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Method and device for preparing high-purity ruthenium

A high-purity, absorption device technology, applied in the field of preparing high-purity ruthenium, can solve the problems of long oxidative distillation time, high operating cost, difficult removal of iron and silicon, etc., and achieves short oxidative distillation time, improved purity, and high ruthenium extraction rate. Effect

Inactive Publication Date: 2012-09-05
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention can effectively solve the problems in the prior art that the oxidative distillation time is too long, the distillation efficiency is too low, the operating cost is relatively large, the separation of osmium is not complete, and the removal of iron and silicon is difficult, and it can be used for large-scale industrial purification of ruthenium Hydrochloric acid solution and preparation of high-purity ruthenium

Method used

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  • Method and device for preparing high-purity ruthenium
  • Method and device for preparing high-purity ruthenium
  • Method and device for preparing high-purity ruthenium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] (1) One-stage oxidation and vacuum distillation to catch osmium.

[0076] Put 1.5L ruthenium hydrochloric acid absorbing stock solution containing ruthenium 31.53g / L in the quartz flask (22), heat the ruthenium solution to 80°C by the oil bath heater (23), turn on the vacuum pump (19), and pass through the vacuum two-way valve (18) Adjust the internal vacuum to about 20KPa, turn on the rotary packing bed (7), and adjust the rotor speed of the rotary packing bed to 2000r / min through the frequency converter. (25) the ruthenium solution in the quartz flask (22) is regulated as 0.5m through liquid flowmeter (24) 3 / h enters the central liquid distributor (3) of the rotating packed bed from the liquid inlet pipe (2), and simultaneously from the constant pressure funnel (20) on the liquid inlet pipeline (2) according to the reaction equivalent multiple (due to the 3M In the hydrochloric acid system, ruthenium mainly exists as tetravalent, and a small amount of ruthenium exis...

Embodiment 2

[0092] (1) One-stage oxidation and vacuum distillation to catch osmium.

[0093] The one-stage oxidative vacuum distillation for removing osmium is basically the same as in Example 1, except that the rotational speed of the rotating packed bed rotor is adjusted to 1200 r / min.

[0094] (2) Two-stage oxidation and vacuum distillation to extract ruthenium.

[0095] The extraction of ruthenium by two-stage oxidation and vacuum distillation is basically the same as in Example 1, except that the rotor speed of the rotating packed bed is adjusted to 2000 r / min, and the reaction temperature is adjusted to 80°C.

[0096] (3) Repeat oxidation distillation to extract ruthenium.

[0097] Repeat once oxidative distillation to extract ruthenium. The operating conditions are completely the same as the two-stage oxidative vacuum distillation in Example 2 to extract ruthenium. The results of analysis of impurity elements in the three ruthenium hydrochloric acid absorption solutions are shown...

Embodiment 3

[0105] (1) One-stage oxidation and vacuum distillation to catch osmium.

[0106] One-stage oxidative vacuum distillation to remove osmium The operating conditions are completely the same as in Example 1.

[0107] (2) Two-stage oxidation and vacuum distillation to extract ruthenium.

[0108] The operating conditions for extracting ruthenium by two-stage oxidation and vacuum distillation are completely the same as in Example 1.

[0109] (3) Repeat oxidation distillation to extract ruthenium.

[0110] Repeat once oxidative distillation to extract ruthenium operating condition completely with embodiment 1. The results of analysis of impurity elements in the three ruthenium hydrochloric acid absorption solutions are shown in Table 2.

[0111] (4) Ammonium chloride crystallization precipitates ruthenium.

[0112] The operating conditions for ammonium chloride crystallization and precipitation of ruthenium are basically the same as in Example 1, except that the holding temperatur...

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Abstract

The invention relates to a method and a device for preparing high-purity ruthenium. The method comprises the following steps that: hydrogen dioxide is added into ruthenium hydrochloride solution to be undertaken one section of oxidation distillation reaction, then oxidant is added into the liquid to be undertaken a second section of adequate oxidation distillation reaction, then the oxidation distillation is repeatedly performed to extract the ruthenium, ruthenium tetroxide gas which is discharged from the second section of oxidation reaction is adequately collected, the ruthenium tetroxide gas is transformed to ruthenium hydrochloride absorption liquid, ammonium chloride is added into the ruthenium hydrochloride absorption liquid to be crystallized and precipitated, and the prepared ammonium chloride ruthenium precipitant is calcined and reduced to sponge ruthenium under the atmosphere of hydrogen; and the prepared sponge ruthenium is dried under the atmosphere of the hydrogen after being boiled and washed by mixed acid of aqua regia and hydrofluoric acid to obtain the high-purity ruthenium.

Description

technical field [0001] The invention relates to a method and a device for preparing high-purity ruthenium. The high-purity ruthenium prepared in the invention refers to high-purity ruthenium powder used for sputtering targets. Background technique [0002] The high-purity ruthenium used for sputtering targets in the production of semiconductor VLSI requires its purity to be at least 4N5 (99.995%), and the content of impurities such as alkali metals, transition metal elements, radioactive elements, and gas elements in the materials is also required very low. It is specifically required that in the high-purity ruthenium sputtering target, the gaseous components are excluded, and the purity of pure ruthenium is at least 99.995%. [0003] At present, there are few published literatures about the preparation method of high-purity ruthenium. The main summary is: [0004] (1) Fire refining sponge ruthenium purification technology. Patent No. is the U.S. Patent of " method for p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/26C23C14/34
Inventor 刘伟生章德玉张国林唐晓亮
Owner LANZHOU UNIVERSITY
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