Secondary ion mass spectrometry (SIMS) is a well-known technique for 3D chemical mapping at the nanoscale, with detection sensitivity in the range of ppm or even ppb. Energy dispersive X-ray spectroscopy (EDS) is the standard chemical analysis and imaging technique in modern scanning electron microscopes (SEM), and related dual-beam focussed ion beam (FIBSEM) instruments. Contrary to the use of an electron beam, in the past the ion beam in FIBSEMs has predominantly been used for local milling or deposition of material. Here, we review the emerging FIBSIMS technique which exploits the focused ion beam as an analytical probe, providing the capability to perform secondary ion mass spectrometry measurements on FIBSEM instruments: secondary ions, sputtered by the FIB, are collected and selected according to their mass by a mass spectrometer. In this way a complete 3D chemical analysis with high lateral resolution < 50 rim and a depth resolution < 10 nm is attainable. We first report on the historical developments of both SIMS and FIB techniques and review recent developments in both instruments. We then review the physics of interaction for incident particles using Monte Carlo simulations. Next, the components of modern FIBSIMS instruments, from the primary ion generation in the liquid metal source in the FIB column, the focussing optics, the sputtered ion extraction optics, to the different mass spectrometer types are all detailed. The advantages and disadvantages of parallel and serial mass selection in terms of data acquisition and interpretation are highlighted, while the effects of pressure in the FIBSEM, acceleration voltage, ion take-off angles and charge compensation techniques on the analysis results are then discussed. The capabilities of FIBSIMS in terms of sensitivity, lateral and depth resolution and mass resolution are reviewed. Different data acquisition strategies related to dwell time, binning and beam control strategies as well as roughness and edge effects are discussed. Data analysis routines for mass identification based on isotope ratios and molecular fragments are outlined. Application examples are then presented for the fields of thin films, polycrystalline metals, batteries, cultural heritage materials, isotope labelling, and geological materials. Finally, FIBSIMS is compared to EDS, and the potential of the technique for correlative microscopy with other FIBSEM based imaging techniques is discussed.

In this chapter, the peculiarities of integrating micro-/nano-materials testing within a scanning electron microscope are addressed. The mostly popular techniques are described, including miniaturized tensile tests, compression tests, and nano-indentation tests. Then the subject of image analysis is addressed and, finally a case study combining the use of compressive and tensile testing methods is presented.

The authors have experimentally investigated the compressive strength of GaAs pillars with a diameter of 1μm by uniaxial compression tests. The tests were performed at room temperature and, contrary to macroscopic tests, the micropillars were found to exhibit ductile plasticity comparable to that of metal single crystal micropillars. The yield stress was 1.8±0.4GPa and, for one pillar that was more closely examined, a total deformation of 24% was observed. In the diffraction patterns from transmission electron microscopy studies of this pillar, a high density of twins was observed.