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Preparation method of high-purity high-density zirconium diboride ceramic dense body free of sintering aid

A zirconium diboride and densification technology is applied in the field of preparation of zirconium diboride ceramic dense bodies, which can solve the problems of difficult sintering and densification of ceramic powder, and achieve the effects of low manufacturing cost, high activity and simple process

Inactive Publication Date: 2012-06-20
SICHUAN INST OF MATERIALS & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the invention is to solve the problem of pure phase ZrB in the prior art 2 To solve the problem of difficult sintering and densification of ceramic powder, a method for preparing a high-purity and high-density zirconium diboride ceramic compact without sintering aids is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In this example, we take the following steps:

[0019] a. ZrB with a purity of 99.5% and an average particle size of 10 μm 2 The powder is mixed with zirconia grinding balls and grinding dispersion medium at a mass ratio of 1:8:3 and then put into a zirconia grinding jar, and Ar gas is injected into the grinding jar as a protective atmosphere during the grinding process;

[0020] b. Put the sealed grinding tank into the planetary ball mill for wet grinding, the tank speed is 200r / min, and the grinding time is 18 hours. Separation of zirconium oxide slurry, precipitation and drying of zirconium diboride slurry to obtain ZrB with an average particle size of less than 1 μm 2 High active powder;

[0021] c, the above-mentioned ZrB 2 The high-activity powder is subjected to two-step hot-pressing sintering in a vacuum atmosphere. In the first step, the heat preservation platform is set at 200°C, the vacuum degree is 5Pa, and the heat preservation is 30min; in the second st...

Embodiment 2

[0024] In this example, we take the following steps:

[0025] a. ZrB with a purity of 99.5% and an average particle size of 9 μm 2 The powder is mixed with zirconia grinding balls and grinding dispersion medium at a mass ratio of 1:10:4 and then put into a zirconia ball grinding jar, and Ar gas is injected into the grinding jar as a protective atmosphere during the grinding process;

[0026] b. Put the sealed grinding tank into the planetary ball mill for wet grinding. The rotating speed of the tank is 220r / min, and the grinding time is 19 hours. Separation of zirconium oxide slurry, precipitation and drying of zirconium diboride slurry to obtain ZrB with an average particle size of less than 1 μm 2 High active powder;

[0027] c, the above-mentioned ZrB 2 The high-activity powder is subjected to two-step hot-pressing sintering in a vacuum atmosphere. In the first step, the heat preservation platform is set at 220°C, the vacuum degree is 2Pa, and the heat preservation is 30...

Embodiment 3

[0030] In this example, we take the following steps:

[0031] a. ZrB with a purity of 99.5% and an average particle size of 12 μm 2 The powder is mixed with zirconia grinding balls and grinding dispersion medium at a mass ratio of 1:9:3 and then put into a zirconia grinding jar, and Ar gas is injected into the grinding jar as a protective atmosphere during the grinding process;

[0032] b. Put the sealed grinding tank into the planetary ball mill for wet grinding, the tank speed is 260r / min, and the grinding time is 22 hours. Separation of zirconium oxide slurry, precipitation and drying of zirconium diboride slurry to obtain ZrB with an average particle size of less than 1 μm 2 High active powder;

[0033] c, the above-mentioned ZrB 2 The high-activity powder is subjected to two-step hot-pressing sintering in a vacuum atmosphere. In the first step, the heat preservation platform is set at 240°C, the vacuum degree is 5Pa, and the heat preservation is 30min; in the second step...

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Abstract

The invention relates to a preparation method of a high-purity high-density zirconium diboride ceramic dense body free of a sintering aid, relates to a preparation of a zirconium diboride ceramic dense body, and aims at solving the problem that pure ZrB2 ceramic powder is difficult to sinter and densify in the prior art. The preparation method comprises the steps of: mixing and placing zirconium diboride powder, zirconium dioxide grinding balls and a grinding dispersion medium in a zirconium dioxide grinding tank at a mass ratio of (1-2):(8-10):(3-4), and introducing Ar gas to the grinding tank; placing the grinding tank on a grinding machine, carrying out wet grinding, then separating zirconium dioxide grinding balls and zirconium diboride slurry, and precipitating and drying the slurry to obtain high-purity high-activity sub-microscale ZrB2 powder; and carrying out hot pressed sintering on the ZrB2 powder in vacuum, and then cooling. In the method, the sintering aid is not introduced, the sintering activity of ZrB2 ceramic powder is increased by grinding and refining, and the ZrB2 ceramic dense body with high purity, high density and uniform components and structures is preparedby a step sintering method.

Description

technical field [0001] The invention relates to a method for preparing a zirconium diboride ceramic dense body, in particular to a method for preparing high-purity and high-density zirconium diboride without sintering aids. Background technique [0002] ZrB 2 It has the advantages of extremely high melting point, strength, hardness, good electrical conductivity and thermal conductivity, good chemical stability, low thermal expansion coefficient, flame retardant, corrosion resistance and light weight, etc. It is more and more used in high-temperature structural ceramic materials, refractory materials , composite materials and nuclear control materials and other fields. [0003] ZrB 2 Research on ceramic-based materials can be traced back to the 1960's. Manlab was the first to start ZrB 2 Research on ceramic-based materials, the research object is mainly ZrB 2 and HfB2 and its composite materials, the HfB successfully developed by the hot pressing process 2 / 20vol% SiC c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626
Inventor 庞晓轩杨维才张鹏程李强刘婷婷
Owner SICHUAN INST OF MATERIALS & TECH