ICP/MS, ICP-OES, AAS, ICP/MS/MS, GD/MP/ICP-AES
IndustriesSemiconductor Analysis
ManufacturerAgilent Technologies
Significance of the Topic
Integrated circuit manufacturing demands control of metallic trace elements at the parts-per-trillion level to ensure device reliability and yield. Nanoscale features (down to 10 nm) make contamination from wafer substrates, process chemicals, and equipment a critical challenge.
Objectives and Study Overview
This whitepaper presents Agilent Technologies’ evolution of atomic spectroscopy solutions tailored for semiconductor applications. It reviews the development of single and triple quadrupole ICP-MS, specialized sample introduction systems, automated wafer surface analysis, online monitoring architectures, and complementary techniques such as ICP-OES, MP-AES, and GFAAS.
Methodology and Instrumentation Used
Multi-element analysis of trace contaminants relies principally on inductively coupled plasma mass spectrometry (ICP-MS) and triple quadrupole ICP-QQQ for enhanced interference removal and sensitivity. Key instruments include:
- Agilent 7900 single quadrupole ICP-MS: compact benchtop design, cool plasma, ORS4 collision reaction cell, optional reaction gases for improved detection of P, As, Si, and V (down to <3 ppt).
- Agilent 8800/8900 triple quadrupole ICP-MS: MS/MS operation, dual-stage mass filtering, cool plasma, multiple cell gas lines for advanced reactions, and Pt-tipped interface cones for organic matrices.
- Sample introduction kits: PFA inert kits for HF handling, specialized torches and spray chambers for corrosive acids, Peltier-cooled spray chambers, and oxygen addition via an optional gas line to oxidize carbon in organic solvent analysis.
- Automation platforms: Vapor phase decomposition (VPD) scanners coupled with ICP-MS for surface metal extraction, integrated I-AS autosampler with continuous ultrapure water rinse, CSI and ScoutDX online monitoring systems for real-time process chemical inspection.
Main Results and Discussion
Agilent’s innovations over three decades—off-axis ion lenses, cool plasma, MS/MS, and low-contamination gas paths—have advanced detection limits and accuracy. Demonstrated applications include:
- Direct analysis of volatile organic solvents (IPA, NMP) with controlled oxygen addition, stabilizing the plasma and preventing carbon deposition.
- Accurate measurement of concentrated HF, H₂SO₄, and H₃PO₄ using PFA inert sample introduction with Pt or sapphire injectors and optimized dilution strategies.
- Automated VPD-ICP-MS achieving uniform extraction of metals from thermally grown or native SiO₂ layers (0.25–100 nm), supporting routine wafer contamination assays.
- Continuous online monitoring setups enabling rapid standard addition calibrations and multi-stream sampling for ultrapure water and chemical feeds.
Benefits and Practical Applications of the Method
These solutions deliver:
- Sub-ppt detection limits and broad multi-element coverage in complex matrices.
- High throughput and reduced turnaround times via autosamplers and automated workflows.
- Enhanced process control through online monitoring and immediate contamination alerts.
- Improved yield and device reliability by early identification and mitigation of trace metal sources.
Future Trends and Potential Applications
Emerging directions include integration of field-flow fractionation for nanoparticle characterization, expanded MS/MS reaction chemistries for new elemental targets (S, Cl, rare earth elements), and synergy with machine learning algorithms for predictive quality control. Further miniaturization and cloud-based data analytics will streamline global fab contamination management.
Conclusion
Agilent’s comprehensive atomic spectroscopy portfolio—from ICP-MS and ICP-QQQ to ICP-OES, MP-AES, and GFAAS—addresses the semiconductor industry’s most stringent contamination challenges. Continuous innovation, automation compatibility, and rigorous contamination control practices enable accurate, reliable trace and ultratrace elemental analysis across all stages of IC fabrication.
References
Agilent Technologies. Solutions for the Semiconductor Industry. Publication 5994-1841EN.
Agilent Technologies. Specifications for 7900 and 8900 Semiconductor Configurations. Publications 5991-3780EN and 5991-7009EN.
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