X-ray emission spectroscopy: highly sensitive techniques for time-resolved probing of cerium reactivity under catalytic conditions

Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic pr...

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Published inPhysical chemistry chemical physics : PCCP Vol. 18; no. 47; pp. 32486 - 32493
Main Authors Kopelent, R, van Bokhoven, J. A, Nachtegaal, M, Szlachetko, J, Safonova, O. V
Format Journal Article
LanguageEnglish
Published England 01.01.2016
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Abstract Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic processes. To prove that cerium changes its oxidation state in the catalytic cycle the transient rates of Ce 3+ formation and decay should be compared to the overall reaction rate. For such mechanistic studies the time resolution is essential as the quantification of the Ce 3+ species should be faster than the reaction rate. However, it is challenging to follow the dynamic changes of the cerium oxidation state under reaction conditions, especially when the concentration of cerium atoms involved in the reaction cycle is low. In this paper, we evaluate the sensitivity of high-resolution X-ray emission-based methods for the in situ time-resolved quantification of small concentrations of Ce 3+ in ceria-based materials. We demonstrate that resonant X-ray emission spectroscopy (RXES) at optimal excitation energy is more sensitive than high energy resolution off-resonant spectroscopy (HEROS) and non-resonant X-ray emission spectroscopy (non-resonant XES) and that it can track the reactivity of less than 0.3% of cerium atoms in a 1% Pt/CeO 2 catalyst in a plug-flow reactor with sub-second time resolution. These results demonstrate that X-ray emission-based methods can be used as very sensitive tools and provide new insights into dynamic changes of the oxidation state in reducible oxides in a variety of applications. High sensitivity of X-ray emission spectroscopy based methods for in situ time-resolved quantification of Ce 3+ in ceria-based catalysts and related materials.
AbstractList Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic processes. To prove that cerium changes its oxidation state in the catalytic cycle the transient rates of Ce 3+ formation and decay should be compared to the overall reaction rate. For such mechanistic studies the time resolution is essential as the quantification of the Ce 3+ species should be faster than the reaction rate. However, it is challenging to follow the dynamic changes of the cerium oxidation state under reaction conditions, especially when the concentration of cerium atoms involved in the reaction cycle is low. In this paper, we evaluate the sensitivity of high-resolution X-ray emission-based methods for the in situ time-resolved quantification of small concentrations of Ce 3+ in ceria-based materials. We demonstrate that resonant X-ray emission spectroscopy (RXES) at optimal excitation energy is more sensitive than high energy resolution off-resonant spectroscopy (HEROS) and non-resonant X-ray emission spectroscopy (non-resonant XES) and that it can track the reactivity of less than 0.3% of cerium atoms in a 1% Pt/CeO 2 catalyst in a plug-flow reactor with sub-second time resolution. These results demonstrate that X-ray emission-based methods can be used as very sensitive tools and provide new insights into dynamic changes of the oxidation state in reducible oxides in a variety of applications.
Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic processes. To prove that cerium changes its oxidation state in the catalytic cycle the transient rates of Ce3+ formation and decay should be compared to the overall reaction rate. For such mechanistic studies the time resolution is essential as the quantification of the Ce3+ species should be faster than the reaction rate. However, it is challenging to follow the dynamic changes of the cerium oxidation state under reaction conditions, especially when the concentration of cerium atoms involved in the reaction cycle is low. In this paper, we evaluate the sensitivity of high-resolution X-ray emission-based methods for the in situ time-resolved quantification of small concentrations of Ce3+ in ceria-based materials. We demonstrate that resonant X-ray emission spectroscopy (RXES) at optimal excitation energy is more sensitive than high energy resolution off-resonant spectroscopy (HEROS) and non-resonant X-ray emission spectroscopy (non-resonant XES) and that it can track the reactivity of less than 0.3% of cerium atoms in a 1% Pt/CeO2 catalyst in a plug-flow reactor with sub-second time resolution. These results demonstrate that X-ray emission-based methods can be used as very sensitive tools and provide new insights into dynamic changes of the oxidation state in reducible oxides in a variety of applications.
Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic processes. To prove that cerium changes its oxidation state in the catalytic cycle the transient rates of Ce formation and decay should be compared to the overall reaction rate. For such mechanistic studies the time resolution is essential as the quantification of the Ce species should be faster than the reaction rate. However, it is challenging to follow the dynamic changes of the cerium oxidation state under reaction conditions, especially when the concentration of cerium atoms involved in the reaction cycle is low. In this paper, we evaluate the sensitivity of high-resolution X-ray emission-based methods for the in situ time-resolved quantification of small concentrations of Ce in ceria-based materials. We demonstrate that resonant X-ray emission spectroscopy (RXES) at optimal excitation energy is more sensitive than high energy resolution off-resonant spectroscopy (HEROS) and non-resonant X-ray emission spectroscopy (non-resonant XES) and that it can track the reactivity of less than 0.3% of cerium atoms in a 1% Pt/CeO catalyst in a plug-flow reactor with sub-second time resolution. These results demonstrate that X-ray emission-based methods can be used as very sensitive tools and provide new insights into dynamic changes of the oxidation state in reducible oxides in a variety of applications.
Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe and quantify this activity which involves a change in the cerium oxidation state and to understand the involvement of cerium in catalytic processes. To prove that cerium changes its oxidation state in the catalytic cycle the transient rates of Ce 3+ formation and decay should be compared to the overall reaction rate. For such mechanistic studies the time resolution is essential as the quantification of the Ce 3+ species should be faster than the reaction rate. However, it is challenging to follow the dynamic changes of the cerium oxidation state under reaction conditions, especially when the concentration of cerium atoms involved in the reaction cycle is low. In this paper, we evaluate the sensitivity of high-resolution X-ray emission-based methods for the in situ time-resolved quantification of small concentrations of Ce 3+ in ceria-based materials. We demonstrate that resonant X-ray emission spectroscopy (RXES) at optimal excitation energy is more sensitive than high energy resolution off-resonant spectroscopy (HEROS) and non-resonant X-ray emission spectroscopy (non-resonant XES) and that it can track the reactivity of less than 0.3% of cerium atoms in a 1% Pt/CeO 2 catalyst in a plug-flow reactor with sub-second time resolution. These results demonstrate that X-ray emission-based methods can be used as very sensitive tools and provide new insights into dynamic changes of the oxidation state in reducible oxides in a variety of applications. High sensitivity of X-ray emission spectroscopy based methods for in situ time-resolved quantification of Ce 3+ in ceria-based catalysts and related materials.
Author Szlachetko, J
Safonova, O. V
Kopelent, R
van Bokhoven, J. A
Nachtegaal, M
AuthorAffiliation Institute of Physics
ETH Zürich
Jan Kochanowski University
Paul Scherrer Institute
Institute for Chemical and Bioengineering
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Snippet Oxygen storage materials such as ceria are used in many catalytic applications because they can reversibly bind and release oxygen. Tools are needed to observe...
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SubjectTerms Catalysis
Catalysts
Cerium
Cerium oxide
Dynamics
Emission spectroscopy
Valence
X-rays
Title X-ray emission spectroscopy: highly sensitive techniques for time-resolved probing of cerium reactivity under catalytic conditions
URI https://www.ncbi.nlm.nih.gov/pubmed/27869264
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https://search.proquest.com/docview/1864580714
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