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Method for preparing Hf3AIN ceramic material through in-situ reaction

A ceramic material and in-situ reaction technology, which is applied in the field of preparation of high-temperature structural ceramics, can solve the problems of impractical hafnium-aluminum-nitrogen ceramic materials and achieve good damage tolerance

Inactive Publication Date: 2010-09-08
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses Hf powder, Al powder and AlN powder or Hf powder, Al powder and HfN powder as raw materials, and synthesizes high-purity hafnium aluminum nitrogen (Hf 3 AlN) powder or bulk material, which can solve the problems that the hafnium aluminum nitrogen ceramic material prepared by the prior art is not practical

Method used

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  • Method for preparing Hf3AIN ceramic material through in-situ reaction
  • Method for preparing Hf3AIN ceramic material through in-situ reaction
  • Method for preparing Hf3AIN ceramic material through in-situ reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The raw materials are 100.0 grams of Hf powder, 0.5 grams of Al powder, and 7.2 grams of AlN powder with a particle size of about 400 meshes. They are ball milled for 10 hours, cold-pressed into a cake shape under a pressure of 5 MPa for 10 minutes, and put into graphite molds. , in a hot-press furnace with an inert gas (argon) as a protective gas at a rate of 10°C / min to 1400°C for 1 hour in-situ reaction to synthesize a powder ceramic material, the particle size of the obtained synthetic powder ceramic material is 10 μm. The reaction product is mainly Hf by X-ray diffraction analysis 3 AlN, in addition to small amounts of HfN and HfO 2 Impurities are present. The corresponding X-ray diffraction patterns are listed in the attached figure 1 superior.

Embodiment 2

[0022] The raw materials are 100.0 grams of Hf powder, 7.2 grams of Al powder, and 53.9 grams of HfN powder with a particle size of about 400 mesh. They are ball milled for 15 hours and cold pressed into a cake shape under a pressure of 15 MPa. The cold pressing time is 20 minutes and put into a graphite mold. , in a hot-press furnace with inert gas (argon) as a protective gas, the temperature was raised to 1600 °C at a rate of 15 °C / min for 2 hours, and the hot-pressing pressure was 30 MPa to synthesize a bulk ceramic material. The size of the hafnium aluminum nitrogen block material is Φ25mm×5mm. The reaction product is mainly Hf by X-ray diffraction analysis 3 AlN. The corresponding SEM photographs are listed in the attached figure 2 superior. The reaction product has a strong damage tolerance. The corresponding intensity curves are listed in the attached image 3 superior.

Embodiment 3

[0024] The raw materials are 100.0 grams of Hf powder, 1.1 grams of Al powder, and 8.2 grams of AlN powder with a particle size of about 200 meshes. They are ball-milled for 20 hours and cold-pressed into cakes under a pressure of 10 MPa for 5 minutes. Then, they are put into graphite molds. , under vacuum (the degree of vacuum is 10 -2 Pa) in a hot pressing furnace with a heating rate of 20 ° C / min to 1500 ° C in situ reaction hot pressing for 1 hour, and the hot pressing pressure is 40 MPa to synthesize a bulk ceramic material. The obtained hafnium aluminum nitrogen block material has a size of Φ50mm ×10mm. The reaction product is mainly Hf by X-ray diffraction analysis 3 AlN.

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Abstract

The invention relates to the preparation technology of high-temperature structural ceramics and particularly provides a method for preparing Hf3AlN ceramic material through in-situ reaction, solving the problem that currently, Hf3AIN ceramic material is difficult to prepare and is impractical. The method includes the steps of: taking Hf powder, Al powder and AlN powder or Hf powder, Al powder and HfN powder at certain stoichiometric proportion as raw materials; ball-milling the raw materials for 5-50h and cold-briquetting the raw materials under 5-20MPa; putting the briquette into a graphite mould; heating at the temperature rising rate of 2-50 DEG C / min in a hot pressing furnace filled with inert gas (such as argon) serving as shielding gas (or under vacuum condition) until the temperature reaches 1,200-1,600 DEG C; and allowing in-situ reaction for 0.1-2h. The hot pressing pressure during the process of preparing the briquette is 20-40MPa and the pressure during the process of preparing the powder is zero. The briquette prepared through the method has good breakage tolerance and can be used under the environment within temperature range of room temperature to the high temperature of 1,400 DEG C.

Description

technical field [0001] The invention relates to the preparation technology of high-temperature structural ceramics, and particularly provides an in-situ reaction for the preparation of hafnium aluminum nitrogen (Hf 3 AlN) ceramic material method. Background technique [0002] The ternary hafnium aluminum nitrogen (Hf-Al-N) ceramic system is a new type of high temperature and wear resistant structural ceramic material. They have excellent properties such as high hardness, wear resistance, oxidation resistance and high temperature resistance. They are widely used in aviation and aerospace. , nuclear industry and other high-tech fields have broad application prospects. However, current studies on the ternary single-phase HfAlN (Hf 3 Research on AlN) ceramics is very limited. Document 1 (J.Nucl.Mater. (Acta Nuclear Materials) 120 (1984) 133) used Hf powder, HfN powder, Al powder and AlN powder as raw materials, smelted at 1000 ° C or 1400 ° C, and synthesized for the first ti...

Claims

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Application Information

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IPC IPC(8): C04B35/58C04B35/622
Inventor 周延春李方志
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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