Process for preparing high-density zirconium diboride blocks by spark plasma sintering

A technology of discharge plasma and diboration, which is applied in the direction of chemical instruments and methods, boron/boride, metal boride, etc., can solve the problems of low relative strength, high cost, and difficult sintering, so as to shorten the sintering time, Low energy consumption and time consumption, high-efficiency sintering effect

Inactive Publication Date: 2006-09-27
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve hot pressing performance, it is often necessary to select a suitable sintering aid (such as CrB 2 , VB, ZrO 2 , metal, etc.), but the efficiency of this method is too low, the cost is high, and the amount of sintering aid is too large, which has a negative impact on the high-temperature performance of zirconium boride ceramics
[0005] The main problems faced by the application of zirconium diboride bulk materials are that it is difficult to produce dense sintered bodies, easy to oxidize in high temperature environments, and the relative strength is not high, which limits the application field of zirconium diboride bulk materials
[0007] To prepare zirconium diboride bulk materials, traditional pressureless sintering and hot-press sintering require high temperatures, and it is difficult to obtain dense sintered bodies, which affects the performance of materials and limits the quality of zirconium diboride bulk materials. scope of application

Method used

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  • Process for preparing high-density zirconium diboride blocks by spark plasma sintering
  • Process for preparing high-density zirconium diboride blocks by spark plasma sintering

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0022] 1), Coated ZrB 2 Preparation of composite powder:

[0023] 3 g ZrB 2 Add the powder into 200ml of water, ultrasonically disperse for 5 minutes, and stir evenly to obtain ZrB 2 A slurry of powder and water; drop 200ml of 0.05mol / L zirconium hypochlorite solution into the slurry at a constant speed for 120 minutes, and drop the precipitant ammonia water with pH=11 at the same time to adjust ZrB 2 The pH value of the slurry is always 9, and the stirrer is used to stir continuously. After the zirconium hypochlorite solution is added dropwise, the stirring is continued for 1 hour, and the pH value is kept at 9, and the precursor coated ZrB of the coating layer is obtained. 2 The composite powder of the powder; the composite powder was washed three times and once with deionized water and absolute ethanol respectively, then dried at 100°C and calcined at 600°C to obtain ZrO 2 Coated ZrB 2 Coated ZrB powder particles 2 Composite powder. Coated ZrB 2 The thickness of the ...

Embodiment 2

[0027] 1), Coated ZrB 2 Preparation of composite powder:

[0028] 3 g ZrB 2 Add the powder into 200ml of water, ultrasonically disperse for 5 minutes, and stir evenly to obtain ZrB 2 Slurry of powder and water; drop 300ml of mixed solution (150ml of 0.12mol / L aluminum nitrate and 150ml of 0.2mol / L yttrium nitrate) into the slurry at a constant speed in 180 minutes, and drop the precipitant of pH=11 at the same time Ammonia regulates ZrB 2 The pH value of the slurry is always 9. Stir continuously with a stirrer. After the mixed solution is added dropwise, continue to stir for 1 hour, and keep the pH value at 9 to obtain the precursor of the coating layer coated ZrB 2 The composite powder of the powder; the composite powder was washed three times and once with deionized water and absolute ethanol respectively, then dried at 80°C and calcined at 500°C to obtain Al 2 o 3 and Y 2 o 3 co-coated ZrB 2 Coated ZrB powder particles 2 Composite powder. Coated ZrB 2 The thickne...

Embodiment 3

[0032] Get 2.0g coated zirconium diboride composite powder (the coating layer is 10% ZrO 2) into a graphite mold with an inner diameter of 10 mm, and the surrounding and upper and lower surfaces are lined with graphite paper, and the powder is compacted with an axial pressure of 30 MPa, and the pressure is maintained for 10 minutes. Put the pre-compressed mold into the spark plasma sintering equipment, apply an axial pressure of 50MPa, and under the protection of an inert atmosphere, raise the temperature to 1600°C at a heating rate of 50°C / min for 5 minutes, then cool with the furnace. The density of the sintered zirconium diboride bulk material is 97%.

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Abstract

The invention refers to a method for preparation of zirconium diboride block material. The method is about a discharging plasma sinter high-integrity zirconium diboride block material, the character is lies in it includes steps as follows: directly posting coated format ZrB2 in graphite mould, and then putting mould in discharging plasma sintering furnace, applying axial pressure of 10- 50MPa, adopting vacuum condition or interia atmosphere which vacuum degree is less than 10Pa, sintering in sintered temperature of 1600- 2200Deg C, heating-up with rate of 50-500Deg C/min, heat preserving for 1-30min, cooling under 1300Deg C with cooling rate of 10-100Deg C/min, finally furnace cooling to room temperature, getting high degree of compactness zirconium diboride block material. The produced zirconium diboride block materials have high degree of compactness, hardness, high-temperature strength and oxidation resistance capability.

Description

technical field [0001] The invention relates to a preparation method of a zirconium diboride bulk material. Background technique [0002] Zirconium diboride bulk materials are widely used in high-temperature structural ceramic materials, composite materials, refractory materials, electrode materials and nuclear control materials because of their high melting point and high hardness, good electrical and thermal conductivity, and good neutron control capabilities. It has been paid attention to and widely used in the field. With the deeper research on it, many new uses and prospects will be excavated, and it will be more widely used day by day. [0003] Zirconium diboride is a metalloid structure compound of hexagonal C32 structure, which has the characteristics of high melting point, high hardness, high stability, good electrical conductivity, thermal conductivity and high corrosion resistance. [0004] Zirconium diboride (ZrB 2 ) There are many methods for forming and sint...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04C01G25/00
Inventor 张联盟宋建荣李俊国宋杰光沈强
Owner WUHAN UNIV OF TECH
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