Particulate Ruthenium Production via Controlled Precipitation

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Solution Overview

Problem

Existing methods for producing ruthenium particles with high purity and specific surface area are not efficient in achieving the required specifications for spark plasma sintering processes.

Innovation Solution

A process involving the formation of a reaction mixture by dissolving RuO4 in hydrochloric acid and combining it with an ammonium chloride solution at specific molar ratios and temperatures, followed by separation and calcination to produce particulate ruthenium with a purity of ≥99.99 wt.% and a specific surface area of 0.2 to 0.5 m2/g.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If existing methods are used to produce ruthenium particles, then production can proceed with conventional processes, but the resulting particles do not achieve the required purity and specific surface area specifications for spark plasma sintering

Engineering Contradiction:
Improvepurity and specific surface area of ruthenium particlesVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent applies parameter changes by precisely controlling the molar ratio of ammonium chloride to ruthenium (3:1 to 6:1), maintaining specific temperature ranges (55-90°C), and controlling pH values (-0.6 to 0) during the reaction process. These parameter optimizations enable the production of ruthenium particles with purity ≥99.99 wt.% and specific surface area of 0.2 to 0.5 m2/g, resolving the contradiction between manufacturing precision and ease of manufacture.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs preliminary action by first preparing a hydrochloric solution with dissolved ruthenium species (15-22 wt.% Ru) and an aqueous ammonium chloride solution (200-600 g/litre) before combining them. This pre-preparation of reagents with specific concentrations and compositions ensures that when the reaction occurs, the particles form with the desired properties, achieving high purity and specific surface area while maintaining process simplicity.

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If the molar ratio of ammonium chloride to ruthenium is increased, then particle formation is improved, but reagent consumption and solution volume increase

Engineering Contradiction:
Improveparticle formation qualityVSAvoidammonium chloride consumption
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent applies partial or excessive action by using a molar ratio of ammonium chloride to ruthenium in the range of 3:1 to 6:1. This ratio provides sufficient ammonium chloride to ensure complete reaction and optimal particle formation (improving manufacturing precision) while avoiding excessive reagent consumption. The lower end of this range (3:1) already provides adequate reaction conditions, making the process efficient.

Inventive Principle:
Principle #16Partial or excessive action

3Productivity

If the reaction temperature is increased to improve reaction rate, then productivity increases, but energy consumption and risk of unwanted side reactions increase

Engineering Contradiction:
Improvereaction rateVSAvoidenergy consumption
Core Design Contradiction:
ProductivityVSUse of energy by moving object

Solution Approach 1:

The patent optimizes the reaction temperature parameter within the range of 55-90°C (preferably 65-85°C). This temperature range is sufficiently high to ensure rapid reaction kinetics and high productivity, yet low enough to minimize energy consumption and prevent unwanted side reactions. The specific pH control (-0.6 to 0) works synergistically with this temperature range to achieve optimal reaction conditions without excessive energy input.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The process effectively produces ruthenium particles with the desired purity and surface area, suitable for spark plasma sintering, while maintaining a controlled pH and temperature to ensure high yield and quality.

Implementation Method 1

dissolving RuO4 in hydrochloric acid and has a content of ruthenium in the form of dissolved ruthenium species

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

forming a reaction mixture by dosing the hydrochloric solution provided in step (1) to the aqueous solution provided in step (2)... and separating solid material formed during step (3) from the hydrochloric reaction mixture

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 3

calcinating the solid material separated in step (4) at an object temperature in the range of 350 to 1,000° C.

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Data Source

PatentUS10913120B2Process for production of particulate ruthenium
Publication Date: 2021.02.09 HERAEUS DEUTSCHLAND GMBH & CO KG

AI summary

Process for the production of particulate ruthenium with a purity of ≤99.99 wt. % and a specific surface area of 0.2-0.5 m2/g, comprising: (1) providing a hydrochloric solution prepared by dissolving RuO4 in hydrochloric acid and has a content of ruthenium in the form of dissolved ruthenium species of 15-22 wt. %; (2) providing an aqueous solution with an ammonium chloride content of 200-600 g/litre; (3) forming a reaction mixture by dosing the hydrochloric solution provided in step (1) to the aqueous solution provided in step (2) at a molar ratio of 1 mol ruthenium: 3-6 mol ammonium chloride, at a temperature of 55-90° C. over the course of 0.2-5 hours and while adjusting and maintaining a pH of −0.6 to 0; (4) separating solid material formed during step (3) from the hydrochloric reaction mixture; and (5) calcinating the solid material separated in step (4) at an object temperature of 350-1,000° C.