<i>In Situ</i>Mössbauer Spectroscopy With Synchrotron Radiation on Thin Films

Stankov, S.; Ślęzak, T.; Zając, M.; Ślęzak, M.; Sladecek, M.; Röhlsberger, Ralf; Sepioł, B.; Vogl, G.; Spiridis, N.; Łażewski, J.; Parliński, K.; Korecki, J.

doi:10.1002/9781118714614.ch01

Cited by 4 publications

(5 citation statements)

References 109 publications

(106 reference statements)

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“…Thus, the electronic contribution to the refractive index has only a weak dependence on the x-ray energy. For the case of 2 L -pole transition, the resonant scattering amplitude is given by [45] …”

Section: Nrr Studymentioning

confidence: 99%

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

Sharma

Gupta

et al. 2015

Phys. Rev. B

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Growth of magnetron sputtered Fe films on clean single crystalline MgO (001) substrate has been studied using in situ grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence nuclear resonant scattering (GINRS) measurements. While GISAXS provides information about morphological changes, GINRS provides information about structural and magnetic properties, thus making it possible to correlate the evolution of magnetic properties with that of morphology and structure of the film. The film exhibits a Volmer-Weber type growth, with percolation transition occurring around 2 nm film thickness. Presence of a finite quadrupole splitting, as seen in GINRS measurements, suggests a significant distortion from cubic symmetry up to a film thickness of 3.5 nm, which can be attributed to hybridization between Fe 3d and O 2p orbitals at the interface as well as in-plane tensile strain induced as a result of coalescence of islands. Initially Fe islands exhibit superparamagnetic relaxation, while finite magnetic moment appears upon formation of macroscopic percolation islands. The film exhibits a weak perpendicular magnetic anisotropy (PMA), which vanishes concurrently with disappearance of structural distortion, suggesting that the observed PMA at least partly originates from inherent strain in the film. No presence of any known oxide of Fe was detected at the interface. More precise information about topological and magnetic structure of the interfaces between Fe and MgO layers is obtained using combined x-ray reflectivity and nuclear resonance reflectivity measurements on a 57 Fe/MgO multilayer. Measurements show that about two monolayers of Fe at the interface have a reduced hyperfine field, providing evidence for hybridization with O atoms, as predicted by theory.

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Section: Nrr Studymentioning

confidence: 99%

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

Sharma

Gupta

et al. 2015

Phys. Rev. B

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“…In the presence of more than one discrete resonance transition, the exciton decay leads to a characteristic interference profile in the time domain which is caused by quantum mechanical interference of the coherently emitted photons. 44 The interference pattern, referred to as quantum beats, reflects the energetic differences between the resonance transitions in the time domain. 46,47 An electric quadrupole interaction (Figure 1b) shows two absorption lines (doublet) in MS and periodic quantum beats in NFS (Figure 1e,h).…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…These pulses are absorbed in the sample by the Fe-57 nuclei, which brings them to the excited state indiscriminate of their chemical environment. Due to the short pulse compared to the nuclear lifetime of the excited I e = 3/2 state in Fe-57, a nuclear exciton (coherent superposition of excited states over the resonant atoms) is formed . Consecutively, prior to the next pulse, the decay mode of the delayed forward scattered photons is measured in the time domain while the nuclei return to their ground states .…”

Section: Resultsmentioning

confidence: 99%

“…Due to the short pulse compared to the nuclear lifetime of the excited I e = 3/2 state in Fe-57, a nuclear exciton (coherent superposition of excited states over the resonant atoms) is formed. 44 Consecutively, prior to the next pulse, the decay mode of the delayed forward scattered photons is measured in the time domain while the nuclei return to their ground states. 45 The case of only an electric monopole interaction is shown in Figure 1d that gives a continuous decay in NFS.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…The case of only an electric monopole interaction is shown in Figure d that gives a continuous decay in NFS. In the presence of more than one discrete resonance transition, the exciton decay leads to a characteristic interference profile in the time domain which is caused by quantum mechanical interference of the coherently emitted photons . The interference pattern, referred to as quantum beats, reflects the energetic differences between the resonance transitions in the time domain. , …”

Section: Resultsmentioning

confidence: 99%

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Applying Nuclear Forward Scattering as In Situ and Operando Tool for the Characterization of FeN₄ Moieties in the Hydrogen Evolution Reaction

Heppe,

Gallenkamp,

Snitkoff-Sol

et al. 2024

J. Am. Chem. Soc.

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Nuclear forward scattering (NFS) is a synchrotronbased technique relying on the recoil-free nuclear resonance effect similar to Mossbauer spectroscopy. In this work, we introduce NFS for in situ and operando measurements during electrocatalytic reactions. The technique enables faster data acquisition and better discrimination of certain iron sites in comparison to Mossbauer spectroscopy. It is directly accessible at various synchrotrons to a broad community of researchers and is applicable to multiple metal isotopes. We demonstrate the power of this technique with the hydrogen evolution mechanism of an immobilized iron porphyrin supported on carbon. Such catalysts are often considered as model systems for iron−nitrogen-carbon (FeNC) catalysts. Using in situ and operando NFS in combination with theoretical predictions of spectroscopic data enables the identification of the intermediate that is formed prior to the rate-determining step. The conclusions on the reaction mechanism can be used for future optimization of immobilized molecular catalysts and metal−nitrogen−carbon (MNC) catalysts.

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Characterization of Supported Metal Single‐Atom Catalysts

Zhang¹,

Doyle‐Davis

Sun

2022

Supported Metal Single Atom Catalysis

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In SituMössbauer Spectroscopy With Synchrotron Radiation on Thin Films

Cited by 4 publications

References 109 publications

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

Applying Nuclear Forward Scattering as In Situ and Operando Tool for the Characterization of FeN₄ Moieties in the Hydrogen Evolution Reaction

Characterization of Supported Metal Single‐Atom Catalysts

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In SituMössbauer Spectroscopy With Synchrotron Radiation on Thin Films

Cited by 4 publications

References 109 publications

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

In situsmall-angle x-ray and nuclear resonant scattering study of the evolution of structural and magnetic properties of an Fe thin film on MgO (001)

Applying Nuclear Forward Scattering as In Situ and Operando Tool for the Characterization of FeN4 Moieties in the Hydrogen Evolution Reaction

Characterization of Supported Metal Single‐Atom Catalysts

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Product

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Applying Nuclear Forward Scattering as In Situ and Operando Tool for the Characterization of FeN₄ Moieties in the Hydrogen Evolution Reaction