Review Article

FIB-SEM Three-Dimensional Tomography for Characterization of Carbon-Based Materials

Table 1

Short indicative selection of FIB-SEM for carbon-based materials from the literature.

MaterialApplicationMethodologyPurposeYearReference

Hybrid graphene on Ni foamElectrode of supercapacitorsDual Beam Strata 235 (FEI) and Auriga Compact (Zeiss) microscopeTo analyze the morphologies and structural features of the composites2019[31]
Nanoporous gold-nitrogen-doped carbon nano-onionsElectrode of micro-supercapacitorFIB-FEG-SEM of Carl Zeiss Auriga Compact-4558To determine the thickness of the different layers present in the electrode2019[32]
Graphite fluoride-lithiumLithium batteryFIB-SEM, Scios, FEITo confirm the fine structure of GF-LiF-Li composite2019[33]
Carbon nanofiberSupercapacitorAuriga Cross Beam, Zeiss
Software: Avizo 9.0.0
To examine fiber subsurface microstructure2018[34]
CoalFuelFEI Helios Nanolab 650 FIB-SEM systemTo quantitative evaluate the 3D characterization of pore-fracture networks of coals2017[35]
Conductive carbon black/carbon fiber coating2,6-Naph(COOLi)2 electrodesFIB: 50 nA current and 7 kV acceleration voltage
SEM: operating at 2 kW.
To investigate the nanocarbon coating and the uniformness of pore structures2016[36]
Nanoporous carbon-binderLi-ion batteriesZeiss Auriga 60 dual beam: 20 pA current, 30 kV acceleration voltage, and 9 nm cutting distance
SEM: 5 kV, pixel size of 3 nm
To reconstruct the carbon-binder domain of a LiCoO2 battery cathode2015[37]
Carbon nanotubes (CNTs) in polymer compositesNanotechnologyFEI Helios Nanolab 600 FIB-SEM systemTo investigate the subsurface imaging of CNTs2015[38]
Porous carbon-based electrodeElectrodeFIB: 80 pA current and 30 kV acceleration voltage
SEM: 3 kV voltage
The voxel size was 10 × 10 × 10 nm3
Software: IMOD, ImageJ, and AVIZO software
To analyze the morphologies and build topographic reconstruction of the porous carbon electrode2014[39]
Deposition of porous iron oxide on activated carbon (AC)AdsorbentFIB: 10–1 nA current and 30 kV acceleration voltage
SEM: 2–5 kV voltage
To understand the nature of iron oxide particles within the pores of AC2014[40]
Hierarchical nanoporous carbon synthesized using a hard template methodElectrodeDual-beam workstation FEI Helios Nanolab 600; a field emission gun SEMTo observe the open 3D porous structure of the carbon2013[41]
Nanoporous carbon-supported noble metal catalyst layersFuel cellsFIB: 50 pA current and 30 kV acceleration voltage
SEM: 2 kV voltage
To characterize porosity, connectivity, and pore-size and grain-size distribution2013[42]
Disordered mesoporous carbon with tailored pore sizeFuel cells supercapacitorsFIB: 27 pA current and 30 kV acceleration voltage
SEM: 86 pA current and 5 kV voltage
The voxel size was 3.57 × 3.62 × 10 nm3
Software: Amira® 5.2 software and MAVI
To visualize and study nonordered pore morphology and quantitatively characterize their physical properties2013[30]