Correlative Laboratory Nano-CT and 360° Electron Tomography of Macropore Structures in Hierarchical Zeolites

Apeleo Zubiri B, Wirth J, Drobek D, Englisch S, Przybilla T, Weissenberger T, Schwieger W, Spiecker E (2020)

Publication Type: Journal article

Publication year: 2020

Journal

Advanced Materials Interfaces WILEY-VCH Verlag GmbH & Co. KGaA

DOI: 10.1002/admi.202001154

Abstract

Hierarchical pore structures exhibit morphological features on several length scales, which govern important materials properties in catalysis, such as catalytic activity, diffusivity or selectivity. Correlative tomography offers unique opportunities for a comprehensive and scale-bridging 3D characterization of such complex pore morphologies, which is crucial to further optimize materials design and synthesis routines. This study explores the capabilities of correlative 360° electron tomography (ET) and lab-based nano X-ray computed tomography (Nano-CT) enabling 3D analyses of volumes of up to (60 µm)³ with down to nm resolution, as demonstrated for zeolite particles with embedded macropores. By first applying the two techniques to the same particle the higher resolution and fidelity of ET are used to improve the segmentation of pore space in the Nano-CT reconstruction. Extended statistical relevance and access to interparticle pore space are obtained from reconstructions of larger particle agglomerates, using the large-field-of-view mode of the Nano-CT. The presented correlative approach enables real space analyses of important pore characteristics for comparison with complementary pore characterization techniques. Moreover, by investigating samples from different stages of the synthesis, 360°-ET and Nano-CT provide unique insights into the formation mechanism of porous materials, as demonstrated for the steam-assisted crystallization of the macroporous zeolite particles.

Authors with CRIS profile

Benjamin Apeleo Zubiri Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung) Janis Wirth Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung) Dominik Drobek Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung) Silvan Englisch Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung) Thomas Przybilla Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung) Tobias Weissenberger Lehrstuhl für Chemische Reaktionstechnik (CRT) Wilhelm Schwieger Professur für Technische Chemie (Reaktionstechnik) Erdmann Spiecker Lehrstuhl für Werkstoffwissenschaften (Mikro- und Nanostrukturforschung)

Additional Organisation(s)

Interdisziplinäres Zentrum, Center for Nanoanalysis and Electron Microscopy (CENEM) Graduiertenkolleg 1896/2 In situ Mikroskopie mit Elektronen, Röntgenstrahlen und Rastersonden

Related research project(s)

Microscopic 3D characterisation of functional particles and pore structures (SFB 1411 - C01) Design of particulate products (SFB 1411) Jan. 1, 2020 - Dec. 31, 2023 In-situ Characterization of Nanomaterials with Electrons, X-rays/Neutrons and Scanning Probes (GRK 1896) Oct. 1, 2013 - Sept. 30, 2022

How to cite

APA:

Apeleo Zubiri, B., Wirth, J., Drobek, D., Englisch, S., Przybilla, T., Weissenberger, T.,... Spiecker, E. (2020). Correlative Laboratory Nano-CT and 360° Electron Tomography of Macropore Structures in Hierarchical Zeolites. Advanced Materials Interfaces. https://doi.org/10.1002/admi.202001154

MLA:

Apeleo Zubiri, Benjamin, et al. "Correlative Laboratory Nano-CT and 360° Electron Tomography of Macropore Structures in Hierarchical Zeolites." Advanced Materials Interfaces (2020).

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