Aggregated nanoparticles: Sample preparation and analysis by atom probe tomography

•New procedure to prepare suitable APT sample from aggregate of nanoparticles.•Presence of hidden pores within the tip volume leading to trajectory aberrations.•Nanoparticles can be distinguished in the 3D reconstruction.•APT can be used as compositional quality control experiments. Atom probe tomography (APT) allows measurement of the three-dimensional structure and composition of materials, but specific sample preparation procedures are required for challenging materials such as aggregates of nanoparticles. Indeed, the presence of porosity within the specimen affects both the stability of the sample and the accuracy of the data. Here, aggregates of nanoparticles were transferred onto a micromanipulator tip and embedded via electron-beam-assisted deposition of Pt. Successive FIB-millings and Pt-depositions are needed to create suitable APT tips. The 3D reconstruction reveals the presence of 15–20 nm nanoparticles, and mass-spectral analysis shows the absence of trace elements within the catalyst, thus serving as quality control for the synthesis of nanoparticles with specific compositions. [Display omitted]