Potential of gas-assisted time-of-flight secondary ion mass spectrometry for improving the elemental characterization of complex metal-based systems

Abstract

Enhancing the spatial resolution of Time-Of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS), which provides 3D elemental distribution in combination with high sensitivity and molecular information, is currently one of the hottest...

Mechanisms of Fluorine-Induced Separation of Mass Interference during TOF-SIMS Analysis

“…Interestingly, the shape of 90 Zr + secondary ion distribution can potentially indicate the exact quantitative relation between Zr-containing layers, i.e., 100% Zr content in Zr layer and 50% Zr in ZrMo and ZrAg. However, most likely, this is just a coincidence as the ionization efficiency strongly depends on the matrix, 29,34 and this tendency is observed for neither the Mo + -nor Ag + -ion signals. As mentioned, the increase of signals at m/q = 91 and 95 measured close to the Zr−Si interface probably results from the contribution of Si-containing ions (such as 28 Si 2 19 F 16 O + and 28 Si 2 19 F 2 1 H + , respectively).…”

“…The analytical chamber was equipped with a five-line gas injection system (GIS) allowing for supplementary gas-assisted TOF-SIMS measurements. In contrast to the previously used ,, compact TOF (CTOF), the HTOF detector is located much closer to a sample surface, which implies different ion extraction optics. Consequently, the nominal GIS working position, which is used for standard GIS application (such as increasing sputtering rates, depositing protective layers, and preparing samples for X-ray computed nanotomography or transmission electron microscopy), was not appropriate for gas-assisted TOF-SIMS measurements due to the induced modifications of ion extraction field lines and insufficient secondary ion collection.…”

“…This technology advance, ensuring simultaneous delivery of supplementary gas during FIB-TOF-SIMS measurements, was recently reported as a promising solution for modifying sample surface chemical state under HV. Particularly remarkable results have been achieved in the case of using fluorine gas, which showed great potential for increasing ionization efficiency, ,, and therefore improving the resolution of chemical images, separating mass interference and altering the polarity, from negative to positive, of generated secondary ions. To the best of our knowledge, such beneficial features were not observed for any other gases.…”

Blocking Lithium Dendrite Growth in Solid-State Batteries with an Ultrathin Amorphous Li-La-Zr-O Solid Electrolyte

“…The 3D tomogram in Figure 1.c shows the elemental structure of the film reconstructed from a gas-assisted focused ion beam time-of-flight secondary ion mass spectroscopy (FIB-ToF-SIMS) measurement. 18 The measurement reveals a uniform distribution of the matrix elements of the aLLZO film over the Pt-coated Si substrate. Detailed plots of each element's signal and a depth profile can be found in Figures S1 and S2.…”

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

“…46,51 Furthermore, in some cases, the depth profiles obtained in the presence of fluorine gas has seemed to be less sensitive to the sample's boundary conditions (i.e., surface oxidation and proximity to a substrate), showing more representative data with respect to the sample composition. 47 The beneficial use of fluorine-gas assisted TOF-SIMS (when compared to the results obtained without any gas) was demonstrated in the case of pure metals, 45,49 alloys, 47,49 and complex multilayers. 46,48,50,51 In this work, we demonstrate that, along with the aforementioned advantages, fluorine gas can alter the polarity, from negative to positive, of secondary ions generated during Ga + primary ion beam bombardment.…”