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Method for preparing spherical ruthenium powder through polyol reduction method

A technology of polyol and reduction method is applied in the field of preparing spherical ruthenium powder by polyol reduction method, and achieves the effects of small particle size, high purity and good material dispersibility

Active Publication Date: 2020-11-17
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention is aimed at the problem of the preparation of high-purity ruthenium powder in the prior art, and provides a kind of method that polyalcohol reduction method prepares spherical ruthenium powder, and the present invention adopts polyhydric alcohol as reduction The ruthenium in the ruthenium precursor solution is reduced by the agent, and the high-purity ultrafine spherical ruthenium powder with a particle size of 150-250nm is prepared by controlling the amount of the reducing agent, the pH value of the system, the reaction temperature and the time

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  • Method for preparing spherical ruthenium powder through polyol reduction method
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  • Method for preparing spherical ruthenium powder through polyol reduction method

Examples

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Effect test

Embodiment 1

[0023] Example 1: A method of preparing spherium tantalum powder by a polyol reduction method, the specific steps are as follows:

[0024] (1) Solument of the zeal precursor (trichloride) in deionized water, using a base solution (tetramethylcarbonate solution) regulating system pH of 7 to obtain a ruthenium precursor solution; wherein the ruthenium precursor solution is driven. The molar concentration of the body (trichloride) is 0.1 mol / L;

[0025] (2) The polyol (ethylene glycol) is dissolved in anhydrous ethanol in anhydrous ethanol; wherein the volume fraction of ethylene glycol in the reduction solution is 60%;

[0026] (3) At the temperature of 180 ° C, the stirring rate is 200 rpm, the reduction solution is added to the zearation reaction for 2 h, solid-liquid separation, sequentially use acetone, deionized water, and anhydrous ethanol to wash the solid, placed in temperature Ultra-fine spherium citium powder is obtained in vacuo and ground at 40 ° C; in which the molar ...

Embodiment 2

[0028] Example 2: A method of preparing a sputum powder by a polyol reduction method, the specific steps are as follows:

[0029] (1) Solument of the osmium precursor (trichloride) in deionized water, using a base pH of 6 to obtain a ruthenium precursor solution using an alkali solution (tetramethylcarbonate solution) to obtain a ruthenium precursor solution; wherein the ruthenium precursor solution is driven forward. The molar concentration of the body (trichloride) is 0.05 mol / L;

[0030] (2) The polyol (ethylene glycol) is dissolved in anhydrous ethanol in anhydrous ethanol; wherein the volume fraction of ethylene glycol in the reduction solution is 50%;

[0031] (3) At the temperature of 150 ° C, the stirring rate is 400 rpm, the reduction solution is added to the zearation reaction for 4 h, solid-liquid separation, and sequentially use acetone, deionized water, and anhydrous ethanol to wash the solid, placed in temperature. Ultrafine spherium powder was dried under 40 ° C a...

Embodiment 3

[0033] Example 3: Method for preparing spherium ruthenium powder by a polyol reduction method, the specific steps are as follows:

[0034] ((1) Solument of the osmium precursor (trichloride) in deionized water, using an alkali solution (tetramethylcarbonate solution) regulating the system pH 8 to obtain a ruthenium precursor solution; wherein the ruthenium precursor solution is ruthenium. The molar concentration of precursor (trichloride) was 0.03 mol / L;

[0035] (2) The polyol (ethylene glycol) is dissolved in anhydrous ethanol in anhydrous ethanol; wherein the volume fraction of ethylene glycol in the reduction solution is 80%;

[0036] (3) Under the temperature of 250 ° C, the stirring rate is 600 rpm, the reduction solution is added to the hemorrhid-protected body solution for 2 h, solid-liquid separation, sequentially use acetone, deionized water, and anhydrous ethanol to wash the solid, placed in temperature Ultra-fine spherium powder is obtained in vacuo and ground at 40 ...

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Abstract

The invention relates to a method for preparing spherical ruthenium powder through a polyol reduction method, and belongs to the technical field of precious metal material preparation. According to the method, polyol is adopted as a reducing agent to reduce ruthenium in a ruthenium precursor solution, and by controlling the amount of the reducing agent, the system pH value, reaction temperature and time, the high-purity ultra-fine spherical ruthenium powder with the particle diameter being 150-250 nm is prepared. According to the method, the prepared ruthenium powder is spherical or subsphaeroidal, the technology of the method is simple, the prepared ruthenium powder is high in purity, small in particle size and good in dispersibility, and can serve as a raw material of a ruthenium seriessputtering target material.

Description

Technical field [0001] The present invention relates to a method of preparing spherium tantalum powder by a polyol reduction method, belonging to the technical field of precious metal materials. Background technique [0002] Ruthenium (RU) is a platinum group metal in Group VIII, and the method of preparing high purity pink at home and abroad is mainly chemical. The basic principle is to prepare the tantalum material, and the ruthenium is converted into a cation by a certain oxidant, and then uses Ruo. 4 With a higher vapor pressure, ruthenium is separated from impurity cation separation by distillation, and then a method of separating ruthenium and impurity anion is achieved by a method of precipitation, calcination and reduction, and finally preparing high purity ruthenium powder. The production process has a shortcomings of long production cycle, complex operating process and higher temperature. Therefore, there is a need to develop a production method of short production cycl...

Claims

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Application Information

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IPC IPC(8): B22F9/24
CPCB22F9/24Y02P10/20
Inventor 张佳敏段云彪胡劲张世辉蒋中鸣何亚
Owner KUNMING UNIV OF SCI & TECH
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