be controlled by adjusting the amount of oleic acid; when the amount of oleic acid is 1% to 4% of the total volume of the clear solution, the more the amount of oleic acid is, the final The smaller the particle size of the zirconium boride powder produced, the more spherical the microscopic appearance; when the amount of the oleic acid is 4% to 20% of the total volume of the clear solution, the more The particle size of the final zirconium boride powder is larger.

[0032] (2) In step C, the grinding into powder can be performed by ball milling the dried zirconium boride precursor gel, the ball milling speed is 50-400rpm, and the ball milling time is 0.5-4h, so that the dried boron The zirconium precursor gel changed from block to powder.

[0033] (3) In step C, the high-temperature calcination uses high-purity argon (Ar ...

Embodiment 1

[0042] A method for preparing zirconium boride powder assisted by oleic acid may comprise the following steps:

[0043] Step a1. Weigh 3.875g of boric acid and 6.875g of sorbitol, put them into the same beaker and mix them, then pour 30mL of acetic acid (analytical pure) into it, and use an oil bath magnetic stirrer to gradually raise the temperature to 60°C, and stir at a constant temperature , until the boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining a clear solution.

[0044] Step b1, add 0.6mL oleic acid to the clarified solution, stop heating, keep stirring until it cools down to room temperature, then slowly drop in 9.375mL n-propanol at a constant rate of 0.5-10mL / min under continuous stirring zirconium (taking 10 minutes), so as to prepare zirconium boride precursor sol.

[0045] Step c1, sealing the zirconium boride precursor sol, putting it into a constant temperature box, and placing it at a con...

Embodiment 2

[0049] A method for preparing zirconium boride powder assisted by oleic acid may comprise the following steps:

[0050] Step a2, weigh 3.875g of boric acid and 6.875g of sorbitol, put them into the same beaker and mix them, then pour 30mL of acetic acid (analytical pure) into it, and use an oil bath magnetic stirrer to gradually raise the temperature to 60°C, and stir at a constant temperature , until the boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining a clear solution.

[0051] Step b2, add 1.2mL oleic acid to the clear solution, stop heating, continue to stir until it cools to room temperature, and then slowly drop in 9.375mL n-propanol at a constant speed of 0.5-10mL / min under continuous stirring zirconium (taking 10 minutes), so as to prepare zirconium boride precursor sol.

[0052] Step c2, sealing the zirconium boride precursor sol, putting it into a constant temperature box, and placing it at a co...

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Abstract

The invention discloses a method for preparing zirconium boride powder assisted by oleic acid. Acetic acid, boric acid and sorbitol are mixed together and stirred at a constant temperature so that the boric acid and sorbitol are completely dissolved in acetic acid to obtain a clear solution; Add oleic acid to the clarified solution, cool to room temperature, and then drop zirconium n-propoxide into it at a constant speed to obtain a zirconium boride precursor sol; seal the zirconium boride precursor sol, and place it under constant temperature conditions for a certain period of time , so that it is fully gelled, so that the zirconium boride precursor gel is obtained; the zirconium boride precursor gel is dried, and ground into powder, and then put into a high-temperature tube furnace for high-temperature calcination, thereby producing Zirconium boride powder was obtained. The invention not only has simple preparation process, easy control of reaction process, short production cycle and low cost, but also the prepared zirconium boride powder has high purity, fine particle size and good microscopic appearance, and can be formed in subsequent The mechanical properties and sintering driving force of the sintered body are enhanced during the process.

Description

technical field [0001] The invention relates to the technical field of zirconium boride powder preparation, in particular to a method for preparing zirconium boride powder with oleic acid assistance. Background technique [0002] With the development of aerospace, aviation, atomic energy and other technologies, the performance of materials serving in ultra-high temperature environments needs to be continuously improved to adapt to harsh service conditions. [0003] Zirconium boride (ZrB 2 ) As a member of the ultra-high temperature material family, it has high melting point, high hardness, high thermal shock resistance, high electrical conductivity and high thermal conductivity, etc. Candidate materials for components under service conditions. However, ZrB 2 The sintering performance of ceramic materials is severely restricted by the original powder characteristics such as powder particle size and purity. [0004] At present, the preparation methods of zirconium boride p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/624C04B35/626C04B35/63C04B35/632
CPCC04B35/58078C04B35/62605C04B35/624C04B35/6261C04B35/632C04B35/6325C04B35/6303C04B2235/5445C04B2235/3409
Inventor 胡晨光黄竹林陈本松胡小晔李昕扬李越
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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