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Catalysts
Special Issues
In-Situ Characterisation of Heterogeneous Catalysts and Energy Materials
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In-Situ Characterisation of Heterogeneous Catalysts and Energy Materials

A special issue of Catalysts (ISSN 2073-4344).

Deadline for manuscript submissions: closed (30 September 2021) | Viewed by 9400

Special Issue Editor

Dr. Manfred Erwin Schuster

E-Mail Website
Guest Editor
Johnson Matthey Technology Centre, Blount’s Court, Sonning Common RG4 9NH, U.K.
Diamond Light Source - Harwell Science and Innovation Campus, Fermi Ave, Didcot OX11 0DE, UK
Interests: catalysis; electron microscopy; in-situ microscopy; multilength scale characterization; nanomaterials for energy and environmental applications

Special Issue Information

Dear Colleagues,

In-situ transmission electron microscopy has established itself over the last few years as a reproducible state-of-the-art technique for the study of materials in real time, and under so called “real-world” conditions. The ability to study the dynamic behavior of a catalytically active material during reaction conditions has provided a major step towards understanding catalytic activity and its evolution over time. This is a step-change compared with the traditional ex-situ approach of studying "fresh/spent" catalysts.

Nowadays, two different systems are used for in-situ microscopy: on the one hand, dedicated in-situ environmental transmission electron microscopes (ETEM) with a differentially pumped objective lens enable a window-free imaging of the sample in question, and are limited to several 10 s mbar of pressure; on the other hand, mems-based in-situ TEM holders which allow pressures of up to 1 bar within the cell.

In-situ microscopy and so called “operando” microscopy allow for correlating the dynamic changes the catalyst undergoes to variations in the catalytic performance (e.g., a mass spectrometer analysis of the residual gases to determine changes in the formed products, or in the case of energy materials changes in the cyclic voltammetry curves). Submissions to this special edition are welcome in the form of original research papers which utilize in-situ gas or liquid systems to better understand catalysts and/or energy materials by means of microscopy or spectroscopy techniques.

Dr. Manfred Erwin Schuster
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Catalysts is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • in-situ microscopy
  • operando
  • dynamic
  • ETEM
  • mems
  • catalysis
  • energy materials

Published Papers (2 papers)

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Research

17 pages, 4129 KiB  
Article
Hydrothermal Sintering and Oxidation of an Alumina-Supported Nickel Methanation Catalyst Studied Using In Situ Magnetometry
by Malebelo Maphutha, Dominic de Oliveira, Thulani M. Nyathi, Mohamed I. Fadlalla, Robert Henkel, Nico Fischer and Michael Claeys
Catalysts 2021, 11(5), 636; https://doi.org/10.3390/catal11050636 - 16 May 2021
Cited by 2 | Viewed by 2504
Abstract
The presented study investigated the effects of temperature (350–650 °C) and gas environment (pure Ar versus a H2O/H2 partial pressure ratio (PH2O/PH2) of 5) on the extent of sintering and oxidation of Al2O3 [...] Read more.
The presented study investigated the effects of temperature (350–650 °C) and gas environment (pure Ar versus a H2O/H2 partial pressure ratio (PH2O/PH2) of 5) on the extent of sintering and oxidation of Al2O3-supported Ni0 nanoparticles (≈4 nm). We note that a PH2O/PH2 of 5 corresponds to a simulated CO conversion of 94% during methanation. Sintering and oxidation were studied using in situ magnetometry, while ex situ TEM analyses confirmed the particle sizes before and after the magnetometry-based experiments. It was found that increasing the temperature from 350 to 650 °C in Ar at atmospheric pressure causes a negligible change to the average size and degree of reduction (DOR) of the starting Ni0 nanoparticles. However, studying the same temperature window under hydrothermal conditions at 10 bar causes significant particle growth (≈9 nm) and the development of a bimodal distribution. Furthermore, the presence of steam decreases the DOR of Ni0 from 86.2% after initial activation to 22.2% due to oxidation. In summary, this study reports on the expected sintering and oxidation of Ni-based catalysts under high CO conversion conditions at elevated temperatures during methanation. Importantly, we were able to demonstrate how magnetometry-based analyses can provide similar size information (and changes thereof) as those observed with TEM but with the added advantage that this information can be obtained in situ. Full article
(This article belongs to the Special Issue In-Situ Characterisation of Heterogeneous Catalysts and Energy Materials)
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14 pages, 2508 KiB  
Article
Modifying the Surface Structure of Perovskite-Based Catalysts by Nanoparticle Exsolution
by Lorenz Lindenthal, Raffael Rameshan, Harald Summerer, Thomas Ruh, Janko Popovic, Andreas Nenning, Stefan Löffler, Alexander Karl Opitz, Peter Blaha and Christoph Rameshan
Catalysts 2020, 10(3), 268; https://doi.org/10.3390/catal10030268 - 1 Mar 2020
Cited by 33 | Viewed by 5914
Abstract
In heterogeneous catalysis, surfaces decorated with uniformly dispersed, catalytically-active (nano)particles are a key requirement for excellent performance. Beside standard catalyst preparation routines—with limitations in controlling catalyst surface structure (i.e., particle size distribution or dispersion)—we present here a novel time efficient route to precisely [...] Read more.
In heterogeneous catalysis, surfaces decorated with uniformly dispersed, catalytically-active (nano)particles are a key requirement for excellent performance. Beside standard catalyst preparation routines—with limitations in controlling catalyst surface structure (i.e., particle size distribution or dispersion)—we present here a novel time efficient route to precisely tailor catalyst surface morphology and composition of perovskites. Perovskite-type oxides of nominal composition ABO3 with transition metal cations on the B-site can exsolve the B-site transition metal upon controlled reduction. In this exsolution process, the transition metal emerges from the oxide lattice and migrates to the surface where it forms catalytically active nanoparticles. Doping the B-site with reducible and catalytically highly active elements, offers the opportunity of tailoring properties of exsolution catalysts. Here, we present the synthesis of two novel perovskite catalysts Nd0.6Ca0.4FeO3-δ and Nd0.6Ca0.4Fe0.9Co0.1O3-δ with characterisation by (in situ) XRD, SEM/TEM and XPS, supported by theory (DFT+U). Fe nanoparticle formation was observed for Nd0.6Ca0.4FeO3-δ. In comparison, B site cobalt doping leads, already at lower reduction temperatures, to formation of finely dispersed Co nanoparticles on the surface. These novel perovskite-type catalysts are highly promising for applications in chemical energy conversion. First measurements revealed that exsolved Co nanoparticles significantly improve the catalytic activity for CO2 activation via reverse water gas shift reaction. Full article
(This article belongs to the Special Issue In-Situ Characterisation of Heterogeneous Catalysts and Energy Materials)
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