Calibration of the X-Ray Photoelectron Spectroscopy Binding Energy Scale for the Characterization of Heterogeneous Catalysts: Is Everything Really under Control?

Investigations of X‐ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding en...

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Vydáno v:	Chemphyschem Ročník 14; číslo 15; s. 3618 - 3626
Hlavní autoři:	Jacquemin, Marc, Genet, Michel J., Gaigneaux, Eric M., Debecker, Damien P.
Médium:	Journal Article
Jazyk:	angličtina
Vydáno:	Weinheim WILEY-VCH Verlag 21.10.2013 WILEY‐VCH Verlag Wiley Wiley Subscription Services, Inc
Témata:	Calibration carbon contamination Catalysis Chemistry Exact sciences and technology General and physical chemistry heterogeneous catalysis ionicity Spectrum analysis Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry X-ray photoelectron spectroscopy carbon contamination Transition metal Palladium Calibration Carbon Silica Supported catalyst Characterization Heterogeneous catalysis Investigation method Binding energy ionicity Photoelectron spectrometry Platinoid X-ray photoelectron spectroscopy heterogeneous catalysis calibration
ISSN:	1439-4235, 1439-7641, 1439-7641
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Abstract	Investigations of X‐ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2–Al2O3 supports and Pd/SiO2–Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument‐related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. Taking control: X‐ray photoelectron spectroscopy (XPS) analysis of heterogeneous catalysts usually relies on binding energy scale calibration by using the C 1s peak as an internal standard. The inorganic solid can, however, have a marked impact on the photoelectron emitted from the adventitious carbon, and this creates an important calibration bias that must be taken into account and corrected for proper use of XPS data.
AbstractList	Investigations of X-ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C-(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2-Al2O3 supports and Pd/SiO2-Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument-related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. Investigations of X-ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C-(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2-Al2O3 supports and Pd/SiO2-Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument-related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered.Investigations of X-ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C-(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2-Al2O3 supports and Pd/SiO2-Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument-related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. Investigations of X‐ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C (C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO 2 –Al 2 O 3 supports and Pd/SiO 2 –Al 2 O 3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument‐related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. Investigations of X‐ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C(C,H) component of the C 1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2–Al2O3 supports and Pd/SiO2–Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument‐related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. Taking control: X‐ray photoelectron spectroscopy (XPS) analysis of heterogeneous catalysts usually relies on binding energy scale calibration by using the C 1s peak as an internal standard. The inorganic solid can, however, have a marked impact on the photoelectron emitted from the adventitious carbon, and this creates an important calibration bias that must be taken into account and corrected for proper use of XPS data. Investigations of X-ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous catalysts and their supports, the C(C,H) component of the C1s peak is often used as an internal standard for the calibration of the binding energy scale. Although this method is widely recognized as suitable for the study of heterogeneous catalysts, we show that a significant calibration bias can be encountered upon comparing samples with different bulk composition. In this paper, a series of SiO2-Al2O3 supports and Pd/SiO2-Al2O3 catalysts with various Si/Al ratios were studied. The spectra issued from these samples were processed with the classical calibration method on the basis of the carbon peak. Important discrepancies in the relative position of the photoelectron peaks were noticed. After systematically discarding instrument-related issues, a true chemical influence of the bulk matrix on the analyzed surface species was evidenced. The extent of this chemical effect was dependent on the composition of the sample and more precisely on its ionicity. Two possible mechanisms for this chemical effect were proposed and discussed. Finally, an alternative calibration method was offered. [PUBLICATION ABSTRACT]
Author	Gaigneaux, Eric M. Genet, Michel J. Jacquemin, Marc Debecker, Damien P.
Author_xml	– sequence: 1 givenname: Marc surname: Jacquemin fullname: Jacquemin, Marc organization: Institute of Condensed Matter and Nanosciences (IMCN), Molecules, Solids and Reactivity (MOST), Université catholique de Louvain, Croix du Sud 2/L7.05.17, 1348 Louvain-la-Neuve (Belgium) – sequence: 2 givenname: Michel J. surname: Genet fullname: Genet, Michel J. organization: Institute of Condensed Matter and Nanosciences (IMCN), Bio- and Soft Matter (BSMA) and Surface Characterisation Platform (SUCH), Université catholique de Louvain, Croix du Sud 2/L7.04.01, 1348 Louvain-la-Neuve (Belgium) – sequence: 3 givenname: Eric M. surname: Gaigneaux fullname: Gaigneaux, Eric M. organization: Institute of Condensed Matter and Nanosciences (IMCN), Molecules, Solids and Reactivity (MOST), Université catholique de Louvain, Croix du Sud 2/L7.05.17, 1348 Louvain-la-Neuve (Belgium) – sequence: 4 givenname: Damien P. surname: Debecker fullname: Debecker, Damien P. email: damien.debecker@uclouvain.be organization: Institute of Condensed Matter and Nanosciences (IMCN), Molecules, Solids and Reactivity (MOST), Université catholique de Louvain, Croix du Sud 2/L7.05.17, 1348 Louvain-la-Neuve (Belgium)
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Keywords	carbon contamination Transition metal Palladium Calibration Carbon Silica Supported catalyst Characterization Heterogeneous catalysis Investigation method Binding energy ionicity Photoelectron spectrometry Platinoid X-ray photoelectron spectroscopy heterogeneous catalysis calibration
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Snippet	Investigations of X‐ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous... Investigations of X-ray photoelectron spectra from solid samples need corrections for the surface charging effect. For powder samples such as heterogeneous...
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SubjectTerms	Calibration carbon contamination Catalysis Chemistry Exact sciences and technology General and physical chemistry heterogeneous catalysis ionicity Spectrum analysis Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry X-ray photoelectron spectroscopy
Title	Calibration of the X-Ray Photoelectron Spectroscopy Binding Energy Scale for the Characterization of Heterogeneous Catalysts: Is Everything Really under Control?
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