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A kind of low-temperature preparation method of zirconium diboride powder

The technology of zirconium diboride and powder is applied in the field of low-temperature preparation of zirconium diboride powder, which can solve the problems of low product purity, high synthesis temperature, easy agglomeration yield of particles, etc., and achieves simple synthesis process and raw materials. The effect of low cost and lower production cost

Active Publication Date: 2021-04-27
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to solve the existing problems of high synthesis temperature, high energy consumption, long production cycle, low efficiency, and the need for vacuum or inert atmosphere protection, low product purity, easy agglomeration of particles or low yield, etc. , providing a low-temperature synthesis method of zirconium diboride powder

Method used

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  • A kind of low-temperature preparation method of zirconium diboride powder
  • A kind of low-temperature preparation method of zirconium diboride powder
  • A kind of low-temperature preparation method of zirconium diboride powder

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preparation example Construction

[0022] A low-temperature preparation method of zirconium diboride powder, comprising the following steps:

[0023] (1) Weigh the zirconium-containing compound and the boron-containing compound in a molar ratio of 1:1-1:10, and mix them to obtain a Zr-B mixture;

[0024] (2) Weigh the Zr-B mixture and the chloride molten salt respectively according to the weight ratio of 1:1-1:8, and mix them to obtain the zirconium diboride precursor;

[0025] (3) The zirconium diboride precursor is heated, kept warm, cooled, and the resulting product is soaked in water;

[0026] (4) Washing, suction filtering, acid leaching, water washing and drying the obtained product to obtain black zirconium diboride powder.

Embodiment 1

[0028] (1) Weigh zirconium hydroxide and sodium borohydride at a molar ratio of 1:5, and then use an agate mortar to fully mix the two to obtain a mixture of zirconium hydroxide and sodium borohydride (Zr-B mixture for short) .

[0029] (2) Weigh the Zr-B mixture and potassium chloride molten salt according to the weight ratio of 1:4, and put them into an agate mortar and mix them evenly to obtain the zirconium diboride precursor.

[0030] (3) Put an appropriate amount of zirconium diboride precursor into an alumina crucible with a lid, and heat it to 800°C at a heating rate of 5°C / min in a high-temperature resistance furnace and hold it for 2h. Then, cool down to room temperature naturally, take out the crucible and soak it in 80°C distilled water for 2h.

[0031] (4) Repeated washing with hot distilled water at 80°C, suction filtration 4 times, and acid leaching with diluted hydrochloric acid (0.5mol / L) solution for 0.5h to remove residual salt and by-products. After washi...

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Abstract

The invention discloses a low-temperature preparation method of zirconium diboride powder. The method comprises the following steps: (1) respectively weighing a zirconium-containing compound and a boron-containing compound according to a molar ratio of 1:1-1:10, and mixing them to obtain Zr-B mixture; (2) weigh Zr-B mixture and chloride molten salt respectively according to the weight ratio of 1:1-1:8, mix to obtain zirconium diboride precursor; (3) zirconium diboride The precursor is heated, kept warm, cooled, and the obtained product is soaked in water; (4) the obtained product is washed, suction filtered, acid leached, washed with water, and dried to obtain black zirconium diboride powder. The method of the invention can greatly reduce the temperature for synthesizing zirconium diboride; it can be synthesized in air, the cost of raw materials is low, the molten salt can be recycled, the production efficiency is high, the product has high purity and good particle shape, and the synthesis process flow is simple. The product has good repeatability and is easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a low-temperature preparation method of zirconium diboride powder. Background technique [0002] At present, the materials that can meet the requirements of extreme high temperature environments are mainly concentrated in ultra-high temperature ceramic materials such as high melting point borides and carbides, among which zirconium diboride is a metal boride with a hexagonal structure. In its crystal, Zr atoms Zr-B and B-atom faces alternately appear to form a two-dimensional network structure. This graphite-like structure determines that zirconium diboride has good electrical and thermal conductivity; and Zr-B bonds and B-B bonds have strong covalent Bonding and large bond energy make zirconium diboride have an ultra-high melting point (3245°C), and its sintered ceramic products have excellent mechanical properties, good chemical stability, and high temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/04
CPCC01B35/04C01P2002/72C01P2004/03
Inventor 马峻峰曹善桥陈琪王讯陈玉林
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)