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Download Hi-Res ImageDownload to MS-PowerPointCite This:Anal. Chem. 2020, 92, 18, 12518-12527
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Elemental Characterization of Al Nanoparticles Buried under a Cu Thin Film: TOF-SIMS vs STEM/EDX

  • Agnieszka Priebe*
    Agnieszka Priebe
    Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
    *Email: [email protected]
    More by Agnieszka Priebe
    Orcidhttp://orcid.org/0000-0003-0425-246X
  • , 
  • Jean-Paul Barnes
    Jean-Paul Barnes
    Univ. Grenoble Alpes, CEA, LETI, 38000 Grenoble, France
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  • , 
  • Thomas Edward James Edwards
    Thomas Edward James Edwards
    Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
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  • , 
  • Emese Huszár
    Emese Huszár
    Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
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  • , 
  • Laszlo Pethö
    Laszlo Pethö
    Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
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  • , and 
  • Johann Michler
    Johann Michler
    Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
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Cite this: Anal. Chem. 2020, 92, 18, 12518–12527
Publication Date (Web):August 18, 2020
https://doi.org/10.1021/acs.analchem.0c02361
Copyright © 2020 American Chemical Society
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    Abstract

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    In this work, we present a comprehensive comparison of time-of-flight secondary ion mass spectrometry (TOF-SIMS) and scanning transmission electron microscopy combined with energy-dispersive X-ray spectroscopy (STEM/EDX), which are currently the most powerful elemental characterization techniques in the nano- and microscale. The potential and limitations of these methods are verified using a novel dedicated model sample consisting of Al nanoparticles buried under a 50 nm thick Cu thin film. The sample design based on the low concentration of nanoparticles allowed us to demonstrate the capability of TOF-SIMS to spatially resolve individual tens of nanometer large nanoparticles under ultrahigh vacuum (UHV) as well as high vacuum (HV) conditions. This is a remarkable achievement especially taking into account the very small quantities of the investigated Al content. Moreover, the imposed restriction on the Al nanoparticle location, i.e., only on the sample substrate, enabled us to prove that the measured Al signal represents the real distribution of Al nanoparticles and does not originate from the artifacts induced by the surface topology. The provided comparison of TOF-SIMS and STEM/EDX characteristics delivers guidelines for choosing the most optimal method for efficient characterization of nano-objects.

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.analchem.0c02361.

    • Diagram of the deposition setup (Figure S1); size distribution of Al nanoparticles measured with a quadrupole mass spectrometer (Figure S2); TOF-SIMS depth profiles of Al nanoparticles buried under the Cu thin film obtained with Bi32+ beam (Figure S3); topology of the sample surface imaged with SEM (Figure S4); 2D side views (in depth) of the sample’s main isotopes: 27Al+, 63Cu+, 28Si+, and their overlay obtained with the 69Ga+ beam (Figure S5); TOF-SIMS depth profiles of Al nanoparticles buried under the Cu thin film obtained with Ga+ beam (Figure S6); STEM/EDX depth profiles (Figure S7) (PDF)

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    Cited By

    This article is cited by 13 publications.

