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Surfaces
Special Issues
In Situ and Operando Catalyst Characterization
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In Situ and Operando Catalyst Characterization

A special issue of Surfaces (ISSN 2571-9637).

Deadline for manuscript submissions: 31 December 2024 | Viewed by 4710

Special Issue Editors

Prof. Dr. Gaetano Granozzi

E-Mail Website
Guest Editor
Department of Chemical Science, Universita degli Studi di Padova, Padua, Italy
Interests: ultrathin films; 2D materials; model electrocatalysts; model catalysts; HER, ORR and CRR
Special Issues, Collections and Topics in MDPI journals
Dr. Tomasz Kosmala

E-Mail Website
Guest Editor
Institute of Experimental Physics, Faculty of Physics and Astronomy, University of Wrocław, 50-204 Wrocław, Poland
Interests: surface science; electrochemistry; model catalyst; heterogeneous catalysis; water splitting; ultra-thin films; 2D materials; X-ray photoelectron spectroscopy; in-operando/in-situ EC-STM

Special Issue Information

Dear Colleagues,

The development of new technologies to meet the current energy and environmental challenges requires the acquisition of very fundamental knowledge regarding the structure and activity of catalytic materials at the nanometric scale. With the beginning of the new millennium, two “old” Latin words have attracted the attention of people working in the field of catalyst characterization: in situ and operando. We speak of in situ investigations when the evaluation of the catalyst is made under controlled pressure, atmosphere and temperature conditions, like those encountered during catalysis, but without this automatically implying any temporal evolution. Conversely, we speak of operando when the in situ investigations monitor the temporal evolution of the catalytic system and catalytic performances as the reactions take place. These concepts can be applied to a variety of advanced characterization techniques.  

A particularly challenging endeavor is to derive an accurate correlation between an atomically well-defined site and its catalytic activity. In many cases, standard characterization techniques provide only area-averaged information, so connecting specific figures of merit concerning the reactivity to a single type of catalytic site is not trivial, given that various structural and morphological features can be co-present on the same “real” catalyst. Nowadays, some advanced techniques (e.g., scanning probe microscopies and electron microscopies) can focus on single atomic sites and allow us to observe the atoms at work during the reaction that takes place on the surfaces of a catalyst.  

In this Special Issue, we cordially invite manuscripts that address advanced in situ and operando characterizations of catalysts, electrocatalysts, and, in general, other dynamic processes occurring on surfaces, both through local and defocused probes. We also welcome papers employing in silico approaches to study dynamic processes on surfaces.

Prof. Dr. Gaetano Granozzi
Dr. Tomasz Kosmala
Guest Editors

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. Surfaces is an international peer-reviewed open access quarterly 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 1600 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 and operando characterization
  • structure–activity relationships
  • knowledge-based approach for catalysts for energy, environment and industrial applications
  • study of the initial stage of the corrosion process
  • self-assembly, adsorption and related phenomena
  • STM/AFM and electrochemical STM/AFM
  • TEM and X-ray adsorption techniques (XANES and EXAFS)
  • ambient-pressure X-ray photoelectron spectroscopy
  • scanning electrochemical microscopy (SECM)
  • fourier-transform infrared spectroscopy (FTIR) and Raman spectroscopy
  • theoretical and computational studies

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Published Papers (4 papers)

