In Situ/Operando Characterization of Complex Materials Employing Advanced Synchrotron-Based Techniques

A special issue of Catalysts (ISSN 2073-4344). This special issue belongs to the section "Catalytic Materials".

Deadline for manuscript submissions: closed (30 July 2023) | Viewed by 3283

Special Issue Editor

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Guest Editor
Institute of Technical and Polymer Chemistry, Karlsruhe Institute of Technology, Karlsruhe, Germany
Interests: X-ray-based characterization techniques; synchrotron radiation; in situ/operando experiments; electronic structure; modulation excitation spectroscopy; theoretical calculation of spectra

Special Issue Information

Dear Colleagues,

The interest in the development of bimetallic catalysts is growing fast due to the important role played by these catalysts in the field of energy, environment, and industry. Bimetallic nanoparticle catalysts are promising because the synergy between two metals can lead to enhanced activity in catalysis or allow for bifunctional properties such as magnetic and plasmonic properties. Assessing the structure–activity relationship of these complex catalyst systems is a major challenge as there are several parameters affecting the measurements. With the increased sensitivity of modern synchrotrons and improved analysis methods, X-ray based methods have become a standard technique for the structural characterization of catalytic nanoparticles. Using high-energy X-rays, it is possible to conduct experiments under realistic reaction conditions, i.e., high temperature, pressure, and flow of reactants. To perform such in situ/operando time resolved experiments, portable cells and set-ups are designed based on various applications. Other than developing the in situ/operando reactor set-up to perform advance characterization of the bimetallic systems, the development of new theoretical as well as analysis methods is also required to understand the large amount of data recorded during experiments. Challenges that occur during such complicated time-resolved experiments, e.g., low sensitivity of characterization bulk techniques toward minority species or occurrence of several intermediate species during complex chemical transformations have led to sustained progress in the areas of experimental as well as theoretical methods. Application of enhanced experimental techniques combined with rigorous data analysis methods can provide information about the active sites of the bimetallic catalyst which would not be possible to gather with conventional characterization techniques/methods.

Submissions to this Special Issue are welcome in the form of original research papers which will cover in situ/operando characterization of bimetallic catalysts by employing advanced synchrotron-based techniques and rigorous data analysis methods to unravel the minute structural/phase changes occurring during catalytic reactions.

Dr. Abhijeet Gaur
Guest Editor

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  • in situ
  • operando
  • bimetallic catalysts
  • X-ray-based methods
  • synchrotron radiation

Published Papers (1 paper)

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15 pages, 2607 KiB  
In Situ H2 Reduction of Al2O3-Supported Ni- and Mo-Based Catalysts
by Sabrina Maria Gericke, Jenny Rissler, Marie Bermeo, Harald Wallander, Hanna Karlsson, Linnéa Kollberg, Mattia Scardamaglia, Robert Temperton, Suyun Zhu, Kajsa G. V. Sigfridsson Clauss, Christian Hulteberg, Andrey Shavorskiy, Lindsay Richard Merte, Maria Elise Messing, Johan Zetterberg and Sara Blomberg
Catalysts 2022, 12(7), 755; - 08 Jul 2022
Cited by 6 | Viewed by 2525
Nickel (Ni)-promoted Molybdenum (Mo)-based catalysts are used for hydrotreatment processes in the chemical industry where the catalysts are exposed to high-pressure H2 at elevated temperature. In this environment, the catalyst transforms into the active phase, which involves the reduction of the oxide. [...] Read more.
Nickel (Ni)-promoted Molybdenum (Mo)-based catalysts are used for hydrotreatment processes in the chemical industry where the catalysts are exposed to high-pressure H2 at elevated temperature. In this environment, the catalyst transforms into the active phase, which involves the reduction of the oxide. Here, we report on the first in situ study on the reduction of alumina supported Ni- and Mo-based catalysts in 1 mbar H2 using ambient-pressure X-ray photoelectron spectroscopy (APXPS). The study confirms that mixing Ni and Mo lowers the reduction temperature of both Ni- and Mo-oxide as compared to the monometallic catalysts and shows that the MoO3 reduction starts at a lower temperature than the reduction of NiO in NiMo/Al2O3 catalysts. Additionally, the reduction of Ni and Mo foil was directly compared to the reduction of the Al2O3-supported catalysts and it was observed that the reduction of the supported catalysts is more gradual than the reduction of the foils, indicating a strong interaction between the Ni/Mo and the alumina support. Full article
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