    1. Agnieszka Priebe, Abdessalem Aribia, Jordi Sastre, Yaroslav E. Romanyuk, Johann Michler. 3D High-Resolution Chemical Characterization of Sputtered Li-Rich NMC811 Thin Films Using TOF-SIMS. Analytical Chemistry 2023, 95 (2) , 1074-1084. https://doi.org/10.1021/acs.analchem.2c03780
    2. Agnieszka Priebe, Bryan Dousse, Chia-Yu Tzou, Georgios Papadopoulos, Ivo Utke, Abdelhak Bensaoula, Johann Michler, Carlos Guerra-Nuñez. Real-Time In Situ Parallel Detection of Elements and Molecules with TOFMS during ALD for Chemical Quality Control of Thin Films. The Journal of Physical Chemistry C 2022, 126 (4) , 1901-1912. https://doi.org/10.1021/acs.jpcc.1c09544
    3. Agnieszka Priebe, Jordi Sastre, Moritz H. Futscher, Jakub Jurczyk, Marcos V. Puydinger dos Santos, Yaroslav E. Romanyuk, Johann Michler. Detection of Au+ Ions During Fluorine Gas-Assisted Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) for the Complete Elemental Characterization of Microbatteries. ACS Applied Materials & Interfaces 2021, 13 (34) , 41262-41274. https://doi.org/10.1021/acsami.1c10352
    4. Agnieszka Priebe, Emese Huszar, Marek Nowicki, Laszlo Pethö, Johann Michler. Mechanisms of Fluorine-Induced Separation of Mass Interference during TOF-SIMS Analysis. Analytical Chemistry 2021, 93 (29) , 10261-10271. https://doi.org/10.1021/acs.analchem.1c01661
    5. Dmitriy S. Verkhoturov, Bruno P. Crulhas, Michael J. Eller, Yong D. Han, Stanislav V. Verkhoturov, Yordanos Bisrat, Alexander Revzin, Emile A. Schweikert. Nanoprojectile Secondary Ion Mass Spectrometry for Analysis of Extracellular Vesicles. Analytical Chemistry 2021, 93 (20) , 7481-7490. https://doi.org/10.1021/acs.analchem.1c00689
    6. Agnieszka Priebe, Laszlo Pethö, Emese Huszar, Tianle Xie, Ivo Utke, Johann Michler. High Sensitivity of Fluorine Gas-Assisted FIB-TOF-SIMS for Chemical Characterization of Buried Sublayers in Thin Films. ACS Applied Materials & Interfaces 2021, 13 (13) , 15890-15900. https://doi.org/10.1021/acsami.1c01627
    7. Emese Huszar, Amit Sharma, Liza Szekely, Rejin Raghavan, Barbara Putz, Thomas E.J. Edwards, Ralph Spolenak, Johann Michler, Laszlo Petho. Synthesis and mechanical properties of co-deposited W nanoparticle and ZrCuAg metallic glass thin film composites. Thin Solid Films 2023, 357 , 139822. https://doi.org/10.1016/j.tsf.2023.139822
    8. Agnieszka Priebe, Johann Michler. Review of Recent Advances in Gas-Assisted Focused Ion Beam Time-of-Flight Secondary Ion Mass Spectrometry (FIB-TOF-SIMS). Materials 2023, 16 (5) , 2090. https://doi.org/10.3390/ma16052090
    9. Dongxian Li, Tao Zhang, Weisheng Yue, Ping Gao, Yunfei Luo, Changtao Wang, Xiangang Luo. Identification and classification of particle contaminants on photomasks based on individual-particle Raman scattering spectra and SEM images. RSC Advances 2022, 12 (51) , 33349-33357. https://doi.org/10.1039/D2RA05672K
    10. Till-Niklas Kröger, Patrick Harte, Sven Klein, Thomas Beuse, Markus Börner, Martin Winter, Sascha Nowak, Simon Wiemers-Meyer. Direct investigation of the interparticle-based state-of-charge distribution of polycrystalline NMC532 in lithium ion batteries by classification-single-particle-ICP-OES. Journal of Power Sources 2022, 527 , 231204. https://doi.org/10.1016/j.jpowsour.2022.231204
    11. Yu Zhang, Charlie Kong, Giuseppe Scardera, Malcolm Abbott, David N.R. Payne, Bram Hoex. Large volume tomography using plasma FIB-SEM: A comprehensive case study on black silicon. Ultramicroscopy 2022, 233 , 113458. https://doi.org/10.1016/j.ultramic.2021.113458
    12. Simon Carter, Robert Clough, Andy Fisher, Bridget Gibson, Ben Russell. Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials. Journal of Analytical Atomic Spectrometry 2021, 36 (11) , 2241-2305. https://doi.org/10.1039/D1JA90049H
    13. Agnieszka Priebe, Tianle Xie, Laszlo Pethö, Johann Michler. Potential of gas-assisted time-of-flight secondary ion mass spectrometry for improving the elemental characterization of complex metal-based systems. Journal of Analytical Atomic Spectrometry 2020, 35 (12) , 2997-3006. https://doi.org/10.1039/D0JA00372G
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