DCR Sublimation Purification via Carbon Monoxide Atmosphere
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Solution Overview
Problem
Conventional methods for producing dodecacarbonyl triruthenium (DCR) are inefficient for large-scale purification due to low sublimation rates and thermal decomposition issues, limiting the stable supply of high-purity DCR for industrial applications.
Innovation Solution
A sublimation method using a carbon monoxide atmosphere at elevated temperatures, allowing for efficient purification of crude DCR with reduced impurity elements, where the crude DCR is heated in a CO atmosphere and then cooled to precipitate high-purity DCR, while suppressing thermal decomposition.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If the heating temperature is elevated to increase the sublimation efficiency, then the sublimation rate improves, but thermal decomposition of crude DCR occurs and the yield of DCR is lowered
Solution Approach 1:
The patent applies an inert atmosphere (nitrogen or carbon monoxide gas) during the sublimation process to prevent thermal decomposition of crude DCR. The inert gas environment excludes oxygen and other reactive substances that could cause decomposition, allowing the crude DCR to be heated to higher temperatures (100-150°C) to achieve high sublimation rates while maintaining product integrity and yield.
2Manufacturing precision
If a small amount of crude DCR is treated by sublimation, then the purification efficiency is good, but a large amount of crude DCR cannot be treated at a time
Solution Approach 1:
The patent employs a sublimation apparatus with multiple heating zones and a layered arrangement of crude DCR samples. The crude DCR is divided into multiple portions placed at different positions (e.g., multiple boats or layered arrangement), allowing simultaneous treatment of large quantities while maintaining uniform heating and efficient sublimation across all portions, thus scaling up production without sacrificing purification efficiency.
3Stability of the object's composition
If the crude DCR is heated to about 80°C and sublimated, then the sublimation process is gentle, but it takes a long time and a large amount of crude DCR cannot be homogeneously treated
Solution Approach 1:
The patent utilizes a dynamic heating system with multiple independently controlled heating zones at different temperatures (e.g., first heating zone at 80-100°C, second heating zone at 100-150°C). This allows the sublimation process to progress dynamically through different temperature stages, initially gentle to preserve composition, then intensifying to reduce overall processing time and ensure homogeneous treatment of large amounts of crude DCR.
Data Source
AI summary
The present invention provides a method for producing DCR that can efficiently sublimate a large amount of crude DCR to stably supply DCR. Also, the present invention relates to a sublimation apparatus applicable to the production method. The method for producing an organoruthenium compound for a chemical vapor deposition raw material containing dodecacarbonyl triruthenium (DCR) includes the step for purifying DCR by separating impurity elements from crude DCR by a sublimation method, and in the purification step, crude DCR is heated and sublimated in an atmosphere having a carbon monoxide concentration of 30 to 100% and then cooled to precipitate DCR. According to the present invention, a large amount of crude DCR can be efficiently sublimated, and thus a large amount of DCR can be supplied stably.