Novel sample-stage for combined near ambient pressure x-ray photoelectron spectroscopy, catalytic characterization and electrochemical impedance spectroscopy

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Novel sample-stage for combined near ambient pressure x-ray photoelectron spectroscopy, catalytic characterization and electrochemical impedance spectroscopy. / Rameshan, Raffael; Nenning, Andreas; Raschhofer, Johannes et al.
in: Crystals, Jahrgang 10.2020, Nr. 10, 947, 17.10.2020.

Publikationen: Beitrag in FachzeitschriftArtikelForschung(peer-reviewed)

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@article{844dee0c60a447e6bfddfebcc076c6d6,
title = "Novel sample-stage for combined near ambient pressure x-ray photoelectron spectroscopy, catalytic characterization and electrochemical impedance spectroscopy",
abstract = "For an in-depth characterization of catalytic materials and their properties, spectroscopic in-situ (operando) investigations are indispensable. With the rapid development of advanced commercial spectroscopic equipment, it is possible to combine complementary methods in a single system. This allows for simultaneously gaining insights into surface and bulk properties of functional oxides, such as defect chemistry, catalytic characteristics, electronic structure, etc., enabling a direct correlation of structure and reactivity of catalyst materials, thus facilitating effective catalyst development. Here, we present a novel sample-stage, which was specifically developed to pave the way to a lab–based combination of near ambient pressure X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy with simultaneous catalytic operando measurements. This setup is designed to probe different (model) systems under conditions close to real heterogeneous catalysis, with a focus on solid oxide electrochemical cells. In a proof of concept experiment using an electrochemical model cell with the doped perovskite Nd0.6 Ca0.4 Fe0.9 Co0.1 O3-δ as working electrode, the precise control of the surface chemistry that is possible with this setup is demonstrated. The exsolution behavior of the material was studied, showing that at a lower temperature (500◦ C) with lower reducing potential of the gas phase, only cobalt was exsolved, forming metallic particles on the surface of the perovskite-type oxide. Only when the temperature was increased to 600◦ C and a cathodic potential was applied (−250 mV) Fe also started to be released from the perovskite lattice.",
keywords = "Catalytic materials, Electrochemical impedance spectroscopy, In-situ spectroscopy, NAP-XPS",
author = "Raffael Rameshan and Andreas Nenning and Johannes Raschhofer and Lorenz Lindenthal and Thomas Ruh and Harald Summerer and Opitz, {Alexander Karl} and Huber, {Tobias Martin} and Christoph Rameshan",
note = "Publisher Copyright: {\textcopyright} 2020 by the authors. Licensee MDPI, Basel, Switzerland.",
year = "2020",
month = oct,
day = "17",
doi = "10.3390/cryst10100947",
language = "English",
volume = "10.2020",
journal = "Crystals",
issn = "2073-4352",
publisher = "Multidisciplinary Digital Publishing Institute (MDPI)",
number = "10",

}

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TY - JOUR

T1 - Novel sample-stage for combined near ambient pressure x-ray photoelectron spectroscopy, catalytic characterization and electrochemical impedance spectroscopy

AU - Rameshan, Raffael

AU - Nenning, Andreas

AU - Raschhofer, Johannes

AU - Lindenthal, Lorenz

AU - Ruh, Thomas

AU - Summerer, Harald

AU - Opitz, Alexander Karl

AU - Huber, Tobias Martin

AU - Rameshan, Christoph

N1 - Publisher Copyright: © 2020 by the authors. Licensee MDPI, Basel, Switzerland.

PY - 2020/10/17

Y1 - 2020/10/17

N2 - For an in-depth characterization of catalytic materials and their properties, spectroscopic in-situ (operando) investigations are indispensable. With the rapid development of advanced commercial spectroscopic equipment, it is possible to combine complementary methods in a single system. This allows for simultaneously gaining insights into surface and bulk properties of functional oxides, such as defect chemistry, catalytic characteristics, electronic structure, etc., enabling a direct correlation of structure and reactivity of catalyst materials, thus facilitating effective catalyst development. Here, we present a novel sample-stage, which was specifically developed to pave the way to a lab–based combination of near ambient pressure X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy with simultaneous catalytic operando measurements. This setup is designed to probe different (model) systems under conditions close to real heterogeneous catalysis, with a focus on solid oxide electrochemical cells. In a proof of concept experiment using an electrochemical model cell with the doped perovskite Nd0.6 Ca0.4 Fe0.9 Co0.1 O3-δ as working electrode, the precise control of the surface chemistry that is possible with this setup is demonstrated. The exsolution behavior of the material was studied, showing that at a lower temperature (500◦ C) with lower reducing potential of the gas phase, only cobalt was exsolved, forming metallic particles on the surface of the perovskite-type oxide. Only when the temperature was increased to 600◦ C and a cathodic potential was applied (−250 mV) Fe also started to be released from the perovskite lattice.

AB - For an in-depth characterization of catalytic materials and their properties, spectroscopic in-situ (operando) investigations are indispensable. With the rapid development of advanced commercial spectroscopic equipment, it is possible to combine complementary methods in a single system. This allows for simultaneously gaining insights into surface and bulk properties of functional oxides, such as defect chemistry, catalytic characteristics, electronic structure, etc., enabling a direct correlation of structure and reactivity of catalyst materials, thus facilitating effective catalyst development. Here, we present a novel sample-stage, which was specifically developed to pave the way to a lab–based combination of near ambient pressure X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy with simultaneous catalytic operando measurements. This setup is designed to probe different (model) systems under conditions close to real heterogeneous catalysis, with a focus on solid oxide electrochemical cells. In a proof of concept experiment using an electrochemical model cell with the doped perovskite Nd0.6 Ca0.4 Fe0.9 Co0.1 O3-δ as working electrode, the precise control of the surface chemistry that is possible with this setup is demonstrated. The exsolution behavior of the material was studied, showing that at a lower temperature (500◦ C) with lower reducing potential of the gas phase, only cobalt was exsolved, forming metallic particles on the surface of the perovskite-type oxide. Only when the temperature was increased to 600◦ C and a cathodic potential was applied (−250 mV) Fe also started to be released from the perovskite lattice.

KW - Catalytic materials

KW - Electrochemical impedance spectroscopy

KW - In-situ spectroscopy

KW - NAP-XPS

UR - http://www.scopus.com/inward/record.url?scp=85092715058&partnerID=8YFLogxK

U2 - 10.3390/cryst10100947

DO - 10.3390/cryst10100947

M3 - Article

AN - SCOPUS:85092715058

VL - 10.2020

JO - Crystals

JF - Crystals

SN - 2073-4352

IS - 10

M1 - 947

ER -