Large volume 'chunk' lift out for 3D tomographic analysis using analytical plasma focussed ion beam -- scanning electron microscopy

TL;DR

This paper presents a method for large volume 3D material characterization using plasma FIB-SEM with EBSD, enabling detailed analysis of microstructures in substantial volumes for materials science.

Contribution

It introduces a workflow for site-specific large volume lift out and serial sectioning optimized for 3D EBSD analysis using plasma FIB-SEM, including a step-by-step guide.

Findings

Successful 3D EBSD analysis of a magnesium polycrystal

Workflow applicable to various materials for 3D microstructure characterization

Demonstrated large volume lift out technique for detailed structural analysis

Abstract

Characterization of the structure and properties of materials in three dimensions, including grains and the residual pattern of deformation, provides necessary information required to guide materials design as well as support materials modelling efforts. In this work, we present an overview of site-specific large volume 'chunk' lift out and 3D serial sectioning of substantive volumes (e.g. 200 x 200 x 400 um3), where sectioning is optimized for 3D electron backscatter diffraction (EBSD) based crystallographic analysis, using a plasma (Xe) focussed ion beam scanning electron microscope (plasma FIB-SEM) equipped to perform EBSD using a 'static' configuration (i.e. slicing and EBSD-mapping are performed without moving the sample). This workflow is demonstrated through the 3D plasma FIB-SEM based EBSD analysis of an indent made within a polycrystal of pure magnesium. The lift out approach is suitable for a wide range of materials, and we offer a step-by-step guide within the present work to provide opportunity for others to more easily enter this field and collect valuable data.