Large volume serial section tomography by Xe Plasma FIB dual beam microscopy

Ga⁺ Focused Ion Beam-Scanning Electron Microscopes (FIB-SEM) have revolutionised the level of microstructural information that can be recovered in 3D by block face serial section tomography (SST), as well as enabling the site-specific removal of smaller regions for subsequent transmission electron microscope (TEM) examination. However, Ga⁺ FIB material removal rates limit the volumes and depths that can be probed to dimensions in the tens of microns range. Emerging Xe⁺ Plasma Focused Ion Beam-Scanning Electron Microscope (PFIB-SEM) systems promise faster removal rates. Here we examine the potential of the method for large volume serial section tomography as applied to bainitic steel and WC–Co hard metals. Our studies demonstrate that with careful control of milling parameters precise automated serial sectioning can be achieved with low levels of milling artefacts at removal rates some 60× faster. Volumes that are hundreds of microns in dimension have been collected using fully automated SST routines in feasible timescales (<24 h) showing good grain orientation contrast and capturing microstructural features at the tens of nanometres to the tens of microns scale. Accompanying electron back scattered diffraction (EBSD) maps show high indexing rates suggesting low levels of surface damage. Further, under high current Ga⁺ FIB milling WC–Co is prone to amorphisation of WC surface layers and phase transformation of the Co phase, neither of which have been observed at PFIB currents as high as 60 nA at 30 kV. Xe⁺ PFIB dual beam microscopes promise to radically extend our capability for 3D tomography, 3D EDX, 3D EBSD as well as correlative tomography. - Highlights: • The uptake of dual beam FIBs has been rapid but long milling times have limited imaged volumes to tens of micron dimensions. • Emerging plasma Xe⁺ PFIB-SEM technology offers materials removal rates at least 60× greater than conventional Ga⁺ FIB systems with comparable or less damage. • The PFIB-SEM can provide a critical link between non-destructive X-ray imaging and destructive serial sectioning within a correlative tomography framework.