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

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

Active Publication Date: 2009-07-01
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. With Zr powder (purity: 99.9%) with an average particle size of 30 μm and B powder (purity: 99%) with an average particle size of 8 μm, wet-mix evenly at an atomic ratio of 1.03:2, compact after drying, and put into a graphite crucible, placed in a vacuum furnace, ignited by a tungsten wire, and a self-propagating high-temperature synthesis reaction occurs. After the reaction is completed and the system is cooled, the reaction product is taken out, and after mechanical crushing, a purity of about 99.8% is obtained. ZrB 2 Powder.

[0035] 2. Weigh a certain amount of ZrB 2 powder, placed in a graphite mold with a workpiece size of 100×100mm, and placed in a hot-press furnace after cold pressing. Vacuum down to 1×10 -1 After Pa, start to heat up to 1200°C and keep it warm for 30 minutes; then raise the temperature, fill with Ar gas, and pressurize at the same time, raise the temperature to 1750°C, and the pressure is 20 tons. When the temperature reached 1500°C, th...

Embodiment 2

[0037] Take by weighing the ZrB that same amount embodiment one makes 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 down to 1×10 -1 After Pa, start to heat up to 1200°C and keep it warm for 30 minutes; then simultaneously raise the temperature, fill with Ar gas, and pressurize to 1850°C with a pressure of 30 tons. After holding the heat for 2 hours, turn off the heating power supply and start to cool down. When the temperature reached 1400°C, the pressure was released. After cooling for 13 hours, the temperature in the furnace dropped to 70°C and the material was discharged. The blank is then ground, cleaned and vacuum dried. The purity analysis of the target 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. Mix Hf powder with an average particle size of 50 μm (purity: 99.9%) and B powder (purity: 99%) with an atomic ratio of 1.01:2, dry and press into a graphite crucible , placed in a vacuum furnace, ignited by W wire, and a self-propagating high-temperature synthesis reaction occurs. After the reaction is completed and the system is cooled, the reaction product is taken out, and after mechanical crushing, HfB with a purity of nearly 99.8% and an average particle size of about 70 μm is obtained. 2 Powder.

[0040] 2. Weigh a certain amount of HfB 2 powder, placed in a graphite mold with a workpiece size of 100×100mm, and placed in a hot-press furnace after cold pressing. Vacuum down to 1×10 -1 After Pa, start to heat up to 1300°C and keep it warm for 30 minutes; then simultaneously raise the temperature, fill with Ar gas, and pressurize to 1800°C with a pressure of 20 tons. After holding the heat for 2 hours, turn off the heating power supply and start to cool down. ...

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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 preparation method of high-purity ultra-high temperature ceramic target material, specifically high-purity zirconium boride ZrB 2 / hafnium boride HfB 2 The invention relates to a hot-press preparation method of an ultra-high temperature ceramic target, belonging to the technical field of ceramic targets. Background technique [0002] Ultra-High Temperature Ceramics (UHTCS) is a class of ceramics that are widely used in aerospace due to their unique characteristics such as high melting point, high strength, high hardness, good oxidation resistance and flame retardancy. and other technical fields, such ceramics mainly include ZrB 2 , HfB 2 , ZrC, HfC and their composite ceramic materials. With the continuous progress of modern industry, thin-film technology and thin-film materials have developed rapidly, and have achieved fruitful results both in academics and in practical applications, and have become the most active fiel...

Claims

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Application Information

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Patent Type & Authority Applications(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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