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A Macroscopically Relevant 3D‐Metrology Approach for Nanocatalysis Research
Author(s) -
LópezHaro Miguel,
Tinoco Miguel,
FernándezGarcia Susana,
Chen Xiaowei,
Hungria Ana Belén,
Cauqui Miguel Ángel,
Calvino José Juan
Publication year - 2018
Publication title -
particle and particle systems characterization
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.877
H-Index - 56
eISSN - 1521-4117
pISSN - 0934-0866
DOI - 10.1002/ppsc.201700343
Subject(s) - metrology , nanometrology , characterization (materials science) , materials science , electron tomography , nanoscopic scale , tomography , nanotechnology , segmentation , scanning transmission electron microscopy , nanomaterial based catalyst , computer science , biological system , optics , nanoparticle , artificial intelligence , transmission electron microscopy , atomic force microscopy , physics , biology
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 CeO 2 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.