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Method for preparing boron-carbon-zirconium material by liquid phase process

A liquid phase method, boron carbon technology, applied in the field of structural ceramics, can solve the problems of large particle size of boron carbon zirconium powder, uneven phase distribution of complex ceramics, difficult sintering, etc., and achieve the effect of overcoming relatively expensive

Inactive Publication Date: 2008-06-25
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing ultrafine boron carbon zirconium powder by liquid phase method to solve the shortcomings of industrially prepared boron carbon zirconium powder with large particle size, difficult sintering and uneven phase distribution of multiphase ceramics

Method used

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Effect test

Embodiment 1

[0019] Dissolve 32.25g of zirconium oxychloride in 500ml of ethanol and water with a volume ratio of 4:1, and stir to dissolve it. Add 12.36g of boric acid and mix evenly, and add 3.60g of polyethylene glycol as a dispersant, then add 25vol% dilute ammonia water dropwise, adjust the pH to about 3, and form a zirconia sol. Add 20g of phenolic resin (the amount of residual carbon is about 50%, the concentration is 50vol%) to form a mixed sol. Continue to add ammonia water dropwise to make it condense. The gel was transferred to a ball mill jar, milled with zirconia as a ball mill for 24 hours, and dried at 80° C. for 12 hours to obtain a powder precursor. Calcined at 1500°C for 1 hour to obtain ZrB 2 Powder. It is obvious from the XRD pattern that ZrB 2 phase, no other intermediate phase exists. (See Figure 2) From the SEM photos, it can be seen that the powder is dispersed evenly, and the average particle size is about 50-200nm. (See Figure 5)

Embodiment 2

[0021] Dissolve 41.16g of zirconium oxychloride in 500ml of ethanol and water with a volume ratio of 4:1, and stir to dissolve it. Add 12.36g of boric acid and mix evenly, and add 4.80g of polyethylene glycol as a dispersant, then add 25vol% dilute ammonia water dropwise, adjust the pH to about 3, and form a zirconia sol. Add 23.28g of phenolic resin (the amount of residual carbon is about 50%, the concentration is 50vol%) to form a mixed sol. Continue to add ammonia water dropwise to make it condense. The gel was transferred to a ball mill jar, milled with zirconia as a ball mill for 24 hours, and dried at 80° C. for 12 hours to obtain a powder precursor. Calcined at 1500°C for 1 hour to obtain ZrB 2 -ZrC composite powder, the theoretical content of ZrC in the composite powder is 20wt%, and ZrB is clearly seen in the XRD figure 2 And ZrC phase exists, there is no other intermediate phase. (See Figure 3)

Embodiment 3

[0023] Dissolve 49.99g of zirconium oxychloride in 500ml of ethanol and water with a volume ratio of 4:1, and stir to dissolve it. Add 12.36g of boric acid and mix evenly, and add 4.90g of polyethylene glycol as a dispersant, then add 25vol% dilute ammonia water dropwise, adjust the pH to about 3, and form a zirconia sol. Add 26.55g of phenolic resin (the amount of residual carbon is about 50%, the concentration is 50vol%) to form a mixed sol. Continue to add ammonia water dropwise to make it condense. The gel was transferred to a ball mill jar, milled with zirconia as a ball mill for 24 hours, and dried at 80° C. for 12 hours to obtain a powder precursor. Calcined at 1500°C for 1 hour to obtain ZrB 2 -ZrC composite powder, the theoretical content of ZrC in the composite powder is 50wt%.

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Abstract

The invention relates to a method for preparing boron carbon zirconium materials by liquid phase method, which belongs to the field of structural ceramics. By using carbothermal reduction as the basic principle and adopting zirconium oxychloride, boric acid and phenolic resin as the main materials, the method comprises the steps as follows: the phenolic resin is mixed with zirconia sol which is formed by titration of ammonia; then gel is formed by the titration of the ammonia; finally ball milling is carried out; after drying, screening and heat treatment, the ultrafine boron carbon zirconium materials can be obtained. The boron carbon zirconium materials which are prepared by the invention, with product granularity smaller than 200nm and excellent molding and sintering performance, can be applied to fields such as electron materials and refractory materials.

Description

technical field [0001] The invention relates to a method for preparing a boron carbon zirconium material by a liquid phase method, belonging to the field of structural ceramics. Background technique [0002] ZrB 2 Both ZrC and ZrC have high melting point, high modulus, high hardness, high thermal conductivity and electrical conductivity, no phase change and good thermal shock resistance, especially ZrB 2 With comprehensive characteristics such as extremely strong chemical bonds, low saturated vapor pressure, and low high-temperature thermal expansion coefficient, zirconium boride-zirconium carbide and its composite ceramics have become potential candidate materials for high-temperature structural applications, and are expected to be used in composite materials, refractory materials, and electrode materials. and other fields have been applied. [0003] At present, the industrial preparation of ZrB 2 The solid-phase method and gas-phase method are mostly used for ZrC and Zr...

Claims

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Application Information

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IPC IPC(8): C01B31/32C01B35/04C04B35/56C04B35/58C04B35/624C04B35/66C01B32/942
Inventor 闫永杰黄政仁刘学建董绍明
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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