title: Large volume serial section tomography by Xe Plasma FIB dual beam microscopy.
abstract: 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 (<24h) 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 60nA at 30kV. Xe(+) PFIB dual beam microscopes promise to radically extend our capability for 3D tomography, 3D EDX, 3D EBSD as well as correlative tomography.
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK; FEI Company, Achtseweg Noord 5, Bldg, 5651 GG, Eindhoven, The Netherlands.
authors.forename: T L
authors.initials: TL
authors.lastname: Burnett
authors.affiliation: FEI Company, 5350 NE Dawson Creek Drive, Hillsboro, OR 97124, United States.
authors.forename: R
authors.initials: R
authors.lastname: Kelley
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK; FEI Company, Achtseweg Noord 5, Bldg, 5651 GG, Eindhoven, The Netherlands.
authors.forename: B
authors.initials: B
authors.lastname: Winiarski
authors.affiliation: FEI Company, 5350 NE Dawson Creek Drive, Hillsboro, OR 97124, United States.
authors.forename: L
authors.initials: L
authors.lastname: Contreras
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK.
authors.forename: M
authors.initials: M
authors.lastname: Daly
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK.
authors.forename: A
authors.initials: A
authors.lastname: Gholinia
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK.
authors.forename: M G
authors.initials: MG
authors.lastname: Burke
authors.affiliation: School of Materials, University of Manchester, Manchester M13 9PL, UK; BP International Centre for Advanced Materials, University of Manchester, Manchester M13 9PL, UK. Electronic address: P.J.Withers@manchester.ac.uk.
authors.forename: P J
authors.initials: PJ
authors.lastname: Withers
keywords: 3D imaging; A508 grade 3 steel; Scanning electron microscopy; X-ray micro-tomography (micro-CT); Xe(+) Plasma FIB-SEM dual beam microscope