Magnetic Sector Secondary Ion Mass Spectrometry on FIB-SEM Instruments for Nanoscale Chemical Imaging.

The structural, morphological, and chemical characterization of samples is of utmost importance for a large number of scientific fields. Furthermore, this characterization very often needs to be performed in three dimensions and at length scales down to the nanometer. Therefore, there is a stringent necessity to develop appropriate instrumentational solutions to fulfill these needs. Here we report on the deployment of magnetic sector secondary ion mass spectrometry (SIMS) on a type of instrument widely used for such nanoscale investigations, namely, focused ion beam (FIB)-scanning electron microscopy (SEM) instruments. First, we present the layout of the FIB-SEM-SIMS instrument and address its performance by using specific test samples. The achieved performance can be summarized as follows: an overall secondary ion beam transmission above 40%, a mass resolving power (M/ΔM) of more than 400, a detectable mass range from 1 to 400 amu, a lateral resolution in two-dimensional (2D) chemical imaging mode of 15 nm, and a depth resolution of ∼4 nm at 3.0 keV of beam landing energy. Second, we show results (depth profiling, 2D imaging, three-dimensional imaging) obtained in a wide range of areas, such as battery research, photovoltaics, multilayered samples, and life science applications. We hereby highlight the system's versatile capability of conducting high-performance correlative studies in the fields of materials science and life sciences.

Initial experimental results on a magnetic beam separator spectrometer for the SEM.

This article describes preliminary experiments to test the concept of scanning electron microscope (SEM) using a round magnetic beam separator to perform energy spectroscopy. Two experiments with an add-on attachment inside a conventional SEM were performed, one to estimate the sector image aberrations and the other to capture an energy spectrum of scattered electrons. The experiments show that the sector image aberrations lie well below 2 nm and that it is possible to capture the energy spectrum of secondary electrons.

A second-order focusing electrostatic toroidal electron spectrometer with 2pi radian collection.

This paper presents a toroidal electron energy spectrometer designed to capture electrons in the full 2pi azimuthal angular direction while at the same time having second-order focusing optics. Simulation results based upon direct ray tracing predict that the relative energy resolution of the spectrometer will be 0.146% and 0.0188% at input angular spreads of +/- 6 degrees and +/- 3 degrees, respectively, comparable to the theoretically best resolution of the cylindrical mirror analyzer (CMA), and an order of magnitude better than existing toroidal spectrometers. Also predicted for the spectrometer is a parallel energy acquisition mode of operation, where the energy bandwidth is expected to be > +/- 10% (20% total) of the pass energy. The spectrometer is designed to allow for retardation of the pass energy without the need to incorporate auxiliary lenses.

Redesign of the scanning electron microscope for parallel energy spectral acquisition.

This paper presents a scanning electron microscope (SEM) design that is compatible with parallel electron energy spectrum acquisition. The SEM should in principle be capable of capturing the energy spectrum of all scattered electrons simultaneously, from low energy secondary electrons to elastic backscattered electrons. Preliminary simulation results predict that the beam separator spectrometer will have a relatively high transmission-energy resolution performance, comparable or better than the cylindrical mirror analyzer (CMA), while at the same time being able to capture the entire energy range of scattered electrons.