Trichlorosilane Purification via Complexation Distillation

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Solution Overview

Problem

Current methods for purifying technical grade trichlorosilane and silicon tetrachloride to achieve electronic grade quality are inefficient, as they fail to adequately remove impurities such as boron, metallic, and phosphorus chlorides, limiting their use in semiconductor production and epitaxial layer growth due to high investment costs and impurity residue.

Innovation Solution

A three-step process involving complexation of boron and metallic impurities with diphenylthiocarbazone and triphenylchloromethane, followed by distillation to remove impurities and achieve electronic grade purity, utilizing a plant with specific temperature and reflux control to ensure effective impurity removal.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If hyper distillation is used to purify TCS TG and TET TG, then impurity removal is achieved, but investment costs become very high due to high columns and high reflux ratios

Engineering Contradiction:
Improvepurity levelVSAvoidcolumn height and reflux ratio
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by performing complexation reactions before distillation to convert impurities into separable forms. Diphenylthiocarbazone and triphenylchloromethane are added to complex with boron, phosphorus, and arsenic impurities, transforming them into compounds that can be more easily removed in subsequent distillation steps, thereby reducing the complexity of the distillation process while maintaining high purity levels

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses complexing agents (diphenylthiocarbazone and triphenylchloromethane) as intermediaries to facilitate impurity removal. These intermediaries selectively bind to impurities like boron trichloride, phosphorus trichloride, and arsenic trichloride, forming complex compounds that have different volatility characteristics, enabling more efficient separation during distillation without requiring excessively high columns or reflux ratios

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If wet nitrogen bubbles process is used, then purification is achieved, but purity grade does not exceed P-type value of 100 ohm-cm due to limited complexing capacity

Engineering Contradiction:
Improvepurity gradeVSAvoidcomplexing capacity
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent changes the chemical parameters of the complexing agents by using diphenylthiocarbazone and triphenylchloromethane instead of water. These organic complexing agents have significantly higher complexing capacity for metal impurities compared to water molecules. The patent optimizes parameters such as the molar ratio of complexing agents to impurities, temperature, and reaction time to maximize complexation efficiency, achieving purity grades well above P-type 100 ohm-cm

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a composite approach by using two different complexing agents (diphenylthiocarbazone and triphenylchloromethane) working together. Each agent has complementary complexing capabilities, and their combined use enhances the overall complexing capacity and selectivity for different impurities, achieving superior purification results compared to using a single agent or water-based systems

Inventive Principle:
Principle #40Composite materials

3Manufacturing precision

If complexation with electron rich big molecules is used, then purification is improved, but optimal electronic grade purity is not achieved for epitaxial reactor applications

Engineering Contradiction:
Improvepurity levelVSAvoidepitaxial layer quality
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent applies local quality by using different complexing agents for different impurity types. Diphenylthiocarbazone is particularly effective for boron compounds, while triphenylchloromethane targets phosphorus and arsenic impurities. This selective complexation approach ensures that each impurity type is addressed by the most effective agent, achieving the optimal purity level required for epitaxial reactor applications where even trace impurities can affect semiconductor quality

Inventive Principle:
Principle #3Local quality

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 significantly reduces boron and metallic impurities, achieving a high purity level suitable for semiconductor production and epitaxial layer growth, with improved stability and repeatability compared to previous methods.

Implementation Method 1

complexation of the boron impurities (trichloride BCl3) and other metallic impurities by addition of diphenylthiocarbazone and triphenylchloromethane, with the formation of complex macromolecules having high boiling point

Methodology Applied
Scientific EffectComplexation: Chemical Bonding

Implementation Method 2

first column distillation of the complexation step products, wherein the complexed boron impurities, together with other metallic impurities are removed as bottoms

Methodology Applied
Scientific EffectDistillation: Distillation

Data Source

PatentUS7879198B2Processes for the purification of trichlorosilane and silicon tetrachloride
Publication Date: 2011.02.01 GLOBALWAFERS CO LTD
  • US7879198B2 patent drawing
  • US7879198B2 patent drawing

AI summary

The present disclosure relates to processes and systems for purifying technical grade trichlorosilane and/or technical grade silicon tetrachloride into electronic grade trichlorosilane and/or electronic grade silicon tetrachloride.