Method for preparing high-purity spherical ruthenium powder

A ruthenium powder and spherical technology is applied in the field of preparation of high-purity spherical ruthenium powder, which can solve the problem of high impurity content of ruthenium powder, and achieve the effects of low impurity content and simple process

Inactive Publication Date: 2018-08-17
SINO PLATINUM METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of Na, K, Fe, Cl and other impurities in the produced ruthenium powder is relatively high

Method used

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  • Method for preparing high-purity spherical ruthenium powder
  • Method for preparing high-purity spherical ruthenium powder
  • Method for preparing high-purity spherical ruthenium powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1, see attached figure 1 , the solid ruthenium trichloride is dissolved with high-grade pure hydrochloric acid+deionized water, and the gained ruthenium solution removes cationic impurities by a cation exchange resin to obtain a pure ruthenium solution. :8 Add superior-grade pure urea, age for 24h, then heat the solution to 90°C, stir and react at a constant temperature for 4h, a hydrolysis precipitation reaction occurs, and generate a spherical ruthenium powder precursor—a hydrated ruthenium oxide, which is separated by filtration, washed, and dried; The precursor was placed in a tube furnace, calcined and dehydrated at a constant temperature of 300°C for 1 hour, continued to heat up to 600°C, introduced high-purity hydrogen, and reduced for 4 hours at a constant temperature, and then passed in nitrogen to cool to room temperature to obtain ruthenium powder; then the obtained ruthenium The powder was boiled and washed with nitric acid + hydrofluoric acid in ...

Embodiment 2

[0023] Embodiment 2, see attached figure 1 , the solid ruthenium trichloride is dissolved with superior-grade pure hydrochloric acid+deionized water, and the gained ruthenium solution removes cationic impurities by a cation exchange resin to obtain a pure ruthenium solution; the pH of the ruthenium solution is adjusted to be 5, by ruthenium: urea molar ratio of 1: 6 Add high-grade pure urea, age for 24 hours, then heat the solution to 90°C, stir and react at a constant temperature for 4 hours, hydrolysis and precipitation reaction occurs, and a spherical ruthenium powder precursor - hydrated ruthenium oxide is generated, which is separated by filtration, washed and dried; The body is placed in a tube furnace at a constant temperature of 350°C for calcination and dehydration for 2 hours, then the temperature is raised to 650°C, high-purity hydrogen is introduced, and the constant temperature is reduced for 3 hours, and then nitrogen is passed into and cooled to room temperature ...

Embodiment 3

[0024] Embodiment 3, see attached figure 1 , the solid ruthenium trichloride is dissolved with high-grade pure hydrochloric acid+deionized water, and the gained ruthenium solution removes cationic impurities by a cation exchange resin to obtain a pure ruthenium solution. 6 Add high-grade pure urea, age for 24 hours, then heat the solution to boiling, stir and react at constant temperature for 4 hours, hydrolysis and precipitation reaction occurs, and generate spherical ruthenium powder precursor——hydrated ruthenium oxide, which is separated by filtration, washed, and dried; Place it in a tube furnace at a constant temperature of 350°C for calcination and dehydration for 2 hours, continue to heat up to 650°C, feed high-purity hydrogen, reduce at a constant temperature for 3 hours, and then feed nitrogen to cool to room temperature to obtain ruthenium powder; then the obtained ruthenium powder is in Nitric acid + hydrofluoric acid was used to boil and wash in a polytetrafluoroet...

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Abstract

The invention discloses a method for preparing high-purity spherical ruthenium powder. The method includes the steps that (1) dissolving is conducted, and hydrochloric acid is used for dissolving to obtain a ruthenium hydrochloride solution; (2) ion exchange purification impurity removing is carried out so that a pure ruthenium solution can be obtained; (3) a precursor is prepared, the initial pHvalue of the ruthenium solution obtained in the step (2) is adjusted, a sediment initiator is added, and ageing, heating and stirring are performed to generate the ruthenium powder precursor-sphericalruthenium oxide hydrate; (4) calcination dehydration-hydrogen reduction is carried out, the precursor obtained in the step (3) is put into a tube furnace to be subjected to calcination dehydration atfirst, then nitrogen is connected in for high-temperature reduction, and accordingly spherical metal ruthenium powder is obtained; and (5) mixed acid boiling washing and filtering separation are carried out, deionized water is used for sufficient washing, and the high-purity spherical ruthenium powder can be obtained after vacuum drying. By adoption of the method, the technology is simple, the impurity content in the prepared ruthenium powder is smaller than 10ppm, the microstructure of the ruthenium powder is spherical, the granularity is smaller than 5 microns, and the high-purity sphericalruthenium powder can be used as a raw material for a ruthenium-system sputtering target material.

Description

technical field [0001] The invention relates to the preparation of noble metal powder, in particular to a preparation method of high-purity spherical ruthenium powder. Background technique [0002] The ruthenium powder for computer hard disk memory material target has special index requirements, and the impurities and powder morphology must be strictly controlled, the purity must be above 99.999%, and the microscopic morphology requires spherical or quasi-spherical shape. [0003] At present, the preparation method of domestic ruthenium powder generally adopts secondary oxidation distillation, and the absorption liquid is concentrated and crystallized to obtain RuCl 3 Calcination and hydrogen reduction to prepare ruthenium powder, or oxidize the ruthenium absorption solution and add ammonium chloride for precipitation, calcining and hydrogen reduction to prepare ruthenium powder. The ruthenium powder obtained by this method has coarse and uneven particles, high impurity con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/26B22F1/00
CPCB22F9/26B22F1/065
Inventor 董海刚赵家春崔浩杨海琼李艳琼吴跃东保思敏王亚雄童伟锋吴晓峰
Owner SINO PLATINUM METALS CO LTD
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