Leica em vct500 shuttle

Top-view images of pristine and cycled pellets were obtained by a Merlin high-resolution scanning electron microscope (Carl Zeiss AG, Germany) at an acceleration voltage of 5 kV. Energy-dispersive X-ray (EDX) spectroscopy of the cross-sectional view of the cell was carried out using an XMAX EXTREME EDX detector (Oxford Instruments, U.K.) at an acceleration voltage of 7 kV. The samples were transferred with a Leica EM VCT500 shuttle (Leica Microsystems GmbH).

To avoid exposure to the ambient environment, the sample transfer process from the glovebox to the SIMS instrument was conducted with a Leica EM VCT500 shuttle (Leica Microsystems GmbH) under the exclusion of air. ToF-SIMS characterizations were carried out with a Hybrid SIMS M6 system (IONTOF GmbH, Münster, Germany). All measurements were conducted in negative ion mode, and Bi₃⁺⁺ ions (60 keV) were applied as primary ion species. To compare the difference in the mass spectra, the spectrometry mode (bunched mode) of the Bi-gun with a beam aperture of 1,100 μm was chosen to analyze the surface of pellets, which enables a high mass resolution (FWHM m/Δm > 6000 @ m/z = 31.97 (S⁻)). For charge compensation, the sample was flooded with low energetic electrons and argon at the main chamber pressure of 5 × 10⁻⁶ mbar. The analysis area was set to 150 × 150 μm² and was rasterized with 256 × 256 pixels. The cycle time was 100 μs. The measurements were stopped at a primary ion dose of 10¹² ions/cm². In all, 10 mass spectra were collected in different regions on the surface of each pellet to make the results reproducible and reliable. For the measurement and data evaluation, the Surface Lab 7.1 software (IONTOF GmbH, Münster, Germany) was used.