Special Issue "Advanced Synchrotron Radiation Techniques for Nanostructured Materials"

A special issue of Nanomaterials (ISSN 2079-4991).

Deadline for manuscript submissions: closed (31 March 2019).

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editor

Prof. Chiara Battocchio
Website
Guest Editor
Department of Science, Roma Tre University, 00146 Roma, Italy
Interests: molecular and electronic structure of nanostructured materials carried out by state-of-the-art Synchrotron Radiation (SR)-induced techniques such as X-ray Photoelectron Spectroscopy (SR-XPS), X-ray Absorption Spectroscopy (XAS), and Near-Edge X-ray Absorption Fine Structure spectroscopy (NEXAFS), as well as conventional XPS, UV–visible absorption and emission and FT-IR spectroscopies. Main topics of research are metal nanoparticles stabilized by organic molecules and biomolecules for technological applications and biocompatible materials for tissue engineering applications
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Special Issue Information

Dear Colleagues,

Nanostructured materials exploit physical phenomena and mechanisms that cannot be derived by simply scaling down the associated bulk structures and phenomena; furthermore, new quantum effects come into play in nanosystems. The exploitation of these emerging nanoscale interactions prompts the innovative design of nanomaterials.

Understanding the behavior of materials on all length scales, from the nanostructure up to the macroscopic response, is a critical challenge for materials science. Modern analytical technologies based on Synchrotron Radiation (SR) allow the non-destructive investigation of the chemical, electronic, and magnetic structure of materials in any environment. SR facilities have developed revolutionary new ideas and experimental set-ups to characterize nanomaterials, involving spectroscopy, diffraction, scatterings, microscopy, tomography, and all kinds of highly sophisticated combinations of such investigation techniques.

This Special Issue seeks to cover all aspects of Synchrotron Radiation applied to the investigation of chemical, electronic, and magnetic structure of nanostructured materials.

Prof. Chiara Battocchio
Guest Editor

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Keywords

  • Synchrotron Radiation techniques
  • Synchrotron Radiation-induced spectroscopies
  • X-ray absorption spectroscopy
  • X-ray photoelectron spectroscopy
  • X-ray diffraction
  • Nanostructured materials
  • Molecular structure of nanomaterials
  • Magnetic structure of nanomaterials
  • Electronic structure of nanomaterials

Published Papers (9 papers)

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Editorial

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Open AccessEditorial
Advanced Synchrotron Radiation Techniques for Nanostructured Materials
Nanomaterials 2019, 9(9), 1279; https://doi.org/10.3390/nano9091279 - 07 Sep 2019
Abstract
Nanostructured materials exploit physical phenomena and mechanisms that cannot be derived by simply scaling down the associated bulk structures and behaviors; furthermore, new quantum effects come into play in nanosystems [...] Full article

