Preparation method of high-purity metal hafnium

A high-purity, metal technology, applied in the field of rare metals, can solve the problems of uneven particle size, low purity of metal hafnium, complex process, etc., and achieve the effect of uniform size and high purity

Inactive Publication Date: 2019-08-16
南通晶朋新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the metal hafnium synthesized by the prior art has the problems of low purity, complex process and non-uniform particle size.

Method used

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  • Preparation method of high-purity metal hafnium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for preparing high-purity metal hafnium, including:

[0024] S1. Dissolve the hafnium tetrachloride solid in deionized water to obtain a hafnium oxychloride solution with a concentration of 0.01g / mL. At room temperature, slowly add the sodium hydroxide solution with a concentration of 0.01g / mL to the oxygen chloride In the hafnium solution, a mixed solution is obtained;

[0025] S2. Pour the mixed solution into a high-pressure hydrothermal reaction kettle, put the reaction kettle in an oven, the temperature of the oven is 120°C, and place it in the oven for 12 hours;

[0026] S3. Pour the suspension of the reaction kettle into the flask, wash the solid obtained by centrifugation with ethanol and deionized water alternately, centrifuge, and repeat three times. The final product is dried at 60℃ for 12h to obtain hafnium oxide, such as figure 1 As shown, the positions of the diffraction peaks of hafnium oxide are 24.64°, 28.30°, 31.76° and 50.46°, and the corresponding c...

Embodiment 2

[0029] A method for preparing high-purity metal hafnium, including:

[0030] S1. Dissolve the solid hafnium tetrachloride in deionized water to obtain a hafnium oxychloride solution with a concentration of 0.05g / mL. At room temperature, slowly add a sodium hydroxide solution with a concentration of 0.05g / mL to the oxygen chloride. In the hafnium solution, a mixed solution is obtained;

[0031] S2. Pour the mixed solution into a high-pressure hydrothermal reaction kettle, put the reaction kettle in an oven, the temperature of the oven is 100°C, and place it in the oven for 24 hours;

[0032] S3. Pour the suspension in the reaction kettle into the flask, wash the solid obtained by centrifugation alternately with ethanol and deionized water, centrifuge, and repeat three times. The final product obtained is dried at 60°C for 24 hours to obtain hafnium oxide, monoclinic crystal form, Hafnium oxide with a particle size of 120nm;

[0033] S4. Mixing excess Ca powder with a particle size of ...

Embodiment 3

[0035] A method for preparing high-purity metal hafnium, including:

[0036] S1. Dissolve the hafnium tetrachloride solid in deionized water to obtain a hafnium oxychloride solution with a concentration of 0.02g / mL. At room temperature, slowly add a sodium hydroxide solution with a concentration of 0.02g / mL to the oxygen chloride In the hafnium solution, a mixed solution is obtained;

[0037] S2. Pour the mixed solution into a high-pressure hydrothermal reaction kettle, and place the reaction kettle in an oven with a temperature of 110°C and place it in the oven for 16 hours;

[0038] S3. Pour the suspension of the reaction kettle into the flask, wash the solid obtained by centrifugation alternately with ethanol and deionized water, centrifuge, and repeat three times. The final product obtained is dried at 50°C for 16 hours to obtain hafnium oxide, monoclinic crystal, Hafnium oxide with a particle size of 80nm;

[0039] S4. Mixing excess Ca powder with a particle size of 1 μm and haf...

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Abstract

The invention discloses a preparation method of high-purity metal hafnium. The preparation method comprises the steps that tetrachloride hafnium solid is dissolved into deionized water, an oxygen hafnium chloride solution is obtained, a sodium hydroxide solution is slowly dropwise added into the oxygen hafnium chloride solution at the room temperature, and mixed liquid is obtained; the mixed liquid is poured into a high-pressure water thermal reaction kettle, and the reaction kettle is placed into a drying oven; suspension liquid of the reaction kettle is poured into a flask, solid obtained through centrifugation is alternately cleaned by ethyl alcohol and the deionized water, centrifugation is carried out repeatedly for three times, a product finally obtained is dried at 40-60 DEG C for 12-24 h, and hafnium oxide is obtained; and an excessive amount of Ca powder and the hafnium oxide are mixed, and are subjected to reduction in a sealed reactor, and the high-purity metal hafnium is obtained. According to the preparation method, the hafnium oxide prepared by a hydrothermal method is uniform in size, the metal hafnium obtained through reduction of the Ca powder is high in purity, and the metal hafnium is uniform in size.

Description

Technical field [0001] The invention relates to the technical field of rare metals, in particular to a method for preparing high-purity metal hafnium. Background technique [0002] Hafnium is a rare metal material. Because it is difficult to extract and the quantity is small, high-purity hafnium is mainly used as a control material for nuclear reactors. High-purity hafnium can be processed into different specifications of rods, plates, wires, and wires according to its excellent processing performance. Tube is also the object of research and development for new alloys. Because of its high melting point, hafnium is a trace additive for aviation, aerospace, and cemented carbide. With the development of large-scale modernization in the defense industry and mechanical special processing industry. High-purity hafnium is an important metal material indispensable for machining as a special alloy for aviation and aviation. Hafnium has been used as an alloy additive. Adding a small amou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/14C22B5/04
CPCC22B5/04C22B34/14
Inventor 成瑞清丁锦明
Owner 南通晶朋新材料科技有限公司
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