Herein, we employ
a serial sectioning technique on a dual beam FIB followed
by 3D volume reconstruction for comprehensive analysis of
tubular metal nanostructures encapsulated within porous anodic alumina. Using this technique, we demonstrate a
nano-tomography characterisation protocol that can be used
for analysis of nanoporous structures with emphasis on
their channel uniformity and orientation. We demonstrate
that high-resolution nano-tomography can be performed to
visualise pores as small as 60 nm in diameter, with conical
or globular shapes, and to quantitatively estimate their localisation and distribution along one-dimensional metal
structures. We specifically chose to examine Cu-nanotubes,
deposited electrochemically within anodic alumina template,
because there is a great deal of debate regarding the deposition
process. Hence, the comprehensive analysis shown here is
not only demonstrating the applicability of the developed
characterisation methodology but it is also, in conjunction
with other advanced electron microscopy methods such
as elemental nano-scale STEM/EDX mapping, providing
conclusive evidence of the key factors at play during the
deposition process.