4.8 Article

Detection of Au+ Ions During Fluorine Gas-Assisted Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) for the Complete Elemental Characterization of Microbatteries

Journal

ACS APPLIED MATERIALS & INTERFACES
Volume 13, Issue 34, Pages 41262-41274

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/acsami.1c10352

Keywords

elemental characterization; mass spectrometry; ions; fluorine gas; Au; Li-ion batteries; microdevices

Funding

  1. Swiss Commission for Technology and Innovation (CTI) project [25592.1PFNM-NM]
  2. Swiss National Science Foundation [200021_172764]
  3. EU Horizon 2020 Marie Curie-Sklodowska Innovative Training Network ELENA [722149]
  4. Strategic Focus Area (SFA) Advanced Manufacturing of the ETH Domain (project X-ray Diagnostics)
  5. Swiss National Science Foundation (SNF) [200021_172764] Funding Source: Swiss National Science Foundation (SNF)
  6. Marie Curie Actions (MSCA) [722149] Funding Source: Marie Curie Actions (MSCA)

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Gold is commonly used in new microdevices for energy applications, microelectronics, and biomedical solutions due to its excellent electric conductivity and chemical inertness. Fluorine gas coinjection has been found to alter the polarity of gold secondary ions, aiding in the understanding of operation mechanisms and potential degradation processes in microdevices.
Due to excellent electric conductivity and chemical inertness, Au can be used in new microdevices for energy applications, microelectronics, and biomedical solutions. However, the chemical analysis of Au-containing systems using time-of-flight secondary ion mass spectrometry (TOF-SIMS) can be difficult because of the negative ionization of Au, as most metals form positive ions, and therefore cannot be detected from the same analytical volume. In this work, we present the potential of fluorine gas coinjection for altering the polarity, from the negative to positive, of Au secondary ions generated under Ga+ beam bombardment. The importance of detecting Au+ ions and representing their spatial distribution in nanoscale was demonstrated using a novel solid electrolyte for Li-ion solid-state batteries, amorphous Li7La3Zr2O12 (aLLZO). This allowed for assessing the migration of mobile Li+ ions outside the aLLZO layer and alloying the Au layer with Li, which explained the presence of an internal electric field observed during the polarization measurements. Remarkably, during fluorine gas-assisted TOF-SIMS measurements, the trace amount of Au content (5 ppm) was detected in a Pt layer (unattainable under standard vacuum conditions). In conclusion, fluorine gas-assisted TOF-SIMS can help understanding operation mechanisms and potential degradation processes of microdevices and therefore help optimizing their functionality.

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