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High-purity superfine high-entropy ceramic powder and preparation method thereof

A ceramic powder, high-purity technology, applied in the field of high-entropy ceramic powder and its preparation, high-entropy ceramic powder, can solve the problems of difficult preparation of high-entropy ceramic materials, achieve the effect of improving sintering behavior, realizing performance, and being easy to participate in the reaction

Inactive Publication Date: 2020-02-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the difficulty of preparing high-entropy ceramic materials is an important factor restricting its application.

Method used

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  • High-purity superfine high-entropy ceramic powder and preparation method thereof
  • High-purity superfine high-entropy ceramic powder and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Raw material ratio (by mass percentage): HfO 2 : 16.00%, MoO 3 : 10.98%, Nb 2 o 5 : 10.15%, Ta 2 o 5 : 16.87%, TiO 2 : 6%, sucrose powder: 40.00%;

[0020] Preparation process: Put the above powders in a ball mill, add an appropriate amount of distilled water and mix them evenly, and then dry them to obtain a mixed powder with a particle size of 0.15-5 μm; then put the mixed powder into a graphite mold and place it in a discharge plasma Sintering in a sintering furnace; the sintering parameters are: the vacuum degree is lower than 5×10 -1 Pa, the average heating rate is 80°C / min, the sintering temperature is 1800°C, the pressure is 3 MPa, and the holding time is 15 min. After sintering, cool down to room temperature with the furnace to obtain high-entropy ceramic powder, denoted as HC1. The average particle size of the high-entropy ceramic powder is 100-250 nm, and the purity is 99.1%.

Embodiment 2

[0022] Raw material ratio (by mass percentage): HfO 2 : 14.59%, MoO 3 : 10.04%, Nb 2 o 5 : 9.23%, Ta 2 o 5 : 15.43%, TiO 2 : 5.44%, sucrose powder: 45.27wt%;

[0023] Preparation process: Put the above-mentioned powders in a ball mill, add an appropriate amount of distilled water and mix them evenly, and then dry them to obtain mixed powders with a particle size of 0.15-5 μm; then put the mixed powders into graphite molds, and place them in spark plasma sintering Sintering in the furnace; the sintering parameters are: the degree of vacuum is lower than 5×10 -1 Pa, the average heating rate is 80°C / min, the sintering temperature is 2000°C, the pressure is 3 MPa, and the holding time is 15 min. After sintering, cool down to room temperature with the furnace to obtain high-entropy ceramic powder, denoted as HC2. The average particle size of the high-entropy ceramic powder is 120-260 nm, and the purity is 99.3%.

Embodiment 3

[0025] Raw material ratio (by mass percentage): HfO 2 : 13.71%, MoO 3 : 9.35%, Nb 2 o 5 : 8.55%, Ta 2 o 5 : 14.29%, TiO 2 : 5.20%, sucrose powder: 48.9%;

[0026] Preparation process: Put the above-mentioned powders in a ball mill, add an appropriate amount of distilled water and mix them evenly, then dry them to obtain mixed powders with a particle size of 0.15-5 μm; then put the mixed powders into graphite molds and place them in discharge plasma Sintering in a sintering furnace; the sintering parameters are: the vacuum degree is lower than 5×10 -1 Pa, the average heating rate is 80°C / min, the sintering temperature is 2100°C, the pressure is 3 MPa, and the holding time is 15 min. After sintering, cool down to room temperature with the furnace to obtain high-entropy ceramic powder, denoted as HC3. The average particle size of the high-entropy ceramic powder is 140-300 nm, and the purity is 99.5%.

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Abstract

The invention discloses a preparation method of high-purity superfine high-entropy ceramic powder. The method includes: putting HfO2, MoO3, Nb2O5, Ta2O5, TiO2 and sucrose into a ball mill according tocertain ratio, adding distilled water, performing mixing, then conducting drying and sieving treatment to obtain mixed powder with a particle size of 0.15-5microm; then putting the mixed powder intoa graphite mold, and putting the graphite mold into a spark plasma sintering furnace for sintering; and at the end of sintering, performing furnace cooling to room temperature, thus obtaining the high-entropy ceramic powder. The high-entropy ceramic powder prepared by the method provided by the invention has high purity and small particle size, is beneficial to lowering the sintering temperature of the ceramic material, is easier for densification, and is particularly suitable for preparation of ceramic blocks which have stable properties when serving under an ultrahigh-temperature working condition. In addition, by adjusting the formula and technological parameters, regulation and control of the performance of the high-entropy ceramic powder material can be achieved.

Description

technical field [0001] The invention relates to a high-entropy ceramic powder, in particular to a high-purity ultra-fine high-entropy ceramic powder and a preparation method thereof, belonging to the technical field of ceramic nanomaterials. Background technique [0002] The reliability and stability of structural materials play a key role in the safe, stable and efficient operation of high-end equipment mechanical systems. With the rapid development of high technology, the working conditions of the new generation of nuclear reactors, jet engines, rocket nozzles, and supersonic vehicles are becoming more and more harsh, and the demand for ultra-high temperature materials is more urgent. Since the existing ultra-high temperature ceramics cannot meet the requirements under extreme working conditions, the research and development of ultra-high temperature ceramic materials has attracted much attention. [0003] In recent years, with the rapid development of high-entropy alloys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/56C01B32/907C01B32/90
CPCC01P2002/72C01P2004/62C01P2006/80C04B35/5622C04B35/62675C04B2235/5445C01B32/90C01B32/907
Inventor 杨军孙奇春刘维民朱圣宇程军
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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