X-Ray Absorption Spectroscopy (XAS): Surface Structural Determination of Alloy Nanoparticles

Guanghui Zhang; Nicole LiBretto; Stephen Purdy; Laryssa Cesar; Jeffrey Miller

doi:10.1007/978-3-031-07125-6_30

X-Ray Absorption Spectroscopy (XAS): Surface Structural Determination of Alloy Nanoparticles

Guanghui Zhang, Nicole LiBretto, Stephen Purdy, Laryssa Cesar, Jeffrey Miller

Chemical Process Scale Up

Research output: Chapter in Book/Report/Conference proceeding › Chapter › peer-review

1 Scopus citations

Abstract

In catalysis since reactions occur on the surface of nanoparticles (NP), it is essential to determine the composition of this structure, rather than that of the nanoparticles, since the two may be, and often are, different. Conventional techniques including X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are powerful techniques, but these data reflect the average composition of the entire particle. In this chapter, we introduce the method of EXAFS analysis, which isolates the surface atoms of nanoparticles based on its sensitivity to chemical reactions, specifically surface oxidation. As shown in our case studies, if the surface of a Pt-based nanoparticle is contacted by air at room temperature, the surface will selectively oxidize, resulting in the loss of Pt-Pt and Pt-M bonds to the formation of Pt-O bonds. The difference between the completely reduced and surface-oxidized nanoparticle allows for the isolation of signal from the catalytic surface. Although these examples highlight Pt alloys, similar analysis is also possible for other group 8 and IB bimetallic catalysts.

Original language	English
Title of host publication	Springer Handbooks
Publisher	Springer Science and Business Media Deutschland GmbH
Pages	659-669
Number of pages	11
DOIs	https://doi.org/10.1007/978-3-031-07125-6_30
State	Published - 2023

Publication series

Name	Springer Handbooks
ISSN (Print)	2522-8692
ISSN (Electronic)	2522-8706

Funding

This chapter is based on work supported by the National Science Foundation under cooperative agreement no. EEC-1647722. GZ would like to acknowledge the National Natural Science Foundation of China (21902019) and Fundamental Research Funds for the Central Universities (DUT18RC(3)057 and DUT20RC(5)002). Use of the Advanced Photon Source was supported by the US Department of Energy, Office of Basic Energy Sciences, under contract no. DE-AC02-06CH11357. MRCAT operations, beamline 10-BM, are supported by the Department of Energy and the MRCAT member institutions. The authors also acknowledge the use of beamline 11-ID-C at APS.

Funders	Funder number
National Science Foundation	EEC-1647722
U.S. Department of Energy
Basic Energy Sciences	DE-AC02-06CH11357
National Natural Science Foundation of China	21902019
Fundamental Research Funds for the Central Universities	DUT20RC(5)002, DUT18RC(3)057

Keywords

Intermetallic alloy
Propane dehydrogenation
Pt alloy catalysts
Resonant inelastic X-ray scattering
Surface structure
Surface-sensitive X-ray absorption

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10.1007/978-3-031-07125-6_30

Cite this

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title = "X-Ray Absorption Spectroscopy (XAS): Surface Structural Determination of Alloy Nanoparticles",

abstract = "In catalysis since reactions occur on the surface of nanoparticles (NP), it is essential to determine the composition of this structure, rather than that of the nanoparticles, since the two may be, and often are, different. Conventional techniques including X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are powerful techniques, but these data reflect the average composition of the entire particle. In this chapter, we introduce the method of EXAFS analysis, which isolates the surface atoms of nanoparticles based on its sensitivity to chemical reactions, specifically surface oxidation. As shown in our case studies, if the surface of a Pt-based nanoparticle is contacted by air at room temperature, the surface will selectively oxidize, resulting in the loss of Pt-Pt and Pt-M bonds to the formation of Pt-O bonds. The difference between the completely reduced and surface-oxidized nanoparticle allows for the isolation of signal from the catalytic surface. Although these examples highlight Pt alloys, similar analysis is also possible for other group 8 and IB bimetallic catalysts.",

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author = "Guanghui Zhang and Nicole LiBretto and Stephen Purdy and Laryssa Cesar and Jeffrey Miller",

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T2 - Surface Structural Determination of Alloy Nanoparticles

AU - Zhang, Guanghui

AU - LiBretto, Nicole

AU - Purdy, Stephen

AU - Cesar, Laryssa

AU - Miller, Jeffrey

PY - 2023

Y1 - 2023

N2 - In catalysis since reactions occur on the surface of nanoparticles (NP), it is essential to determine the composition of this structure, rather than that of the nanoparticles, since the two may be, and often are, different. Conventional techniques including X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are powerful techniques, but these data reflect the average composition of the entire particle. In this chapter, we introduce the method of EXAFS analysis, which isolates the surface atoms of nanoparticles based on its sensitivity to chemical reactions, specifically surface oxidation. As shown in our case studies, if the surface of a Pt-based nanoparticle is contacted by air at room temperature, the surface will selectively oxidize, resulting in the loss of Pt-Pt and Pt-M bonds to the formation of Pt-O bonds. The difference between the completely reduced and surface-oxidized nanoparticle allows for the isolation of signal from the catalytic surface. Although these examples highlight Pt alloys, similar analysis is also possible for other group 8 and IB bimetallic catalysts.

AB - In catalysis since reactions occur on the surface of nanoparticles (NP), it is essential to determine the composition of this structure, rather than that of the nanoparticles, since the two may be, and often are, different. Conventional techniques including X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are powerful techniques, but these data reflect the average composition of the entire particle. In this chapter, we introduce the method of EXAFS analysis, which isolates the surface atoms of nanoparticles based on its sensitivity to chemical reactions, specifically surface oxidation. As shown in our case studies, if the surface of a Pt-based nanoparticle is contacted by air at room temperature, the surface will selectively oxidize, resulting in the loss of Pt-Pt and Pt-M bonds to the formation of Pt-O bonds. The difference between the completely reduced and surface-oxidized nanoparticle allows for the isolation of signal from the catalytic surface. Although these examples highlight Pt alloys, similar analysis is also possible for other group 8 and IB bimetallic catalysts.

KW - Intermetallic alloy

KW - Propane dehydrogenation

KW - Pt alloy catalysts

KW - Resonant inelastic X-ray scattering

KW - Surface structure

KW - Surface-sensitive X-ray absorption

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X-Ray Absorption Spectroscopy (XAS): Surface Structural Determination of Alloy Nanoparticles

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