Dodecacarbonyl Triruthenium Purification via Low-Oxygen Recrystallization
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Solution Overview
Problem
Ruthenium thin films formed by chemical vapor deposition using dodecacarbonyl triruthenium (DCR) purified by sublimation methods can be contaminated with impurities, and conventional recrystallization methods may introduce gray substances during the purification process.
Innovation Solution
A recrystallization method is optimized by maintaining a dissolved oxygen concentration of 0.2 mg/L or less in the solvent during the dissolution stage, which effectively separates trace impurities and prevents the formation of gray substances, ensuring high-purity DCR for chemical vapor deposition.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If a sublimation method is used to purify DCR, then low-sublimability elements such as Fe can be separated, but the formed ruthenium film is sometimes contaminated with a small amount of impurities
Solution Approach 1:
The patent applies an inert atmosphere (nitrogen or argon gas) during the recrystallization process to prevent oxidation of DCR and formation of gray substances. The inert gas replaces air in the reaction system, creating an oxygen-free environment that eliminates harmful oxidation reactions while allowing effective purification through controlled recrystallization.
Solution Approach 2:
The patent changes the dissolved oxygen concentration parameter to 0.2 mg/L or less during the dissolution stage of recrystallization. This precise parameter control prevents formation of gray substances while enabling effective separation of trace impurities, resolving the contradiction between purification effectiveness and film contamination prevention.
2Manufacturing precision
If a conventional recrystallization method is used to purify DCR, then trace impurities can be removed, but gray substances are formed during the purification process
Solution Approach 1:
The patent introduces an inert atmosphere (nitrogen or argon) during recrystallization to prevent oxidation reactions that form gray substances. The inert gas environment eliminates oxygen from the system, preventing the formation of harmful gray by-products while maintaining the purification effectiveness of the recrystallization process.
Solution Approach 2:
The patent严格控制 the dissolved oxygen concentration to 0.2 mg/L or less during the dissolution stage. This precise parameter control prevents oxidation and gray substance formation while enabling effective trace impurity removal, resolving the contradiction between purification and harmful by-product formation.
3Ease of manufacture
If DCR is used in an unpurified state for thin film formation, then the purification process is simplified, but ignition may occur upon opening the material container due to impurity elements such as Fe, Al, and Cr
Solution Approach 1:
The patent extracts harmful impurity elements (Fe, Al, Cr) from DCR through a simplified recrystallization process performed in an inert atmosphere. This selective extraction removes ignition-causing impurities while maintaining process simplicity, resolving the contradiction between manufacturing ease and process safety.
Solution Approach 2:
The patent uses an inert atmosphere during recrystallization to safely handle and purify DCR containing reactive impurities. The inert environment prevents unwanted reactions during purification while enabling effective removal of harmful elements, ensuring both simplicity and safety.
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 method achieves impurity separation even at trace levels, preventing contamination in the formed ruthenium thin films and suppressing the formation of gray substances, thereby ensuring high film purity and stability.
Implementation Method 1
use of the difference in solubility in a predetermined solvent between DCR and impurities
Implementation Method 2
a precipitation stage of precipitating DCR from the solvent
Data Source
AI summary
An object of the present invention is to provide a purification method to give dodecacarbonyl triruthenium (DCR) which serves as a raw material for chemical vapor deposition and does not cause the contamination of a thin film with impurities even when used to form a ruthenium thin film. The present invention relates to a method in which the dissolved oxygen concentration in the solvent is made 0.2 mg/L or less in at least a dissolution stage, and an organic ruthenium compound including DCR as a raw material for chemical vapor deposition is purified by a recrystallization method. The present invention allows a trace amount of impurities to be separated from DCR. When a ruthenium thin film is formed by use of DCR thus obtained, the formed film is hardly contaminated with impurities. Additionally, the purification method of the present invention is also applicable for recovering/purifying DCR after being used for the formation of a ruthenium thin film.