RT Journal Article T1 A Macroscopically Relevant 3D-Metrology Approach for Nanocatalysis Research A1 López Haro, Miguel A1 Tinoco Rivas, Miguel A1 Fernández García, Susana A1 Chen, Xiaowei A1 Hungría, Ana Belén A1 Cauqui, Miguel Ángel A1 Calvino, José Juan AB A 3D nanometrological approach, which considers as an unbiased validation criterion the quantitative match between values of properties determined by macroscopic characterization techniques and those determined from the nanoscopic results, is developed to unveil the details of complex nanocatalysts. This approach takes into account both the peculiar characteristics of this type of materials and the large influence of noise in the tilt series. It combines, in an optimized way, the latest experimental developments in high angle annular dark field scanning transmission electron microscopy mode (HAADF-STEM) tomography, such as batch tomography, image denoising by undecimated wavelet transforms, improved reconstructions by total variation minimization and a more efficient, user-independent, segmentation scheme. To illustrate the use of this novel approach, the 3D structural characterization of a model nanocatalyst comprising gold nanoparticles dispersed on the surface of CeO2 nanocubes is performed, and the obtained results used to compute the values of different macroscopic chemical and textural properties. Comparison with values obtained by macroscopic characterization techniques match very closely those obtained by 3D nanometrology. Importantly, the new approach described in this work also illustrates a pipeline for nearly fully automated HAADF-STEM tomography studies, guaranteeing reliable correlations between nanoscopic and macroscopic properties. SN 0934-0866 YR 2018 FD 2018 LK https://hdl.handle.net/20.500.14352/98019 UL https://hdl.handle.net/20.500.14352/98019 LA eng NO López‐Haro, Miguel, et al. «A Macroscopically Relevant 3D‐Metrology Approach for Nanocatalysis Research». Particle & Particle Systems Characterization, vol. 35, n.o 3, marzo de 2018, p. 1700343. https://doi.org/10.1002/ppsc.201700343. NO Ministerio de Economía y Competitividad (España) NO Ministerio de Ciencia e Innovación (España) DS Docta Complutense RD 8 abr 2025