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Research

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13 pages, 4356 KiB  
Article
Highly Reproducible Automated Tip Coater for In Situ and Operando EC-STM Measurements
by Robert Kurczak, Paulina Wira, Anna Futyma, Radosław Wasielewski and Tomasz Kosmala
Surfaces 2024, 7(4), 990-1002; https://doi.org/10.3390/surfaces7040065 - 18 Nov 2024
Viewed by 484
Abstract
High-quality, reproducible tip coatings are essential for minimizing faradaic currents in electrochemical scanning tunneling microscopy (EC-STM), especially during in situ and operando measurements. The variability inherent in manual coating methods, influenced by the operator’s skill and a lack of standardization, can lead to [...] Read more.
High-quality, reproducible tip coatings are essential for minimizing faradaic currents in electrochemical scanning tunneling microscopy (EC-STM), especially during in situ and operando measurements. The variability inherent in manual coating methods, influenced by the operator’s skill and a lack of standardization, can lead to inconsistent results, increased research costs, and a greater workload. This study introduces an Automated Tip Coater (ATC) designed to automate and standardize the tip coating process. The ATC features a tip movement system using stepper motors, a rotation module with a DC motor, and a heating block based on a soldering iron. It is controlled by an Arduino development board, supported by motor drivers, and has a user-friendly interface with an OLED display and encoder. The ATC coating mechanism includes a redesigned plate with a reduced gap size and a milled tray to precisely control the amount of insulating material applied to the tip. A fast cyclic voltammetry test in a 0.1 M HClO4 electrolyte demonstrated that over 75% of ATC-coated tips achieved excellent insulation with leakage currents below ±50 pA—and 30% below ±10 pA—suitable for highly sensitive experiments. Further measurements with EC-STM using the newly coated tips investigated the electrochemical behavior of highly oriented pyrolytic graphite (HOPG), revealing detailed atomic structures under dynamic electrochemical conditions. The ATC significantly enhances reproducibility, reduces dependency on operator skills, and lowers research costs while improving the accuracy and reliability of EC-STM measurements. Full article
(This article belongs to the Special Issue In Situ and Operando Catalyst Characterization)
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13 pages, 15943 KiB  
Article
Studying the Photoactivity of Ag-Decorated TiO2 Nanotubes with Combined AFM and Raman Spectroscopy
by Manjunath Veeranna Shinnur, Marco Menegazzo, Gianlorenzo Bussetti, Lamberto Duò, MariaPia Pedeferri and Maria Vittoria Diamanti
Surfaces 2024, 7(4), 938-950; https://doi.org/10.3390/surfaces7040061 - 2 Nov 2024
Viewed by 951
Abstract
The drive for the development of systems that can simultaneously investigate chemical and morphological information comes from the requisite to fully understand the structure and chemical reactivity relationships of materials. This is particularly relevant in photocatalysis, a field ruled by surface interactions. An [...] Read more.
The drive for the development of systems that can simultaneously investigate chemical and morphological information comes from the requisite to fully understand the structure and chemical reactivity relationships of materials. This is particularly relevant in photocatalysis, a field ruled by surface interactions. An in-depth understanding of these complex interactions could lead to significant improvements in materials design, and consequently, in photocatalytic performances. Here, we present a first approach to a combined atomic force microscopy (AFM) and Raman spectroscopy characterization of anodic TiO2 nanotubes arrays decorated with Ag nanoparticle electrodeposition from either the same anodizing organic electrolyte or from an aqueous one. Photocatalytic substrates were used in up to 15 consecutive photocatalysis tests to prove their possible deterioration with reuse. Sample aging can, in principle, produce changes in both the morphology and the chemical compounds that characterize the photocatalyst surface. Adopting multiple characterization techniques, such as a combination of AFM and Raman spectroscopy in an original setup, can profitably enable the observation of surface contamination. A significant drop in photocatalytic activity was observed after 10 cycles on samples where silver was deposited from the organic electrolyte, while the others remained stable. Such a drop was ascribed to photocatalyst deactivation. While in other cases, a simple recovery treatment allowed the initial photoactivity to be restored, this deactivation was not restored even after chemical and thermal cleaning treatments. Full article
(This article belongs to the Special Issue In Situ and Operando Catalyst Characterization)
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Review

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18 pages, 6191 KiB  
Review
Catalytically Active Materials Visualized by Scanning Photoelectron Spectro-Microscopy
by Matteo Amati, Lada V. Yashina, Philipp Winkler, Kevin Sparwasser, Zygmunt Milosz, Günther Rupprechter and Luca Gregoratti
Surfaces 2024, 7(3), 442-459; https://doi.org/10.3390/surfaces7030028 - 26 Jun 2024
Viewed by 1323
Abstract
Modern catalysts are complex systems whose performance depends both on space and time domains and, most importantly, on the operational environment. As a direct consequence, understanding their functionalities requires sophisticated techniques and tools for measurement and simulation, addressing the proper spatial and temporal [...] Read more.
Modern catalysts are complex systems whose performance depends both on space and time domains and, most importantly, on the operational environment. As a direct consequence, understanding their functionalities requires sophisticated techniques and tools for measurement and simulation, addressing the proper spatial and temporal scale and being capable of mimicking the working conditions of every single component, such as catalyst supports, electrodes, electrolytes, as well as of the entire assembly, e.g., in the case of fuel cells or batteries. Scanning photoelectron spectro-microscopy (SPEM) is one of the approaches that allow combining X-ray photoelectron spectroscopy with sub-micron spatial resolution; in particular, the SPEM hosted at the ESCA Microscopy beamline at Elettra has been upgraded to conduct in situ and operando experiments. Three different case studies are presented to illustrate the capabilities of the SPEM in the investigation of catalytic materials in different conditions and processes. Full article
(This article belongs to the Special Issue In Situ and Operando Catalyst Characterization)
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44 pages, 10192 KiB  
Review
Metal–Perovskite Interfacial Engineering to Boost Activity in Heterogeneous Catalysis
by Christoph Malleier and Simon Penner
Surfaces 2024, 7(2), 296-339; https://doi.org/10.3390/surfaces7020020 - 6 May 2024
Viewed by 1194
Abstract
In this review, we have assessed the possibility of metal–perovskite interfacial engineering to enhance the catalytic activity and selectivity in a range of heterogeneous catalytic reactions. We embarked on a literature screening of different perovskite material classes and reactions to show the versatility [...] Read more.
In this review, we have assessed the possibility of metal–perovskite interfacial engineering to enhance the catalytic activity and selectivity in a range of heterogeneous catalytic reactions. We embarked on a literature screening of different perovskite material classes and reactions to show the versatility of the perovskite structures to induce the formation of such hetero-interfaces and the widespread nature of the phenomenon in catalytic research. There is almost no limitation on the chemical composition of the used perovskites and the nature of the catalyzed reaction, be it under reduction or oxidation conditions. We attempted to classify the perovskite materials, discuss the different strategies leading to the hetero-interfaces, and detail the synergistic action of the components of the respective interfaces. We also provide a critical assessment of the large body of data that is available in terms of a knowledge-based approach to the comparison of differently prepared interfaces with varying interfacial extent to gain a deeper understanding of the bi-functional operation of the interfaces and the urgent necessity to study and characterize such interfaces under realistic operation conditions. Full article
(This article belongs to the Special Issue In Situ and Operando Catalyst Characterization)
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