Online TOF-MS Impurity Detection for Semiconductor Chemicals

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Solution Overview

Problem

Current methods fail to effectively detect and quantify organic molecular impurities in semiconductor-grade chemicals, which can lead to reduced quality and even ruin semiconductor wafers due to contamination, especially with plasticizers, organophosphates, amines, and antioxidants, and are incompatible with electrospray ionization mass spectrometry due to non-volatile additives.

Innovation Solution

An automated online detection system using remote sampling and preparation modules with pneumatic transfer to a central mass spectrometer, capable of detecting organic analyte impurities through electrospray ionization and mass spectrometry, operating in infusion and speciation modes, with software for semi-quantitative analysis and automatic calibration, and employing organic solvents for better solubility and ionization suppression mitigation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional detection methods are used for organic molecular impurities, then the detection process is simple, but the detection limit is insufficient and cannot achieve sub-parts-per-billion sensitivity

Engineering Contradiction:
Improvedetection limitVSAvoidsystem complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The system is divided into multiple specialized modules: remote sampling module, pneumatic transfer module, organic solvent extraction module, electrospray ionization module, and mass spectrometry module. Each module performs a specific function to achieve sub-ppb detection sensitivity while managing overall system complexity through functional segmentation.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

Organic solvents are introduced as intermediary substances to extract organic molecular impurities from the semiconductor chemicals. The solvents facilitate better solubility and ionization of organic compounds, enabling detection at sub-parts-per-billion levels that conventional methods cannot achieve.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Reliability

If non-volatile additives are present in the sample, then the sample represents real semiconductor chemicals, but electrospray ionization mass spectrometry cannot effectively analyze them

Engineering Contradiction:
Improvesample representativenessVSAvoidionization compatibility
Core Design Contradiction:
ReliabilityVSDifficulty of detecting and measuring

Solution Approach 1:

The system extracts organic molecular impurities from the semiconductor chemical samples using organic solvent extraction. This separation removes the interference of non-volatile additives while maintaining the representativeness of the original sample matrix, enabling effective electrospray ionization mass spectrometry analysis of the extracted organics.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The system changes the physical and chemical parameters of the sample by introducing organic solvents that alter solubility and ionization characteristics. This parameter transformation makes the organic impurities compatible with electrospray ionization while preserving the reliability of the detection results for semiconductor-grade chemical analysis.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If automated online detection is implemented, then real-time monitoring is achieved, but the system complexity and cost increase

Engineering Contradiction:
Improvemonitoring speedVSAvoidautomation level
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The system performs preliminary automated actions including remote sampling, pneumatic transfer, and organic solvent extraction before mass spectrometry analysis. These pre-processing steps are fully automated to enable near-real-time monitoring while reducing manual intervention requirements.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The mass spectrometry system is designed to handle multiple functions: detecting various types of organic impurities (plasticizers, organophosphates, amines, antioxidants), performing quantitative analysis, and providing near-real-time monitoring. This multi-functionality justifies the system complexity by delivering comprehensive semiconductor chemical analysis.

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 system achieves sub-parts-per-billion detection limits, near-real-time monitoring, and improved sensitivity by selectively removing anions and using organic solvents, reducing matrix-induced suppression and cross-contamination, thereby ensuring high-quality semiconductor processing.

Implementation Method 1

capable of detecting organic analyte impurities through electrospray ionization and mass spectrometry

Methodology Applied
Scientific EffectElectrospray ionization: Electrohydrodynamics

Implementation Method 2

remote sampling and preparation modules with pneumatic transfer to a central mass spectrometer

Methodology Applied
Scientific EffectPneumatic transfer: Pressure Gradient

Data Source

PatentUS20240426796A1Automated system for online detection of organic molecular impurities in semiconductor grade chemicals
Publication Date: 2024.12.26 ELEMENTAL SCI
  • US20240426796A1 patent drawing
  • US20240426796A1 patent drawing
  • US20240426796A1 patent drawing

AI summary

An embodiment of an analysis system can include an initial multi-port valve, at least one intermediate multi-port valve, a further multi-port valve, and a time-of-flight mass spectrometer (TOF-MS). The initial multi-port valve can be configured to receive a sample. The at least one intermediate multi-port valve can be fluidly connected to the initial multi-port valve and configured to receive the sample from the initial multi-port valve. A given intermediate multi-port valve can have an ion-exchange column associated therewith. The given intermediate multi-port valve can be configured selectably to one of direct the sample through the ion-exchange column associated therewith (in a speciation mode) or bypass the ion-exchange column (in an infusion mode). The further multi-port valve can be fluidly connected with the at least one intermediate multi-port valve and configured to receive the sample from therefrom. The time-of-flight mass spectrometer (TOF-MS) can be fluidly connected to the further multi-port valve.