Nano rodlike zirconium boride powder and preparation method thereof

Abstract

The invention relates to nano rodlike zirconium boride powder and a preparation method thereof. According to the technical scheme, the preparation method comprises the step of uniformly mixing, by weight, 27-39% of zirconium oxide powder, 8-16% of boron carbide powder, 4-8% of non-formalized carbon powder, 12-26% of sodium chloride powder and 24-36% of potassium chloride powder, so that a mixture is obtained; putting a crucible containing the mixture into a saggar, then placing the saggar in a microwave oven, preserving the temperature for 20-40 minutes under the conditions that the vacuum degree is 10-50 Pa, argon atmosphere is provided, and the temperature ranges from 1000 DEG C to 1200 DEG C, conducting natural cooling, then conducting cleaning with deionized water, and preserving the temperature for 6-12 hours at the temperature of 65-80 DEG C in a vacuum drying box, so that the nano rodlike zirconium boride powder is obtained. The preparation method has the advantages of being low in cost, simple in process, low in reaction temperature, high in reaction velocity, suitable for industrialized production and environmentally friendly, and the obtained nano rodlike zirconium boride powder is high in purity, of a uniform rodlike structure, controllable in dimension, large in specific surface area and good in sintering property.

Description

technical field

[0001] The invention belongs to the technical field of zirconium boride powder. Specifically relates to a nano-rod zirconium boride powder and a preparation method thereof. Background technique

[0002] As a representative of new ultra-high temperature ceramics, zirconium boride ceramics have low density, high melting point, high hardness, high specific strength, high specific stiffness, good thermal conductivity, excellent electrical conductivity, excellent ablation resistance and oxidation resistance It is considered to be one of the most promising structural / functional integrated materials, and has been widely used in aerospace, military manufacturing, metallurgy, minerals, and mechanical processing. The current main method for preparing zirconium boride ceramics is to sinter zirconium boride powder under high temperature and high pressure conditions. Therefore, the preparation of zirconium boride powder with high purity and good sintering performance is...

Examples

Embodiment 1

[0037] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0038] (1) 36-39wt% zirconia powder, 14-16wt% boron carbide powder, 4-8wt% amorphous carbon powder, 12-16wt% sodium chloride powder and 24-30wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0039] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0040] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1000-1150°C at a heating rate of 10-20°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Keep warm for 20-25 minutes, and cool naturally to obtain rough zirconium boride powder.

[0041] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain nanoro...

Embodiment 2

[0044] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0045](1) 32-37wt% zirconia powder, 11-15wt% boron carbide powder, 6-7wt% amorphous carbon powder, 14-18wt% sodium chloride powder and 27-33wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0046] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0047] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1000-1200°C at a heating rate of 10-30°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Insulate for 20-30 minutes, and cool naturally to obtain rough-treated zirconium boride powder.

[0048] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain ...

Embodiment 3

[0051] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0052] (1) 27-31wt% zirconia powder, 9-12wt% boron carbide powder, 5-6wt% amorphous carbon powder, 17-20wt% sodium chloride powder and 31-36wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0053] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0054] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1150-1200°C at a heating rate of 20-40°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Keep warm for 25-40 minutes, and cool naturally to get rough zirconium boride powder.

[0055] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain nanorod zi...

technical field

[0001] The invention belongs to the technical field of zirconium boride powder. Specifically relates to a nano-rod zirconium boride powder and a preparation method thereof. Background technique

[0002] As a representative of new ultra-high temperature ceramics, zirconium boride ceramics have low density, high melting point, high hardness, high specific strength, high specific stiffness, good thermal conductivity, excellent electrical conductivity, excellent ablation resistance and oxidation resistance It is considered to be one of the most promising structural / functional integrated materials, and has been widely used in aerospace, military manufacturing, metallurgy, minerals, and mechanical processing. The current main method for preparing zirconium boride ceramics is to sinter zirconium boride powder under high temperature and high pressure conditions. Therefore, the preparation of zirconium boride powder with high purity and good sintering performance is...

Examples

Embodiment 1

[0037] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0038] (1) 36-39wt% zirconia powder, 14-16wt% boron carbide powder, 4-8wt% amorphous carbon powder, 12-16wt% sodium chloride powder and 24-30wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0039] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0040] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1000-1150°C at a heating rate of 10-20°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Keep warm for 20-25 minutes, and cool naturally to obtain rough zirconium boride powder.

[0041] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain nanoro...

Embodiment 2

[0044] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0045](1) 32-37wt% zirconia powder, 11-15wt% boron carbide powder, 6-7wt% amorphous carbon powder, 14-18wt% sodium chloride powder and 27-33wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0046] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0047] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1000-1200°C at a heating rate of 10-30°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Insulate for 20-30 minutes, and cool naturally to obtain rough-treated zirconium boride powder.

[0048] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain ...

Embodiment 3

[0051] A nanorod-shaped zirconium boride powder and a preparation method thereof. Described preparation method is:

[0052] (1) 27-31wt% zirconia powder, 9-12wt% boron carbide powder, 5-6wt% amorphous carbon powder, 17-20wt% sodium chloride powder and 31-36wt% The potassium chloride powder is mixed uniformly to obtain a mixture.

[0053] (2) Put the mixture into a crucible, put the crucible into a sagger, and then fill the gap between the sagger and the crucible with silicon carbide powder.

[0054] (3) Place the sagger after filling the gap in a microwave heating furnace, and raise the temperature to 1150-1200°C at a heating rate of 20-40°C / min under a vacuum degree of 10-50Pa and a flowing argon atmosphere, Keep warm for 25-40 minutes, and cool naturally to get rough zirconium boride powder.

[0055] (4) Wash the coarsely treated zirconium boride powder with deionized water for 3 to 5 times, and keep it in a vacuum oven at 65 to 80°C for 6 to 12 hours to obtain nanorod zi...

Images