3D
characterization of assemblies of nanoparticles is of great
importance to determine their structure–property connection.
Such investigations become increasingly more challenging when the
assemblies become larger and more compact. In this paper, we propose
an optimized approach for electron tomography to minimize artifacts
related to beam broadening in high angle annular dark-field scanning
transmission electron microscopy mode. These artifacts are typically
present at one side of the reconstructed 3D data set for thick nanoparticle
assemblies. To overcome this problem, we propose a procedure in which
two tomographic tilt series of the same sample are acquired. After
acquiring the first series, the sample is flipped over 180°,
and a second tilt series is acquired. By merging the two reconstructions,
blurring in the reconstructed volume is minimized. Next, this approach
is combined with an advanced three-dimensional reconstruction algorithm
yielding quantitative structural information. Here, the approach is
applied to a thick and compact assembly of spherical Au nanoparticles,
but the methodology can we used to investigate a broad range of samples.