Organotin Precursor Synthesis for High-Purity Tin Oxide Deposition
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Solution Overview
Problem
Existing methods struggle to produce organotin compounds with alkyl and alkylamino groups in highly pure forms, particularly for use in the deposition of high-purity tin oxide films in microelectronic device manufacturing, due to the difficulty in separating polyalkyl by-products with similar boiling points.
Innovation Solution
A process involving the reaction of a compound of Formula R1SnX3 with Li(R)2N and R2NH, where R2NH is in molar excess, forming an intermediate Lewis base adduct that enhances the selectivity and purity of compounds like tris(dimethylamido)isopropyl tin, minimizing impurities such as bis(dimethylamido)diisopropyl tin.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional distillation methods are used to separate polyalkyl by-products from organotin compounds, then the separation process is simple, but the purity of the organotin compound cannot be sufficiently improved due to close proximity in boiling points
Solution Approach 1:
The invention changes the chemical parameters of the reaction system by using a tin halide compound reacting with an alkyl lithium compound in the presence of an alkylamine. This parameter change in the synthesis pathway fundamentally alters the product distribution, achieving high purity organotin compounds with minimal polyalkyl by-products that cannot be separated by conventional distillation.
Solution Approach 2:
The invention performs preliminary action by carefully controlling the reaction conditions and sequence - first forming the organotin compound with specific stoichiometry, then removing the alkylamine solvent under reduced pressure before any by-products can form or accumulate. This preliminary control prevents the formation of difficult-to-separate impurities.
2Manufacturing precision
If conventional synthesis methods are used to prepare organotin compounds with alkyl and alkylamino groups, then the synthesis process is straightforward, but the selectivity is insufficient resulting in polyalkyl by-products that cannot be effectively removed
Solution Approach 1:
The invention changes key reaction parameters including using specific molar ratios of reactants (tin halide:alkyl lithium:alkylamine), controlling the addition sequence, and performing the reaction at controlled temperatures. These parameter changes achieve exceptional selectivity for the desired organotin compound while maintaining a relatively simple synthesis process.
Solution Approach 2:
The alkylamine serves as an intermediary substance that facilitates the reaction between tin halide and alkyl lithium compound. It acts as a solvent and potential ligand during the reaction, then is easily removed under reduced pressure, leaving behind high-purity organotin compound without polyalkyl by-products.
3Manufacturing precision
If high-purity organotin compounds are produced through multiple purification steps, then the purity is improved, but the production time and complexity increase
Solution Approach 1:
The invention performs preliminary action by removing the alkylamine solvent under reduced pressure immediately after the reaction is complete, before any decomposition or side reactions can occur. This preliminary removal step prevents the formation of difficult-to-separate by-products, eliminating the need for multiple subsequent purification steps and maintaining high productivity.
Solution Approach 2:
The invention takes out the alkylamine component from the reaction mixture under reduced pressure, separating it from the organotin compound product. This extraction method is highly effective because the alkylamine is present in excess and has different volatility characteristics, allowing for clean separation that yields high-purity product in a single step.
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 achieves high-purity organotin compounds, with impurity levels below 0.5% by mole, suitable for use in extreme ultraviolet lithography techniques, ensuring high-quality tin oxide film deposition in microelectronic devices.
Implementation Method 1
forming an intermediate Lewis base adduct that enhances the selectivity and purity of compounds like tris(dimethylamido)isopropyl tin
Data Source
AI summary
Provided is a facile process for preparing certain organotin compounds having alkyl and alkylamino substituents. The process provides organotin precursor compounds, for example tris(dimethylamido)isopropyl tin, in a highly pure form. As such, the products of the process are particularly useful in the deposition of high-purity tin oxide films in, for example, extreme ultraviolet light (EUV) lithography techniques used in microelectronic device manufacturing.