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High purity ultra fine zirconium biboride powder and its preparation method

A zirconium diboride and diboride technology is applied in the field of low-cost preparation of high-purity ultra-fine zirconium diboride powder, which can solve the problems of incompleteness, many impurities and low product purity, and achieves high yield, high purity, Efficient effect

Active Publication Date: 2007-04-18
칭다오정왕철강수통제주식유한회사
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Method 1 is simple in process, short in time, low in energy consumption, and high in activity of the synthetic powder, but because the reaction speed is too fast, the reaction may sometimes be incomplete, and there will be correspondingly more impurities, and its reaction process, product structure and performance not easy to control
Method 2 is more suitable for industrial mass production, but its disadvantage is that it is easier to introduce impurities and the purity of the prepared product is not high
Method 3 Usually, the reaction is not easy to complete, the product particles are large, the activity is not high, and it is not conducive to post-processing
Method 4 is limited by expensive raw materials, and often the product activity is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The selected formula is: ZrOCl 2 :B 4 C:C=1:0.5:1.5 (molar ratio). First, weigh B according to the recipe 4 C and carbon powder, put in a beaker, according to solid: H 2 Add deionized water at a ratio of O=1:50, adjust its pH value to 2-5, and then stir and disperse for 30 minutes. Take another beaker, weigh zirconium oxychloride according to the formula, press zirconium oxychloride: H 2 Add deionized water at a ratio of O=1:80 to fully dissolve the zirconium oxychloride to obtain a transparent solution. will disperse after B 4 Mix the suspension of C and carbon powder with the zirconium oxychloride solution, stir it with magnetic force, and add 25% ammonia water drop by drop to the mixed solution while stirring, so that the zirconium oxychloride is fully hydrolyzed and precipitated until the pH value is greater than 9 . Then the suspension was suction filtered and washed with water three times. Then put it into an oven and fully dry it at 100°C. Pass the dried...

Embodiment 2

[0030] The selected formula is: ZrOCl 2 :B 4 C:C=1:0.55:1.5 (molar ratio). First, weigh B according to the recipe 4 C and carbon powder, put in a beaker, according to solid: H 2 Add deionized water at a ratio of O=1:60, adjust its pH value to 2-5, and then stir and disperse for 1 hour. Take another beaker, weigh zirconium oxychloride according to the formula, press zirconium oxychloride: H 2 Add deionized water at a ratio of O=1:60 to fully dissolve the zirconium oxychloride to obtain a transparent solution. will disperse after B 4 Mix the suspension of C and carbon powder with the zirconium oxychloride solution, stir it with magnetic force, and add 25% ammonia water drop by drop to the mixed solution while stirring, so that the zirconium oxychloride is fully hydrolyzed and precipitated until the pH value is greater than 9 . Then the suspension was suction filtered and washed with water three times. Then put it into an oven and fully dry it at 100°C. Pass the dried po...

Embodiment 3

[0032] The selected formula is: ZrOCl 2 :B 4 C:C=1:0.6:1.65 (molar ratio). First, weigh B according to the recipe 4 C and carbon powder, put in a beaker, according to solid: H 2 Add deionized water at a ratio of O=1:80, adjust its pH value to 2-5, and then stir and disperse for 1 h. Take another beaker, weigh zirconium oxychloride according to the formula, press zirconium oxychloride: H 2 Add deionized water at a ratio of O=1:50 to fully dissolve the zirconium oxychloride to obtain a transparent solution. will disperse after B 4Mix the suspension of C and carbon powder with the zirconium oxychloride solution, stir it with magnetic force, and add 25% ammonia water drop by drop to the mixed solution while stirring, so that the zirconium oxychloride is fully hydrolyzed and precipitated until the pH value is greater than 9 . Then the suspension was suction filtered and washed with water three times. Then put it into an oven and fully dry it at 80°C. Pass the dried powder ...

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PUM

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Abstract

The present invention relates to a high-purity ultrafine zirconium diboride powder material and its preparation method. It is characterized by that the described powder material contains zirconium oxychloride, boron carbide powder and active carbon powder, their mole ratio is ZrOcl2:B4C:C=1:0.4-0.8:1.4-1.8. Its preparation method includes the following steps: firstly, mixing boron carbide powder, active carbon powder and water according to mixing ratio, regulating pH value to obtain mixed suspension; dissolving zirconium oxychloride in deionized water to obtain the zirconium oxychloride solution; mixing the above-mentioned suspension and zirconium oxychloride solution, adding ammonia water, making the zirconium oxychloride be fully hydrolyzed and precipitated; making suspension undergo the processes of solid-liquor separation, waster-washing, removing NH4+ and Cl-, drying and sieving; then placing the powder material into a vacuum furnace to make reaction synthesis, its synthesis temperature is 1500-1600 deg.C, heat-insulating for 0.5-4 h; grinding powder and sieving so as to obtain the invented powder material.

Description

technical field [0001] The invention relates to a low-cost preparation of high-purity ultrafine zirconium diboride (ZrB 2 ) powder and a method thereof, belonging to the field of ceramic materials. Background technique [0002] Zirconium diboride (ZrB 2 ) has the characteristics of high melting point, high hardness, good electrical and thermal conductivity, good flame retardancy, heat resistance, oxidation resistance, and corrosion resistance. , Electrode materials for smelting metals and many other fields have very broad application prospects. [0003] At present, there are four main methods for preparing this zirconium diboride powder: the first method is self-propagating high-temperature synthesis (SHS) (document 1: Chinese invention patent: 200510010014); the second method is zirconium dioxide boron reduction method (document 2: J.Am.Ceram.Soc., 78[9] 2534-36 (1995)); the third method is the electrolysis containing metal oxide and B 2 o 3 The molten salt bath method...

Claims

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Application Information

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IPC IPC(8): C01B35/04C04B35/58C04B35/626
Inventor 汪长安王海龙方岱宁黄勇
Owner 칭다오정왕철강수통제주식유한회사
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