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a zrb 2 -sic-vsi 2 Ultra-high temperature ceramic composite material and its preparation method

A technology of ceramic composite materials and ultra-high temperature ceramics, which is applied in the direction of reducing greenhouse gases, nuclear power generation, climate sustainability, etc. The effect of short preparation time, inhibition of grain growth, and easy operation

Active Publication Date: 2022-05-31
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

[0004] The object of the present invention is to provide a kind of ZrB 2 -SiC-VSi 2 The ultra-high temperature ceramic composite material and its preparation method intend to solve the following problems: 1) the existing ZrB 2 -SiC-based ultra-high temperature ceramics have high sintering temperature and long sintering time, which will cause abnormal grain growth and reduce mechanical properties; 2) ZrB 2 - SiC-based ultra-high temperature ceramics are oxidized at high temperature to form a porous SiC-poor layer, resulting in a decline in its high-temperature mechanical and oxidation resistance properties

Method used

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  • a zrb <sub>2</sub> -sic-vsi <sub>2</sub> Ultra-high temperature ceramic composite material and its preparation method
  • a zrb <sub>2</sub> -sic-vsi <sub>2</sub> Ultra-high temperature ceramic composite material and its preparation method
  • a zrb <sub>2</sub> -sic-vsi <sub>2</sub> Ultra-high temperature ceramic composite material and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0041] ZrB with a particle size of 0.5 μm 2 Powder 15.94g, SiC powder with particle size 0.5 2.41g and VSi with particle size 1μm 2 Powder 1.65g (the volume fraction ratio of the three ceramic powders is ZrB 2 : SiC: VSi 2 =70:20:10) Put it into a nylon ball mill jar and mill it for 12h. The mixed ceramic powder was obtained by rotating and drying in a rotary evaporator (evaporating pressure 5kPa) at 60°C at a speed of 70rpm, and then passing through an 80-mesh sieve to obtain a mixed ceramic powder, which was then put into a graphite mold with a diameter of 25mm and the inner wall was coated with BN and cold-pressed at 5kN. 5min. Then, the graphite mold containing the mixed ceramic powder was hot-pressed and sintered in protective Ar with a flow rate of 3 L / min, heated to 1600 °C at a heating rate of 8 °C / min, and the pressure was gradually increased to 30 MPa, and the temperature was kept for 0.5 h. After the insulation, the temperature was lowered to 1200°C at 10°C / min,...

Embodiment 2

[0043] ZrB with a particle size of 2 μm 2 Powder 15.76g, SiC powder with particle size of 2μm 1.79g and VSi with particle size of 3μm 2 Powder 2.45g (the volume fraction ratio of the three ceramic powders is ZrB 2 : SiC: VSi 2 =70:15:15) Put it into a nylon ball mill jar and mill it for 24h. At 55°C at 75 rpm, rotate and dry in a rotary evaporator (evaporation pressure 3 kPa) and pass through a 100-mesh sieve to obtain a mixed ceramic powder, which is then put into a graphite mold with a diameter of 25 mm and the inner wall is coated with BN and cold-pressed at 5 kN. Formed for 8 minutes. Then, the graphite mold containing the mixed ceramic powder was hot-pressed and sintered in a vacuum (vacuum degree 10 -2 Pa), heated to 1550 °C at a heating rate of 8 °C / min, while the pressure was gradually increased to 30 MPa, and kept for 1 h. After the insulation, the temperature was lowered to 1000°C at 12°C / min, and air-cooled to room temperature to obtain ZrB 2 -SiC-VSi 2 Ultra...

Embodiment 3

[0045] ZrB with a particle size of 1 μm 2 Powder 15.03g, SiC powder with particle size of 1μm 2.45g and VSi with particle size of 2μm 2 Powder 2.52g (the volume fraction ratio of the three ceramic powders is ZrB 2 : SiC: VSi 2 =65:20:15) Put it into a nylon ball mill jar and mill it for 16h. The mixed ceramic powder was obtained by rotating and drying in a rotary evaporator (evaporating pressure 8kPa) at 50rpm at 70°C, and then passing through a 120-mesh sieve to obtain a mixed ceramic powder, which was then put into a graphite mold with a diameter of 25mm and coated with BN on the inner wall and cold pressed at 10kN. Formed for 5 minutes. Then, the graphite mold containing the mixed ceramic powder was heated at a flow rate of 5 L / min in a protective N 2 Medium hot pressing sintering, heating to 1650 °C at a heating rate of 15 °C / min, while the pressure was gradually increased to 35 MPa, and the temperature was kept for 0.5 h. After the insulation, the temperature was low...

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Abstract

The invention relates to the field of ultra-high temperature ceramic matrix composite materials, specifically a ZrB 2 ‑SiC‑VSi 2 Ultra-high temperature ceramic composite material and its preparation method. The material is prepared by hot pressing and sintering by powder metallurgy method, in which the dual reinforcement phases SiC and VSi 2 The particles are uniformly dispersed in ZrB 2 In the matrix. The specific operation steps are as follows: 1) ZrB 2 , SiC and VSi 2 The powder is put into a nylon tank, and the powder slurry is obtained by wet ball milling with absolute ethanol as a medium; 2) the powder slurry is rotated and dried and sieved to obtain ZrB 2 ‑SiC‑VSi 2 Mix the powder, and then put it into a graphite mold for cold pressing; 3) Put the molded green body together with the mold into a hot-press furnace, and heat-press and sinter it in a vacuum or inert gas atmosphere to obtain ZrB 2 ‑SiC‑VSi 2 Ultra-high temperature ceramic composite materials. The ZrB 2 ‑SiC‑VSi 2 Composite materials not only have low sintering preparation temperature, but also have excellent high temperature oxidation resistance, and also have the advantages of simple preparation process and short preparation cycle.

Description

technical field [0001] The invention relates to the field of ultra-high temperature ceramic matrix composite materials, in particular to a ZrB 2 -SiC-VSi 2 Ultra-high temperature ceramic composite material and preparation method thereof. Background technique [0002] Ultra-high temperature ceramics refers to a class of non-oxide ceramic materials with a melting point of over 3000 °C, mainly including borides, carbides and nitrides of early transition metals, such as: ZrB 2 , HfB 2 , ZrC, HfC, HfN, etc., which have excellent mechanical and chemical stability, and are ideal candidate material systems for ultra-high temperature thermal structures and thermal protection systems. Among them, ZrB 2 -SiC composite material is one of the most promising ultra-high temperature thermal protection materials due to its high thermal conductivity, moderate thermal expansion coefficient and good oxidation and ablation resistance, so it has received extensive attention. [0003] However...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/622C04B35/64
CPCC04B35/58078C04B35/622C04B35/64C04B2235/3826C04B2235/3891C04B2235/6562C04B2235/6565C04B2235/6567Y02E30/30
Inventor 钱余海张鑫涛杨阳徐敬军左君李美栓
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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