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High purity zirconium boride / hafnium boride and preparation of superhigh temperature ceramic target material

A technology of ultra-high temperature ceramics and targets, which is applied in the preparation of high-purity ultra-high-temperature ceramic targets and the field of hot-pressing preparation of high-purity zirconium boride ZrB2/hafnium boride HfB2 ultra-high temperature ceramic targets, which can solve the problem of ceramic body strength and density Poor uniformity, it is difficult to obtain dense ceramic body, reduce material purity, etc., to achieve uniform density, improve mixing efficiency, and increase sintering temperature

Active Publication Date: 2012-06-20
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ceramic body prepared by this method reduces the purity of the material because of the need to add a sintering aid; in addition, due to pressureless sintering, it is difficult to obtain a high-density ceramic body, and the strength and density uniformity of the ceramic body are relatively poor. , it is difficult to apply to the sputtering process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Take Zr powder with an average particle size of 30μm (purity of 99.9%) and B powder with an average particle size of 8μm (purity of 99%), wet and mix uniformly according to the atomic ratio of 1.03∶2, dry and press the compact, put Put it in a graphite crucible, place it in a vacuum furnace, use tungsten wire to ignite, a self-propagating high-temperature synthesis reaction occurs. After the reaction is completed, the system is cooled, the reaction product is taken out, and after mechanical crushing, a purity close to 99.8% with an average particle size of about 50μm is obtained ZrB 2 Powder.

[0035] 2. Weigh more than a certain amount of ZrB 2 The powder is placed in a graphite mold with a workpiece size of 100×100mm, and after cold pressing, it is placed in a hot pressing furnace. Vacuum to 1×10 -1 After Pa, start to heat up to 1200°C and keep the temperature for 30min; then simultaneously heat up, fill with Ar gas, pressurize, heat up to 1750°C, the pressure is 20 t...

Embodiment 2

[0037] Weigh the same amount of ZrB prepared in Example 1 2 The powder is placed in a graphite mold with a workpiece size of 100×100mm, and after cold pressing, it is placed in a hot pressing furnace. Vacuum to 1×10 -1 After Pa, start to heat up to 1200°C and keep the temperature for 30min; then simultaneously heat up, fill with Ar gas, pressurize, heat up to 1850°C, the pressure is 30 tons, after keeping the pressure for 2 hours, turn off the heating power, start to cool down, and the temperature drops When the temperature reaches 1400°C, the pressure is released. After 13 hours of cooling, the temperature in the furnace drops to 70°C and the material is discharged. Then the blank is ground, cleaned and vacuum dried. The purity analysis of the target material is greater than 99.5%, and the density is greater than 6.0g / cm 3 , The relative density is greater than 98%.

Embodiment 3

[0039] 1. Take Hf powder (purity of 99.9%) with an average particle size of 50μm and B powder (purity of 99%) with an average particle size of 8μm, wet and mix uniformly according to the atomic ratio of 1.01∶2, dry the compact and put it into the graphite crucible , Placed in a vacuum furnace, ignited by W wire, a self-propagating high-temperature synthesis reaction occurs. After the reaction is completed, the system is cooled, the reaction product is taken out, and after mechanical crushing, HfB with a purity of close to 99.8% and an average particle size of about 70 μm is obtained 2 Powder.

[0040] 2. Weigh more than a certain amount of HfB 2 The powder is placed in a graphite mold with a workpiece size of 100×100mm, and after cold pressing, it is placed in a hot pressing furnace. Vacuum to 1×10 -1 After Pa, start to heat up, to 1300℃, keep for 30min; then at the same time, heat up, fill with Ar gas, pressurize, heat up to 1800℃, the pressure is 20 tons, after keeping the press...

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Abstract

The invention discloses a method for preparing a high-purity ultrahigh-temperature ceramic target material which belongs to the technical field of ceramic target materials, and in particular provides a method for preparing high-purity zirconium / hafnium boride powder and a ceramic target material thereof. The method comprises the steps of taking high-purity Zr powder, Hf powder and high-purity B powder as raw materials, adopting a self-propagating method to prepare high-purity ZrB2 and HfB2 powder respectively and then adopting a high-temperature high-pressure hot-pressing molding process to prepare a high-purity dense zirconium / hafnium boride ultrahigh-temperature ceramic target material, wherein the relative density of the target material reaches 95 to 99 percent. Relative to the prior art, metal powder in the method is slightly excessive when the materials are mixed, so as to make up for the metal loss during self-propagating reaction and further guarantee the component unicity of products. Relative to pressureless sintering, the sintering temperature needed in the method is greatly lowered; in addition, as the hot-pressing process adopts two-stage temperature, blank is uniform in temperature field, so as to ensure that the target material with uniform density can be obtained in the late hot-pressing process.

Description

Technical field [0001] The invention belongs to a method for preparing a high-purity ultra-high temperature ceramic target material, specifically high-purity zirconium boride ZrB 2 / Hafnium Boride HfB 2 The hot pressing preparation method of ultra-high temperature ceramic target material belongs to the technical field of ceramic target material. Background technique [0002] Ultra-High Temperature Ceramics (UHTCS) is a type of ceramics: due to their unique characteristics such as high melting point, high strength, high hardness, good oxidation resistance and flame retardancy, they are widely used in aerospace And other technical fields, this type of ceramics mainly include ZrB 2 , HfB 2 , ZrC, HfC and composite ceramic materials based on them. With the continuous progress of modern industry, thin film technology and thin film materials have been developed rapidly, and have achieved fruitful results in both academic and practical applications, and have become the most active in co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/626C04B35/58C04B35/645
Inventor 储茂友王星明邓世斌韩沧张碧田段华英张明贤龚述荣潘德明
Owner 有研资源环境技术研究院(北京)有限公司
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