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Method for preparing MAX phase ceramic Ti3AlC2 powder by molten salt method low temperature sintering

A technology of low temperature sintering and molten salt method, applied in the field of ternary layered MAX phase ceramic powder preparation, can solve the problems of lower sintering temperature, high sintering temperature, no simple operation, etc. The effect of production costs

Active Publication Date: 2018-04-20
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

However, these methods have disadvantages such as complicated operation and sintering temperature higher than 1400 °C. So far, there is no simple operation at home and abroad, which can reduce the sintering temperature to 1000-1250 °C and can synthesize high-purity Ti. 3 AlC 2 Powder Research Report

Method used

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  • Method for preparing MAX phase ceramic Ti3AlC2 powder by molten salt method low temperature sintering
  • Method for preparing MAX phase ceramic Ti3AlC2 powder by molten salt method low temperature sintering
  • Method for preparing MAX phase ceramic Ti3AlC2 powder by molten salt method low temperature sintering

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Experimental program
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Effect test

Embodiment 1

[0044] With TiH 2 Powder (325 mesh, 99%), aluminum powder (1-2 μm), TiC powder (2-4 μm, 99%) are used as raw materials. Raw materials according to Ti 3 AlC 2 The stoichiometric ratio is proportioned, and an excess of 10at% aluminum powder is used; the raw materials are mixed and roller milled for 12 hours to obtain a uniformly mixed powder. Place the well-mixed powder in Al 2 o 3 Put the crucible into a vacuum tube furnace, and then pass in flowing Ar as a protective atmosphere, raise the temperature to 1000°C at a heating rate of 5°C / min, and then raise the temperature to 1250°C at a heating rate of 3°C / min. Keep it warm for 2 hours, then lower the temperature to 1000°C at a rate of 3°C / min, and then cool down to room temperature with the furnace. After the block is cooled, take it out and grind it. Prepared Ti 3 AlC 2 The XRD pattern of the powder is as follows figure 1 shown. Calculated by the XRD characteristic peak intensity of the sample, Ti in the sintered sam...

Embodiment 2

[0046] With TiH 2 Powder (325 mesh, 99%), aluminum powder (1-2 μm), TiC powder (2-4 μm, 99%) are used as raw materials. Raw materials according to Ti 3 AlC 2 The stoichiometric ratio is proportioned, and an excess of 10at% aluminum powder is used; KCl and raw materials are weighed and mixed according to a mass ratio of 2:1, and a uniformly mixed powder is obtained after roller milling for 12 hours. Place the well-mixed powder in Al 2 o 3 Then put the crucible into a vacuum tube furnace, then pass flowing Ar as a protective atmosphere, raise the temperature to 1000°C at a heating rate of 5°C / min, keep it for 5 hours, and then cool to room temperature with the furnace. After the block is cooled, take it out, grind it, and wash away the molten salt with deionized water until the titration of AgNO 3 No precipitation, placed in an environment of 80 ° C for 24 hours to dry Ti 3 AlC 2 Powder. Prepared Ti 3 AlC 2 The XRD pattern of the powder is as follows figure 2 shown. ...

Embodiment 3

[0048] With TiH 2 Powder (325 mesh, 99%), aluminum powder (1-2 μm), TiC powder (2-4 μm, 99%) are used as raw materials. Raw materials according to Ti 3 AlC 2 The stoichiometric ratio is proportioned, and an excess of 10at% aluminum powder is used; KCl and raw materials are weighed and mixed according to a mass ratio of 5:1, and a uniformly mixed powder is obtained after roller milling for 12 hours. Place the well-mixed powder in Al 2 o 3 Then put the crucible into a vacuum tube furnace, then pass flowing Ar as a protective atmosphere, raise the temperature to 1000°C at a heating rate of 5°C / min, keep it for 5 hours, and then cool to room temperature with the furnace. After the block is cooled, take it out, grind it, and wash away the molten salt with deionized water until the titration of AgNO 3 No precipitation, placed in an environment of 80 ° C for 24 hours to dry Ti 3 AlC 2 Powder. Prepared Ti 3 AlC 2 The XRD pattern of the powder is as follows image 3 shown. ...

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Abstract

The invention relates to a method for preparing MAX phase ceramic Ti3AlC2 powder by molten salt method low temperature sintering. The method is as follows: TiH2 powder, Al powder and TiC powder as rawmaterial powder are mixed with a molten salt to obtain a mixed raw material, the molten salt is KCl and / or NaCl, and the resulting mixed raw material is placed in a protective atmosphere, sintered at1000-1250 DEG C for a certain period of time, pulverized and washed to obtain the MAX phase ceramic Ti3AlC2 powder.

Description

technical field [0001] The invention relates to a low-temperature sintering method for preparing MAX phase ceramic Ti by molten salt method 3 AlC 2 The powder method belongs to the field of preparation of ternary layered MAX phase ceramic powder. Background technique [0002] Ternary layer compound M n+1 AX n (MAX phase ceramics) have a layered hexagonal crystal structure with a space group of D 4 6h -P6 3 / mmc. Wherein, n=1, 2, 3, M is a transition metal element, A is a group III and IV element, and X is a C or N element. Ti 3 AlC 2 is M n+1 AX n A typical representative of , the lattice parameters are a=b=0.30753nm, c=1.8578nm, and the theoretical density is 4.25g / cm 3 , which has both metal shaping, thermal conductivity, and electrical conductivity, and at the same time has high strength, high density, and excellent high temperature resistance and oxidation resistance of ceramics. [0003] Pietzka first discovered the ternary layered compound Ti in 1994 while...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/622
CPCC04B35/5618C04B35/622C04B2235/6562C04B2235/6565C04B2235/6567
Inventor 于云陈兵兵冯爱虎江峰于洋米乐宋力昕
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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