Direct quantitative investigation of the inner morphology and structure of materials is of critical importance to provide profound insights for properties evaluation. The scanning electron microscope (SEM) and focused ion beam (FIB), combined known as FIB-SEM or DualBeam, are conventionally recognized as a highly effective method to acquire 3D volume information of soft materials samples. FIB-SEM together with integrated Automated Slice and View software has made the automated 3D data acquisition and analysis possible. However, slicing using Ga ion beam at room temperature has been found inducing severe damage to the beam sensitive materials, resulting in significant deterioration of the 3D data quality. Cutting edge cryo multi-ion source plasma FIB (PFIB) technique provides a fully automated workflow which allows large volume, damage-free ion beam slicing and high spatial resolution SEM acquisition during serial sectioning using various types of plasma ion beams under cryogenic conditions. With automated 3D reconstruction of the micrograph stacks, we can subsequently recover the comprehensive volume information of such beam sensitive materials.

In this paper we present a series of large volume 3D imaging results of extremely beam sensitive polymer samples. The samples were sliced using oxygen plasma ion source on Thermo Scientific Helios Hydra Plasma FIB platform under cryogenic conditions. The slicing and imaging acquisition was achieved using Automated Slice and View software and the subsequent data processing was conducted using Avizo 3D analysis and visualization software. The unique technical experiment set up and comprehensive application experience will be discussed in this presentation.