Multielement Nanoparticle Analysis of Semiconductor Process Chemicals Using spICP-QQQ

Significance of the topic

Semiconductor manufacturing processes require stringent control of nanometer-scale contaminants to ensure device performance and yield. Monitoring metal-containing nanoparticles in process chemicals, wafers, and cleaning solutions is critical to prevent electrical defects and layer growth interference.

Aims and overview of the study

This study demonstrates a single-run, multi-element nanoparticle analysis method for Ag, Fe3O4, Al2O3, Au, and SiO2 in semiconductor-grade tetramethylammonium hydroxide (TMAH) using single particle ICP-QQQ technology. The goal was to streamline detection, sizing, and quantification of diverse nanoparticles within a single analytical sequence.

Methodology and used instrumentation

• Sample preparation: Dispersion of nanoparticle standards into 1 percent TMAH with serial dilutions to achieve ppt to ppb concentrations
• Standards: 60 nm Ag NPs for nebulization efficiency determination, plus Fe3O4, Al2O3, Au, and SiO2 nanoparticle reference materials
• Instrumentation: Agilent 8900 triple quadrupole ICP-MS with quartz torch, PFA concentric nebulizer, quartz spray chamber, platinum-tipped cones, and self-aspirating autosampler
• Operating conditions: MS/MS mode with Q1 and Q2 unit mass resolution; use of H2, NH3, or He cell gas for interference removal; 100 microsecond dwell time in Fast Time Resolved Analysis
• Software: Agilent ICP-MS MassHunter Single Nanoparticle Application Module in Rapid Multi-Element Nanoparticle Analysis mode for sequential acquisition of up to sixteen elements

Main results and discussion

• Nebulization efficiency calculated at 8.1 percent using a 60 nm Ag nanoparticle standard
• Simultaneous acquisition of five elements reduced per-sample analysis time by approximately seven minutes compared to separate runs
• Clear discrimination and sizing of mixed nanoparticles, with detection of 30 nm Fe3O4 alongside 200 nm SiO2
• Stability tests over ten hours revealed dissolution of Ag NPs, sedimentation or adsorption of Fe3O4 NPs, and stable behavior for Al2O3, SiO2, and Au nanoparticles

Benefits and practical applications

This approach offers significant time savings, reduced contamination risk through single-vial analysis, and comprehensive multi-element characterization. It supports quality control in semiconductor fabrication by enabling rapid screening of process chemicals and cleaning baths for nanoparticle contaminants.

Future trends and potential applications

Expansion to additional elements and smaller particle sizes could further enhance contamination monitoring. Integration with automated QA/QC workflows and adoption of advanced reaction cell chemistries may improve sensitivity and extend the technique to complex matrices beyond TMAH solutions.

Conclusion

Single particle ICP-QQQ combined with Rapid Multi-Element Nanoparticle Analysis software enables fast, accurate, and interference-free characterization of diverse nanoparticles in semiconductor-grade chemicals, improving efficiency and reliability in contamination control.

References

• Susana Nunez et al Analysis of 10 nm gold nanoparticles using high sensitivity of the Agilent 8900 ICP-QQQ Agilent publication 5991-6944EN
• Jenny Nelson et al Single Nanoparticle Analysis of Asphaltene Solutions using ICP-QQQ Agilent publication 5991-9498EN
• Michiko Yamanaka Steve Wilbur Accurate determination of TiO2 nanoparticles in complex matrices using Agilent 8900 ICP-QQQ Agilent publication 5991-8358EN
• Michiko Yamanaka Takayuki Itagaki Steve Wilbur High sensitivity analysis of SiO2 nanoparticles using Agilent 8900 ICP-QQQ in MS/MS mode Agilent publication 5991-6596EN
• Michiko Yamanaka Takayuki Itagaki Steve Wilbur Measuring multiple elements in nanoparticles using spICP-MS Acquire NP data for up to 16 elements in Rapid Multi-Element Nanoparticle Analysis mode Agilent publication 5994-0310EN
• Craig Jones Emmett Soffey Mark Kelinske Rapid Multielement Nanoparticle Analysis Using Single-Particle ICP-MS/MS Spectroscopy 2019 34 5 10–20
• Steve Wilbur Michiko Yamanaka Sebastien Sannac Characterization of nanoparticles in aqueous samples by ICP-MS Agilent publication 5991-5516EN