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Preparation of nano zirconium diboride ceramic powder

A technology of zirconium diboride and ceramic powder is applied in the field of preparation of nano-zirconium diboride ceramic powder, which can solve the problems of difficult removal, slow reaction process, coarse product particles, etc. Rapid effect of the preparation process

Inactive Publication Date: 2009-07-22
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages are that the reaction process is slow, the time is long, the reaction conversion rate is not high, more impurities are easy to remain, the by-product components are complex and difficult to remove, the reaction depends on high temperature, the energy consumption is large, and the product particles are coarse (average particle size Usually up to more than ten microns), low activity
This method effectively reduces the ZrB 2 The synthetic temperature and the obtained powder particles are fine, but there are shortcomings such as long reaction time and high energy consumption, and long-term ball milling is easy to introduce impurities
[0006] As can be seen from the above analysis, the existing ZrB 2 Ceramic powder synthesis methods have shortcomings such as low synthesis efficiency, energy consumption, and time consumption to varying degrees. The synthesized ZrB 2 Ceramic powders tend to be coarse, low in activity or high in impurities that are difficult to remove

Method used

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  • Preparation of nano zirconium diboride ceramic powder
  • Preparation of nano zirconium diboride ceramic powder
  • Preparation of nano zirconium diboride ceramic powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Zirconium oxychloride is selected as Zr source, and the molar ratio of Zr to amorphous boron powder in zirconium oxychloride is 1:3. Disperse 1.02g of amorphous boron powder in 100ml of distilled water (molar concentration is 0.3mol / L), adjust the pH value to 8 with a concentration of ammonia solution of 5mol / L, add 0.0102g of sodium dodecylbenzenesulfonate (SDBS ), magnetically stirred for 1 h to obtain an amorphous boron powder suspension; weigh 9.668 g of zirconium oxychloride and prepare a 0.3mol / L solution according to the formula, and add the prepared zirconium oxychloride solution to obtain the amorphous boron powder suspension Mix and magnetically stir for 1 hour to obtain a mixed solution; add dropwise ammonia water with a concentration of 5 mol / L to the mixed solution in a constant temperature water bath at 60°C until the pH value is 9, and magnetically stir for 6 hours to obtain a slurry; filter the slurry and wash with water , until no Cl is detected - So f...

Embodiment 2

[0031] Zirconium oxychloride is selected as Zr source, and the molar ratio of Zr to amorphous boron powder in zirconium oxychloride is 1:5. First weigh 1.70 g of amorphous boron powder after refinement (average particle size of amorphous boron powder is less than 200nm) according to the formula, put it into a beaker, and disperse amorphous boron powder in 100ml deionized water (molar concentration is 0.5mol / L), with a concentration of 10mol / L ammonia solution to adjust the pH value to 9, add 0.034g sodium dodecylbenzenesulfonate (SDBS), and magnetically stir for 1h to obtain a suspension of amorphous boron powder; take another beaker According to the formula, take 9.668g of zirconium oxychloride, prepare a 0.3mol / L solution of zirconium oxychloride, add the prepared zirconium salt solution into the suspension of amorphous boron powder and mix, and stir magnetically for 1h to obtain a mixed solution; Add ammonia water with a concentration of 10mol / L to the mixed solution dropw...

Embodiment 3

[0033] Zirconium oxychloride is selected as the Zr source, and the molar ratio of Zr to amorphous boron powder in zirconium oxychloride is 1:4. First weigh 1.27g of amorphous boron powder after refinement (the average particle size of amorphous boron powder is less than 200nm) according to the formula, put it into a beaker, and disperse the amorphous boron powder in 100ml deionized water (molar concentration is 0.4mol / L), with a concentration of 8mol / L ammonia solution to adjust the pH value to 8, add 0.01905g SDBS, and magnetically stir for 1h to obtain a suspension of amorphous boron powder; take another beaker, weigh zirconium oxychloride according to the formula, and Prepare a 0.3mol / L solution of zirconium oxychloride, add the prepared zirconium salt solution to the suspension of amorphous boron powder and mix, stir magnetically for 1 hour to obtain a mixed solution; add 8mol / L of ammonia solution to fully hydrolyze and precipitate the zirconium salt until the pH value ...

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Abstract

The invention relates to a preparation method for nano zirconium diboride ceramic powder, which is characterized by comprising the following steps: 1) selecting materials: selecting according to a mol ratio of 1 : 3 to 1 : 5 between Zr and amorphous boron powder in soluble zirconium salt; 2) selecting one of the two methods as follows: a) using a coprecipitation method for gel forming to obtain xerogel; b) using a sol-gel method for gel forming to form the xerogel; 3) preparing precursor powder; 4) synthesizing quickly: arranging the materials into a large current reaction synthesizer; the inside of a black lead reactor is protected by vacuum or insert gases; applying a large current directly on the black lead reactor, quickly heating to 800 and 1500 DEG C at the temperature rising speed of 50 to 500 DEG C / min, preserving the temperature for 0 to 60 minutes to obtain a powder sample; and 5) chemical processing for obtaining the nano zirconium diboride ceramic powder. The method has the characteristics of quick synthesizing speed and high efficiency; the purity of the obtained nano zirconium diboride ceramic powder is high (equal to or more than 95 percent); and the grain diameters of the obtained nano zirconium diboride ceramic powder are uniform and thin(the average grain diameter is equal to or less than 300nm).

Description

technical field [0001] The invention relates to a method for preparing nano-zirconium diboride ceramic powder, which belongs to the field of non-oxide nano-ceramic material powder preparation. Background technique [0002] Zirconium boride is the main and common material in boride. There are two zirconium borides with different compositions in the boron-zirconium system: zirconium monoboride (ZrB), zirconium diboride (ZrB 2 ), zirconium dodecaboride (ZrB 12 ), where ZrB 2 It is stable in a wide temperature range, zirconium boride produced in industrial production and the current application is mostly ZrB 2 as the main ingredient. ZrB 2 It is a metalloid structure compound of type C32 in the hexagonal system. The Zr-B ionic bond between the boron atomic plane and the zirconium atomic plane and the strong bond of the B-B covalent bond determine the high melting point, high hardness and stability of this material . Because zirconium diboride ceramics have the characteris...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C01B35/04
Inventor 王皓孙歌王为民傅正义王玉成张清杰
Owner WUHAN UNIV OF TECH
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