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A method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling

A grinding aid, zirconium boride technology, applied in the field of zirconium boride powder preparation, can solve the problem that the particle size, purity and output of zirconium boride powder cannot meet scientific research and production, long production cycle and other problems, and achieve enhanced sintering. The effect of driving force, short production cycle and simple preparation process

Active Publication Date: 2022-04-01
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 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 method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling
  • A method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling
  • A method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0036] (1) In step A, the amount of oleic acid used is 1-20% of the total volume of the clear solution.

[0037] (2) In step C, the grinding into powder is to perform ball milling on 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 boride Zirconium precursor gel changed from block to powder.

[0038] (3) In step C, the calcination uses high-purity argon (Ar ≥ 99.999%) as a protective gas, and the debinding furnace is heated from room temperature to 400-600°C at a rate of 1-5°C / min , keep warm for 10-120 minutes, then raise the temperature to 600-800 ℃ at a rate of 1-5 ℃ / min, keep warm for 10-120 minutes, and then cool naturally to room temperature. This calcination process can remove the organic matter in the zirconium boride precursor gel powder, making the subsequent high-temperature calcination products more uniform.

[0039](4) In step D, the grinding aid is a chlorine-containing organic...

Embodiment 1

[0051] A method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling may include the following steps:

[0052] 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. Add 0.6mL oleic acid to the clarified solution, stop heating, continue to stir until cooled to room temperature, and then slowly drop in 9.375mL zirconium n-propoxide at a constant speed of 0.5-10mL / min under continuous stirring (with time 10 min), thereby preparing the zirconium boride precursor sol.

[0053] Step b1, sealing the zirconium boride precursor sol, putting it into a constant temperature bo...

Embodiment 2

[0058] A method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling may include the following steps:

[0059] 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. Add 0.6mL oleic acid to the clarified solution, stop heating, continue to stir until cooled to room temperature, and then slowly drop in 9.375mL zirconium n-propoxide at a constant speed of 0.5-10mL / min under continuous stirring (with time 10 min), thereby preparing the zirconium boride precursor sol.

[0060] Step b2, sealing the zirconium boride precursor sol, putting it into a constant temperature bo...

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Abstract

The invention discloses a method for preparing high-purity ultrafine zirconium boride powder by grinding aid-assisted sand milling. Acetic acid, boric acid and sorbitol are mixed together, stirred and dissolved at a constant temperature to obtain a clear solution; the clear solution is cooled to room temperature, Drop in zirconium n-propoxide at a constant speed to prepare zirconium boride precursor sol; seal the zirconium boride precursor sol to make it fully gel to obtain zirconium boride precursor gel; gel the zirconium boride precursor The glue is dried and ground into powder, and then calcined in the debinding furnace to obtain inorganic dry powder; the inorganic dry powder and grinding aid are made into a suspension, and then poured into a sand mill for sand grinding to obtain superfine Inorganic dry powder slurry: dry the ultrafine inorganic dry powder slurry, and then put it into a high-temperature tube furnace for high-temperature calcination to obtain high-purity ultrafine zirconium boride powder. The zirconium boride powder prepared by the invention has higher purity, finer particle size and good microscopic appearance, and can enhance the mechanical properties and sintering driving force of the sintered body in the subsequent molding process.

Description

technical field [0001] The invention relates to the technical field of zirconium boride powder preparation, in particular to a method for preparing high-purity ultrafine zirconium boride powder (the ultrafine in this paper refers to a particle size diameter of 100nm to 1000nm) assisted by grinding aids. Background technique [0002] Zirconium boride (ZrB 2 ) has a high melting point (3245°C), high thermal conductivity (57.9W·m -1 ·K -1 ), low thermal expansion coefficient (5.9×10 -6 / °C) and good stability in extreme environments, so zirconium boride is an important strategic ultra-high temperature ceramic material. Zirconium boride has strong covalency, which makes it have excellent mechanical properties (such as high hardness, high bending strength) and good thermal shock and oxidation resistance, so zirconium boride ceramics become supersonic aircraft, return Potential candidate materials for aircraft and rocket propulsion. It has been reported that because zirconium...

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 陈本松胡晨光黄竹林胡小晔李昕扬李越
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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