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Preparation method of high-density ultra-high-temperature Ta4HfC5 ceramic block material

A dense and ceramic block technology, which is applied in the field of preparation of high-density and ultra-high temperature Ta4HfC5 ceramic blocks, can solve various problems such as poor performance, high cost, and low block density, and achieve high density and reduce oxidation. , excellent physical properties

Inactive Publication Date: 2018-03-30
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The solid phase sintering method is sintered under normal pressure, the sintering method is simple, the formed block has low density, and various properties are poor; both the hot pressing sintering method and the hot isostatic pressing sintering method exist C atoms in the graphite mold to the ceramic material. Diffusion produces impurities and high cost problems

Method used

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  • Preparation method of high-density ultra-high-temperature Ta4HfC5 ceramic block material
  • Preparation method of high-density ultra-high-temperature Ta4HfC5 ceramic block material
  • Preparation method of high-density ultra-high-temperature Ta4HfC5 ceramic block material

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: Apply the method provided by the present invention to prepare a kind of high-density ultra-high temperature Ta 4 HfC 5 Ceramic blocks, the specific steps are as follows:

[0022] The first step, choose TaSi 2 As a flux, TaSi 2 The added amount is 6vol.% volume fraction, Ta 4 HfC 5 The volume of the solid solution powder is 94vol.%. According to the volume ratio, the two original powders are mixed.

[0023] Such as figure 1 Curve A shown is the use of X-ray diffractometer to analyze Ta 4 HfC 5 solid solution powder, showing only Ta 4 HfC 5 Crystal phase, indicating that the powder is Ta 4 HfC 5 solid solution.

[0024] In the second step, the mixed powder of the first step is subjected to high-energy ball milling, the ball milling speed is 300r / min, and high-purity Ar gas is used as the protective atmosphere, the ball milling time is 15 hours, and the powder obtained by ball milling is analyzed using a laser particle size analyzer. The D50 of t...

Embodiment 2

[0028] The first step, choose TaSi 2 As a flux, TaSi 2 The added amount is a volume fraction of 12vol%, Ta 4 HfC 5 The volume of the powder is 88vol.%. According to the volume ratio, the two original powders are mixed.

[0029]The second step is to carry out high-energy ball milling after the powder is mixed. The ball milling speed is 200r / min, and high-purity Ar gas is used as the protective atmosphere. The ball milling time is 20 hours. The powder obtained by ball milling is analyzed by a laser particle size analyzer to obtain a powder. The D50 was 1.49 μm, and 3.0 g of mixed powder was weighed.

[0030] The third step is to dry the mixed powder and put it into the SPS graphite mold with a diameter of 10mm. After vacuuming, apply DC pulse current heating to the graphite mold in a vacuum state. The heating rate is 100°C / min. From Start to pressurize at room temperature, slowly pressurize to the preset pressure of 30MPa, and keep the pressure until the sintering is complet...

Embodiment 3

[0033] The first step, choose TaSi 2 As a flux, TaSi 2 The added amount is a volume fraction of 12vol%, Ta 4 HfC 5 The volume of the powder is 88vol%. According to the volume ratio, the two original powders are mixed.

[0034] In the second step, the mixed powder is subjected to high-energy ball milling, the ball milling speed is 300r / min, and high-purity Ar gas is used as the protective atmosphere, and the ball milling time is 5 hours. The particle size analysis of the powder obtained by ball milling is obtained by using a laser particle size analyzer. The D50 of the powder was 1.49 μm, and 3.0 g of the mixed powder was weighed.

[0035] The third step is to dry the mixed powder and put it into the SPS graphite mold with a diameter of 10mm. After vacuuming, apply DC pulse current heating to the graphite mold in a vacuum state. The heating rate is 100°C / min. From Start to pressurize at room temperature, slowly pressurize to the preset pressure of 30MPa, and keep the pressu...

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Abstract

The invention discloses a preparation method for a high-density ultra-high-temperature Ta4HfC5 ceramic block material and belongs to the technical field of ultra-high-temperature ceramics. In the preparation method, a Ta4HfC5 solid solution powder and a sintering flux are mixed according to a volume ratio, and after high-energy ball milling, the high-density ultra-high-temperature Ta4HfC5 ceramicblock material is prepared by SPS. Compared with the prior art, the raw material used in the preparation method is the powder form of the solid solution Ta4HfC5 ceramic material instead of a mixed powder of TaC and HfC, thereby avoiding a complicated procedure of mixing the two powders, and avoiding influence on sintering caused by uneven particle size distribution and uneven mixing of the two powders. The high-density ultra-high-temperature Ta4HfC5 ceramic prepared by the preparation method has a high density, excellent physical properties such as hardness, elastic modulus and fracture toughness. After testing, the Vickers hardness is 1000 HV to 2100 HV, the elastic modulus is 300 GPa to 490 GPa, and the fracture toughness reaches 2.0 MPa*m<1 / 2> to 3.5 MPa*m<1 / 2>.

Description

technical field [0001] The invention relates to a high-density ultra-high temperature Ta 4 HfC 5 The invention discloses a method for preparing ceramic blocks, belonging to the technical field of ultra-high temperature ceramics. Background technique [0002] Hypersonic speed represents the development direction of the next generation of advanced aircraft. The high-speed movement of the aircraft will cause the nose cone and leading edge stagnation point on the surface to generate high temperatures of up to thousands of degrees Celsius, or even thousands of degrees Celsius. At the same time, it is necessary to maintain high temperature structural stability, and its The internal propulsion system scramjet engine can reach 3000°C at high temperature, and there will be oxidation and chemical erosion environment during service. In view of these harsh conditions, refractory metal materials, graphite materials, fiber-reinforced resin composite materials, C / C composite materials ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/622C04B35/626C04B35/64C04B35/66
CPCC04B35/5607C04B35/622C04B35/62615C04B35/64C04B2235/3891C04B2235/666C04B2235/96
Inventor 郭洪波肖晨兵
Owner BEIHANG UNIV
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