Tof sims 5 instrument

Time of flight secondary ion mass spectrometry
(ToF-SIMS) was performed using a ToF–SIMS 5 instrument (ION-TOF,
Münster, Germany). A Bi₃⁺ cluster ion
beam with a kinetic energy of 30 keV was used as an analytical beam.

ToF-SIMS analysis was performed using a TOF.SIMS 5 instrument (ION-TOF GmbH, Münster, Germany). The instrument is equipped with a 25 keV Bi₃⁺ cluster ion gun as the primary ion source and a 10 keV C₆₀⁺ ion source for sputtering and etching. The samples were analyzed using a pulsed primary ion beam (Bi₃⁺⁺, 0.34 pA at 50 keV) with a focus of approximately 2 μm at a field of view of 150 µm × 150 µm. The mass resolution using this setup was at least M/ΔM = 5000 full width at half maximum at m/z 500. All spectra were acquired and processed with the Surface Lab software (version 6.4, ION-TOF GmbH). Depth profile analysis was performed using a C₆₀⁺⁺ beam at 20 keV with a current of 0.2 nA in a non-interlaced mode with 1 s of analysis, 1 s of sputtering, and a pause of 1 s for each sputter cycle at 350 µm × 350 µm. The maximum ion dose density of Bi₃⁺⁺ was kept between 4 × 10¹² and 7 × 10¹² cm⁻² over the whole depth profiling experiment, while the ion dose for C₆₀⁺⁺ ranged from 2 × 10¹⁴ to 4 × 10¹⁴ ions per cm². Low-energy electrons were used for charge compensation during analysis.

ToF-SIMS was performed on a TOF.SIMS5 instrument (ION-TOF GmbH, Münster, Germany) equipped with a Bi cluster primary ion source and a reflectron type time-of-flight analyzer. UHV base pressure was <5 × 10⁻⁹ mbar. For high mass resolution the Bi source was operated in the “high current bunched” mode providing short Bi₃⁺ primary ion pulses at 25 keV energy, a lateral resolution of ~4 μm, and a target current of 0.2 pA at 5 kHz repetition rate. The short pulse length of 0.9 ns allowed for high mass resolution. For depth profiling a dual beam analysis was performed in full interlaced mode: The primary ion source was scanned area of 300 × 300 µm² (128 × 128 data points) and a sputter gun operated with Ar₁₆₅₀⁺ cluster ions, 5 keV, scanned over a concentric field of 500 × 500 µm², (target current 3 nA) was applied to erode the sample. Thereby, the sputter ion dose density was >5000 times higher than the Bi ion dose density. Spectra were calibrated on the omnipresent C⁻, C₂⁻, C₃⁻, or on the C⁺, CH⁺, CH₂⁺, and CH₃⁺ peaks. Based on these datasets the chemical assignments for characteristic fragments were determined. For data visualization, secondary ion intensities were normalized to a maximum of 1.0, each, and plotted over sputter ion fluence [ions/cm²] as an indirect measure for erosion depth.

SEM with a field emission gun (Schottky‐type) was performed to investigate the surface of the electrodes and the particle size and architecture. The measurements were carried out on multiple areas of the sample using an Auriga CrossBeam workstation from Zeiss (Germany). Cross‐sections were prepared by means of FIB milling using gallium ions generated from a liquid metal ion source. EDX was conducted to examine the elemental composition of the surface and cross‐section on multiple areas of the sample. The measurements were performed with an accelerating voltage of 15 kV using an Ultim® Extreme EDX detector and evaluated with the INCA software, both from Oxford Instruments (United Kingdom). ToF‐SIMS was performed using a TOF.SIMS 5 instrument from ION TOF GmbH (Germany). The nanoscale elemental mapping of the cross‐section was carried out with a liquid metal bismuth ion source (Bi⁺ 30 keV) in the imaging mode combined with delayed secondary ion extraction. The positive electrodes were analyzed by SEM, EDX, and ToF‐SIMS after washing with 1 mL EMC.

TOF-SIMS analysis was performed with a TOF.SIMS 5 instrument (ION-TOF GmbH, Münster, Germany) equipped with a 30 keV liquid metal ion gun. Bi₃⁺ ion clusters were applied as the primary beam, and a low energy electron flood gun was used for charge compensation. For all measurements, the ion dose was kept below 10¹² ion/cm² to ensure static mode conditions, and a 0.5 pA current was applied. High mass resolution TOF-SIMS spectra and maps of positive ions were recorded from ten non-overlapping 100 μm × 100 μm areas of each sample with resolution of 128 × 128 points. Spectra mass calibration was performed based on peaks of H⁺, H₂⁺, CH⁺, C₂H₂⁺ and C₄H₅⁺. The mass resolution (m/Δm) was above 8000 at C₄H₅⁺ for all measurements.

A PalmSens2
potentiostat/galvanostat (Palm
Instruments BV, The Netherlands), controlled by PSTrace v.5.6 software,
was used for voltammetric measurements. The experimental setup also
includes a precise (1 rpm resolution) manually controlled stirrer
(Heidolph Schwabach, Germany) in the 0–2000 rpm range and a
Teflon-made customized cell for SPEs, model CFLWCL-CONIC, from Methrom-DropSens
(Oviedo, Spain). The capacity of this novel cell is up to 2.0 mL sample
solution for batch analysis, allowing convenient overhead stirring
and spiking of the solution to perform standard addition methods.
Methrom-DropSens provided disposable LT-SPGEs (ref. 220BT), consisting
of a working electrode (sputtered thin gold film of 4 mm diameter),
a counter electrode (same material as the working electrode), and
a silver pseudoreference electrode, printed on a ceramic surface.
The electrodes were firmly connected to the potentiostat through a
hand-modified crocodile-connector wire, in replacement of the original
sliding connector that we have observed to be very prone to unexpected
disconnections (Figure 1). For surface morphology characterization, we used a scanning electron
microscope FE-SEM Quanta 3D FEG (FEI Company, Oregon, EE.UU.). Qualitative
microanalysis of Au–Hg amalgam by time-of-flight secondary
ion mass spectrometry (TOF-SIMS) was carried out using a TOF-SIMS⁵ instrument (IONTOF, Munster, Germany).