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In-situ self-toughening ZrB2-based composite ceramic material and preparation method thereof

A self-toughening technology for composite ceramics, applied in chemical instruments and methods, inorganic chemistry, zirconium compounds, etc., can solve the problems of low material toughness and application limitations, and achieve the effect of low price and low purity requirements

Inactive Publication Date: 2013-03-20
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, since MoSi 2 The toughness is low, and the toughness of the obtained material is not high (generally at 2.5MPa m 1 / 2 left and right), so it is limited in application

Method used

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  • In-situ self-toughening ZrB2-based composite ceramic material and preparation method thereof
  • In-situ self-toughening ZrB2-based composite ceramic material and preparation method thereof
  • In-situ self-toughening ZrB2-based composite ceramic material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Zirconium powder (≤28μm, 98%), boron powder (≤1μm, 99%), silicon powder (≤50μm, 99%) and molybdenum powder (≤75μm, 99%) are used as raw materials. Design ZrB 2 -MoSi 2 Medium MoSi 2 The volume percentage is 20, that is, the reaction equation Zr+2xSi+xMo+2B=ZrB 2 +xMoSi 2 In x=0.190013 batching, take acetone as the slurry that the solid content of solvent preparation is 10wt%, with the speed of 550 rev / mins, use ZrO 2 The balls and planets were milled for 8 hours, and the resulting slurry was dried by rotary evaporation to obtain a uniformly mixed powder. Put the uniformly mixed powder in a graphite mold coated with BN on the inner wall surface, and carry out reaction sintering in a vacuum. The heating rate during sintering is 10°C / min, and a pressure of 20-30MPa is applied after the temperature rises to 1600°C. 0.5hr. The material density reaches 99.2%. The microstructure of the material is as figure 1 shown. The fracture toughness of the material is 4.9MPa m ...

Embodiment 2

[0025] Zirconium powder (≤28μm, 98%), boron carbide powder (≤2μm, 99%), silicon powder (≤50μm, 99%) and molybdenum powder (≤75μm, 99%) are used as raw materials. Design ZrB 2 -MoSi 2 -MoSi in SiC 2 The volume percentage is 20, that is, the reaction equation Zr+(1+2x)Si+xMo+B 4 C=2ZrB 2 +xMoSi 2 x=0.508135 in +SiC, and the volume percentage of SiC is also 20 at this moment, is the slurry that the solid content is 40wt% of the solvent preparation with acetone, prepares ceramics according to the method for embodiment 1, and sintering temperature is 1900 ℃, material The density reaches 98.9%. The microstructure of the material is as figure 2 shown. The fracture toughness of the material is 4.4MPa m 1 / 2 .

Embodiment 3

[0027] Zirconium powder (≤28μm, 98%), boron powder (≤1m, 99%), silicon powder (≤50μm, 99%) and molybdenum powder (≤75μm, 99%) are used as raw materials. Design ZrB 2 -MoSi 2 Medium MoSi 2 The volume percentage is 20, that is, the reaction equation Zr+2xSi+xMo+2B=ZrB 2 +xMoSi 2 Where x=0.190013, a slurry with a solid content of 30wt% was prepared with acetone as a solvent, and the ball milling method was roller ball milling. Ceramics were prepared according to the method of Example 1, the sintering temperature was 1650° C., and the material density was greater than 98%. The microstructure of the material is as image 3 shown.

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Abstract

The invention relates to an in-situ self-toughening ZrB2-based composite ceramic material and a preparation method thereof. The method comprises the following step of: subjecting zirconium powder with the purity of not lower than 98 percent, boron powder (or boron carbide powder), silicon powder and molybdenum powder to reaction, hot pressing and sintering at the temperature of between 1,600 DEG C and 1,900 DEG C for 0.5-2 hours according to the reaction equation of Zr+2xSi+xMo+2B=ZrB2+xMoSi2 for generating ZrB2-MoSi2, wherein x is more than or equal to 0.08 and less than or equal to 1, and the reaction equation of 2Zr+(1+2x)Si+xMo+B4C=2ZeB2+xMoSi2+SiC for generating ZrB2-MoSi2-SiC, wherein x is more than or equal to 0.2 and less than or equal to 2. By adopting the method, a material with the relative density of greater than 98 percent can be prepared at low temperature. ZrB2 crystal grains generated in the microscopic structure of the material by an in-situ reaction grow in a stick form, so that the toughness of the material is remarkably enhanced.

Description

technical field [0001] The present invention relates to in-situ self-toughening ZrB 2 The invention relates to a matrix composite phase ceramic material and a preparation method thereof, which belong to the field of non-oxide-based ceramic materials. Background technique [0002] Due to ZrB 2 With extremely high melting point and strong covalent bond, low self-diffusion coefficient, it is difficult to obtain dense materials. It is usually prepared by hot pressing and sintering at a temperature range of 1900-2200°C and a pressure higher than 20MPa or even 50MPa. ZrB by Bellosi et al. 2 / HfB 2 The sintering behavior of MoSi was studied, and the study showed that MoSi 2 The introduction of can reduce the sintering temperature most effectively and even realize pressureless sintering, and the prepared ZrB 2 -MoSi 2 The material can still maintain excellent mechanical properties at 1500°C (D.Sciti, S.Guicciardi, and A.Bellosi, "Properties of a Pressureless-SinteredZrB 2 -M...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00C04B35/622C04B35/582
Inventor 张国军吴雯雯阚艳梅王佩玲
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI