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Method for preparing ruthenium powder for target materials from ruthenium trichloride

A technology of ruthenium trichloride and ruthenium powder, which is applied in the field of preparation of precious metal powder, can solve the problems of complex operation, reduced chlorine content of ruthenium powder, and cannot be removed, and achieves the effects of simple process, low impurity content, and improved production efficiency

Active Publication Date: 2015-01-28
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is complicated to operate, and can only reduce the chlorine content of the ruthenium powder, but cannot remove other impurities contained in the ammonium hexachlororuthenate precipitation process, and the final ruthenium powder has a high impurity content and cannot be used for target production

Method used

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  • Method for preparing ruthenium powder for target materials from ruthenium trichloride
  • Method for preparing ruthenium powder for target materials from ruthenium trichloride
  • Method for preparing ruthenium powder for target materials from ruthenium trichloride

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Embodiment 1

[0018] Embodiment 1, see attached figure 1 , dissolving solid ruthenium trichloride with 6-12mol / L hydrochloric acid to obtain a ruthenium chloride solution, passing the resulting solution through a cation exchange resin to remove cationic impurities to obtain a pure ruthenium solution, adding sodium hydroxide to the obtained pure ruthenium solution to generate hydrogen Precipitate ruthenium oxide, add deionized water to slurry, adjust the pH value to 9, and obtain the precursor of ruthenium powder, place the obtained precursor in a high-pressure reactor, heat to 180 ° C, and feed hydrogen to maintain a partial pressure of 2 MPa for 6 hours. Solid-liquid separation, fully washed with deionized water, and vacuum drying at 120°C to obtain pure ruthenium powder.

Embodiment 2

[0019] Embodiment 2, see attached figure 1 , dissolving solid ruthenium trichloride with 6-12mol / L hydrochloric acid to obtain a ruthenium chloride solution, passing the resulting solution through a cation exchange resin to remove cationic impurities to obtain a pure ruthenium solution, adding sodium hydroxide to the obtained pure ruthenium solution to generate hydrogen Precipitate ruthenium oxide, add deionized water to slurry, adjust the pH value to 10, and obtain the precursor of ruthenium powder, place the obtained precursor in a high-pressure reactor, heat to 200°C, and pass in hydrogen to maintain a partial pressure of 1.5 MPa for 6 hours. , solid-liquid separation, fully washed with deionized water, and vacuum-dried at a temperature of 120 ° C to obtain pure ruthenium powder.

Embodiment 3

[0020] Embodiment 3, see attached figure 1 , dissolving solid ruthenium trichloride with 6-12mol / L hydrochloric acid to obtain a ruthenium chloride solution, passing the resulting solution through a cation exchange resin to remove cationic impurities to obtain a pure ruthenium solution, adding sodium hydroxide to the obtained pure ruthenium solution to generate hydrogen Precipitate ruthenium oxide, add deionized water to slurry, adjust the pH value to 10, and obtain the precursor of ruthenium powder, place the obtained precursor in a high-pressure reactor, heat to 220°C, and pass in hydrogen to maintain a partial pressure of 1.2MPa for 8 hours , solid-liquid separation, fully washed with deionized water, and vacuum-dried at a temperature of 120 ° C to obtain pure ruthenium powder.

[0021] The ruthenium powder prepared by the present invention was analyzed by GDMS, and the results are shown in Table 1 below.

[0022] Table 1 GDMS impurity analysis results of ruthenium powder ...

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Abstract

The invention discloses a method for preparing ruthenium powder for target materials from ruthenium trichloride. The method comprises the following steps of (1) dissolving: solid ruthenium trichloride is dissolved by hydrochloric acid to obtain a chlororuthenite solution; (2) ion exchange purification: the solution obtained in the step (1) is subjected to positive ion impurity removal through ion exchange resin to obtain a pure ruthenium solution; (3) precursor preparation: alkali is added into the pure ruthenium solution to generate ruthenium oxide hydrate precipitates, deionized water is continuously added for pulpifying, the pH value is regulated, and ruthenium powder precursors are obtained; and (4) pressurization hydrogen reduction: the precursors obtained in the step (3) are placed into a high-pressure reaction kettle and are heated, hydrogen gas is introduced, certain hydrogen partial pressure is maintained for carrying out reduction, solid-liquid separation is carried out, the deionized water is used for sufficiently washing the materials, and pure ruthenium powder is obtained after the vacuum drying. The method provided by the invention has the advantages that the process is simple, the impurity content of the ruthenium powder is low (lower than 100ppm), the direct yield is greater than 99 percent, the microcosmic micro appearance of the obtained ruthenium powder is in a spherical shape, the granularity is 2 to 5 mum, and the method conforms to the production requirements of ruthenium target materials.

Description

technical field [0001] The invention relates to the preparation of noble metal powder, in particular to a method for preparing ruthenium powder for target materials by using ruthenium trichloride. Background technique [0002] Ruthenium powder for computer hard disk memory material targets has special index requirements, and the total impurities excluding gas elements are less than 100ppm. At present, the preparation method of domestic ruthenium powder generally adopts secondary oxidative distillation, concentrated crystallization of the absorption solution to obtain RuCl3 calcined hydrogen reduction to prepare ruthenium powder, or oxidizes the ruthenium absorption solution and then adds ammonium chloride precipitation, calcined, and hydrogen reduction to prepare ruthenium powder. The ruthenium powder obtained by the above method has coarse and uneven particles, high impurity content, and cannot be used for the production of ruthenium targets. [0003] Chinese patent ZL2005...

Claims

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Application Information

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IPC IPC(8): B22F9/26
Inventor 董海刚赵家春李博捷杨海琼吴跃东保思敏王亚雄童伟锋吴晓峰
Owner KUNMING INST OF PRECIOUS METALS
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