TiI4 Purification and Storage via Sublimation and Inert Sealing
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Solution Overview
Problem
The existing methods for purifying and storing TiI4 for semiconductor chip manufacturing are inadequate, as TiI4 is sensitive to air and its quality is not consistently maintained at the required high purity levels for reliable deposition of Ti-containing films.
Innovation Solution
A method involving the introduction of crude TiI4 into a sublimator with a cold trap to evaporate volatile impurities under vacuum, followed by sublimation in a hot oil bath to achieve high purity, and storage in a dried stainless-steel canister under inert conditions to prevent decomposition.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Reliability
If TiI4 is stored in conventional containers, then storage simplicity is maintained, but TiI4 decomposes due to air exposure and moisture
Solution Approach 1:
The patent applies inert atmosphere by storing purified TiI4 in a glove box filled with inert gas (nitrogen or argon) and sealing the container with metallic sealing. This creates an oxygen-free environment that prevents TiI4 decomposition while maintaining storage simplicity.
Solution Approach 2:
The patent extracts harmful factors (air and moisture) from the storage environment by using a sealed glove box system with inert atmosphere, removing these contaminants before they can contact and decompose the TiI4 material.
2Manufacturing precision
If conventional purification methods are used, then process simplicity is maintained, but TiI4 purity does not reach required levels for consistent film deposition
Solution Approach 1:
The patent applies phase transitions by using sublimation to purify TiI4. The crude TiI4 is heated in a sublimator to vaporize the material, and the vapor condenses on a cold trap coated with tungsten disulfide. This phase change process achieves high purity (99.99% or higher) by separating volatile TiI4 from non-volatile impurities.
Solution Approach 2:
The patent uses a cold trap coated with tungsten disulfide as an intermediary substance that facilitates the purification process. The cold trap surface provides a site for controlled condensation of TiI4 vapor, enabling efficient separation and purification without requiring complex additional equipment.
3Reliability
If TiI4 is handled in conventional environments, then operational simplicity is maintained, but decomposition occurs during handling
Solution Approach 1:
The patent applies inert atmosphere by performing all handling operations within a glove box filled with inert gas. This allows operators to manipulate TiI4 materials without direct air exposure, maintaining quality consistency while keeping the handling process straightforward through sealed container transfer.
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
This method ensures TiI4 purity of 99% w/w or higher, preventing decomposition and ensuring consistent vapor deposition, thereby maintaining high-quality Ti-containing film production.
Implementation Method 1
collecting the evaporated volatile impurities in the cold trap
Implementation Method 2
evaporating volatile impurities in the crude TiI4 under vacuum at room temperature in the sublimator
Implementation Method 3
placing the sublimator, after the step of removing the volatile impurities, in a hot oil bath under vacuum at a temperature to evaporate TiI4 and form powders or a solid in the cold trap of the sublimator
Implementation Method 4
sublimating the powers or the solid under vacuum at the temperature to obtain the purified TiI4
Implementation Method 5
filling the pure TiI4 into the dried stainless-steel canister in the glove box, and sealing the dried stainless steel canister containing the pure TiI4 with metallic sealing in the glove box
Data Source
AI summary
Disclosed are methods for purification of a crude TiI4 for deposition of Ti-containing films including evaporating volatile impurities in the crude TiI4 under vacuum at room temperature in a sublimator and removing the volatile impurities, placing the sublimator in a hot oil bath under vacuum at a temperature to evaporate TiI4 and form powders or a solid, and sublimating the powers or the solid under vacuum at the temperature to obtain the purified TiI4. Disclosed are methods for storage of a pure TiI4 including drying a stainless-steel canister, instantaneously moving the dried stainless steel canister into a glove box under inert atmosphere at room temperature, moving the pure TiI4 into the glove box, filling the pure TiI4 into the dried stainless-steel canister, and sealing the dried stainless steel canister containing the pure TiI4 with metallic sealing.