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Evolution of Hierarchically Porous Nickel Alumina Catalysts Studied by X-Ray Ptychography

Weber, Sebastian ; Diaz, Ana ; Holler, Mirko ; Schropp, Andreas ; Lyubomirskiy, Mikhail ; Abel, Ken L. ; Kahnt, Maik LU orcid ; Jeromin, Arno ; Kulkarni, Satishkumar and Keller, Thomas F. , et al. (2022) In Advanced science (Weinheim, Baden-Wurttemberg, Germany) 9(8). p.2105432-2105432
Abstract

The synthesis of hierarchically porous materials usually requires complex experimental procedures, often based around extensive trial and error approaches. One common synthesis strategy is the sol-gel method, although the relation between synthesis parameters, material structure and function has not been widely explored. Here, in situ 2D hard X-ray ptychography (XRP) and 3D ptychographic X-ray computed tomography (PXCT) are applied to monitor the development of hierarchical porosity in Ni/Al2 O3 and Al2 O3 catalysts with connected meso- and macropore networks. In situ XRP allows to follow textural changes of a dried gel Ni/Al2 O3 sample as a function of temperature during calcination, activation and CO2 methanation reaction.... (More)

The synthesis of hierarchically porous materials usually requires complex experimental procedures, often based around extensive trial and error approaches. One common synthesis strategy is the sol-gel method, although the relation between synthesis parameters, material structure and function has not been widely explored. Here, in situ 2D hard X-ray ptychography (XRP) and 3D ptychographic X-ray computed tomography (PXCT) are applied to monitor the development of hierarchical porosity in Ni/Al2 O3 and Al2 O3 catalysts with connected meso- and macropore networks. In situ XRP allows to follow textural changes of a dried gel Ni/Al2 O3 sample as a function of temperature during calcination, activation and CO2 methanation reaction. Complementary PXCT studies on dried gel particles of Ni/Al2 O3 and Al2 O3 provide quantitative information on pore structure, size distribution, and shape with 3D spatial resolution approaching 50 nm, while identical particles are imaged ex situ before and after calcination. The X-ray imaging results are correlated with N2 -sorption, Hg porosimetry and He pycnometry pore characterization. Hard X-ray nanotomography is highlighted to derive fine structural details including tortuosity, branching nodes, and closed pores, which are relevant in understanding transport phenomena during chemical reactions. XRP and PXCT are enabling technologies to understand complex synthesis pathways of porous materials.

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organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
heterogeneous catalysis, hierarchical porosity, imaging, pore characterization, sol-gel method, X-ray ptychography, X-ray tomography
in
Advanced science (Weinheim, Baden-Wurttemberg, Germany)
volume
9
issue
8
pages
2105432 - 2105432
publisher
John Wiley & Sons Inc.
external identifiers
  • pmid:35289133
  • scopus:85126681870
ISSN
2198-3844
DOI
10.1002/advs.202105432
language
English
LU publication?
yes
additional info
Publisher Copyright: © 2022 The Authors. Advanced Science published by Wiley-VCH GmbH.
id
cd4709fd-013b-416a-a06e-4a685b73e1e6
date added to LUP
2022-04-03 12:35:57
date last changed
2025-03-09 10:57:02
@article{cd4709fd-013b-416a-a06e-4a685b73e1e6,
  abstract     = {{<p>The synthesis of hierarchically porous materials usually requires complex experimental procedures, often based around extensive trial and error approaches. One common synthesis strategy is the sol-gel method, although the relation between synthesis parameters, material structure and function has not been widely explored. Here, in situ 2D hard X-ray ptychography (XRP) and 3D ptychographic X-ray computed tomography (PXCT) are applied to monitor the development of hierarchical porosity in Ni/Al2 O3 and Al2 O3 catalysts with connected meso- and macropore networks. In situ XRP allows to follow textural changes of a dried gel Ni/Al2 O3 sample as a function of temperature during calcination, activation and CO2 methanation reaction. Complementary PXCT studies on dried gel particles of Ni/Al2 O3 and Al2 O3 provide quantitative information on pore structure, size distribution, and shape with 3D spatial resolution approaching 50 nm, while identical particles are imaged ex situ before and after calcination. The X-ray imaging results are correlated with N2 -sorption, Hg porosimetry and He pycnometry pore characterization. Hard X-ray nanotomography is highlighted to derive fine structural details including tortuosity, branching nodes, and closed pores, which are relevant in understanding transport phenomena during chemical reactions. XRP and PXCT are enabling technologies to understand complex synthesis pathways of porous materials.</p>}},
  author       = {{Weber, Sebastian and Diaz, Ana and Holler, Mirko and Schropp, Andreas and Lyubomirskiy, Mikhail and Abel, Ken L. and Kahnt, Maik and Jeromin, Arno and Kulkarni, Satishkumar and Keller, Thomas F. and Gläser, Roger and Sheppard, Thomas L.}},
  issn         = {{2198-3844}},
  keywords     = {{heterogeneous catalysis; hierarchical porosity; imaging; pore characterization; sol-gel method; X-ray ptychography; X-ray tomography}},
  language     = {{eng}},
  month        = {{03}},
  number       = {{8}},
  pages        = {{2105432--2105432}},
  publisher    = {{John Wiley & Sons Inc.}},
  series       = {{Advanced science (Weinheim, Baden-Wurttemberg, Germany)}},
  title        = {{Evolution of Hierarchically Porous Nickel Alumina Catalysts Studied by X-Ray Ptychography}},
  url          = {{http://dx.doi.org/10.1002/advs.202105432}},
  doi          = {{10.1002/advs.202105432}},
  volume       = {{9}},
  year         = {{2022}},
}