Research

Jump to: Editorial

Open AccessArticle
Extracting the Dynamic Magnetic Contrast in Time-Resolved X-Ray Transmission Microscopy
Nanomaterials 2019, 9(7), 940; https://doi.org/10.3390/nano9070940 - 28 Jun 2019
Cited by 2
Abstract
Using a time-resolved detection scheme in scanning transmission X-ray microscopy (STXM), we measured element resolved ferromagnetic resonance (FMR) at microwave frequencies up to 10 GHz and a spatial resolution down to 20 nm at two different synchrotrons. We present different methods to separate [...] Read more.
Using a time-resolved detection scheme in scanning transmission X-ray microscopy (STXM), we measured element resolved ferromagnetic resonance (FMR) at microwave frequencies up to 10 GHz and a spatial resolution down to 20 nm at two different synchrotrons. We present different methods to separate the contribution of the background from the dynamic magnetic contrast based on the X-ray magnetic circular dichroism (XMCD) effect. The relative phase between the GHz microwave excitation and the X-ray pulses generated by the synchrotron, as well as the opening angle of the precession at FMR can be quantified. A detailed analysis for homogeneous and inhomogeneous magnetic excitations demonstrates that the dynamic contrast indeed behaves as the usual XMCD effect. The dynamic magnetic contrast in time-resolved STXM has the potential be a powerful tool to study the linear and nonlinear, magnetic excitations in magnetic micro- and nano-structures with unique spatial-temporal resolution in combination with element selectivity. Full article
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Open AccessArticle
Elemental Distribution and Structural Characterization of GaN/InGaN Core-Shell Single Nanowires by Hard X-ray Synchrotron Nanoprobes
Nanomaterials 2019, 9(5), 691; https://doi.org/10.3390/nano9050691 - 03 May 2019
Cited by 1
Abstract
Improvements in the spatial resolution of synchrotron-based X-ray probes have reached the nano-scale and they, nowadays, constitute a powerful platform for the study of semiconductor nanostructures and nanodevices that provides high sensitivity without destroying the material. Three complementary hard X-ray synchrotron techniques at [...] Read more.
Improvements in the spatial resolution of synchrotron-based X-ray probes have reached the nano-scale and they, nowadays, constitute a powerful platform for the study of semiconductor nanostructures and nanodevices that provides high sensitivity without destroying the material. Three complementary hard X-ray synchrotron techniques at the nanoscale have been applied to the study of individual nanowires (NWs) containing non-polar GaN/InGaN multi-quantum-wells. The trace elemental sensitivity of X-ray fluorescence allows one to determine the In concentration of the quantum wells and their inhomogeneities along the NW. It is also possible to rule out any contamination from the gold nanoparticle catalyst employed during the NW growth. X-ray diffraction and X-ray absorption near edge-structure probe long- and short-range order, respectively, and lead us to the conclusion that while the GaN core and barriers are fully relaxed, there is an induced strain in InGaN layers corresponding to a perfect lattice matching with the GaN core. The photoluminescence spectrum of non-polar InGaN quntum wells is affected by strain and the inhomogeneous alloy distribution but still exhibits a reasonable 20% relative internal quantum efficiency. Full article
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Open AccessArticle
Direct Spectroscopy for Probing the Critical Role of Partial Covalency in Oxygen Reduction Reaction for Cobalt-Manganese Spinel Oxides
Nanomaterials 2019, 9(4), 577; https://doi.org/10.3390/nano9040577 - 09 Apr 2019
Cited by 1
Abstract
Nanocrystalline multivalent metal spinels are considered as attractive non-precious oxygen electrocatalysts. Identifying their active sites and understanding their reaction mechanisms are essential to explore novel transition metal (TM) oxides catalysts and further promote their catalytic efficiency. Here we report a systematic investigation, by [...] Read more.
Nanocrystalline multivalent metal spinels are considered as attractive non-precious oxygen electrocatalysts. Identifying their active sites and understanding their reaction mechanisms are essential to explore novel transition metal (TM) oxides catalysts and further promote their catalytic efficiency. Here we report a systematic investigation, by means of soft X-ray absorption spectroscopy (sXAS), on cubic and tetragonal CoxMn3-xO4 (x = 1, 1.5, 2) spinel oxides as a family of highly active catalysts for the oxygen reduction reaction (ORR). We demonstrate that the ORR activity for oxide catalysts primarily correlates to the partial covalency of between O 2p orbital with Mn4+ 3d t2g-down/eg-up, Mn3+ 3d eg-up and Co3+ 3d eg-up orbitals in octahedron, which is directly revealed by the O K-edge sXAS. Our findings propose the critical influences of the partial covalency between oxygen 2p band and specific metal 3d band on the competition between intermediates displacement of the ORR, and thus highlight the importance of electronic structure in controlling oxide catalytic activity. Full article
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Open AccessArticle
Microscopic Views of Atomic and Molecular Oxygen Bonding with epi Ge(001)-2 × 1 Studied by High-Resolution Synchrotron Radiation Photoemission
Nanomaterials 2019, 9(4), 554; https://doi.org/10.3390/nano9040554 - 04 Apr 2019
Cited by 1
Abstract
In this paper, we investigate the embryonic stage of oxidation of an epi Ge(001)-2 × 1 by atomic oxygen and molecular O2 via synchrotron radiation photoemission. The topmost buckled surface with the up- and down-dimer atoms, and the first subsurface layer behaves [...] Read more.
In this paper, we investigate the embryonic stage of oxidation of an epi Ge(001)-2 × 1 by atomic oxygen and molecular O2 via synchrotron radiation photoemission. The topmost buckled surface with the up- and down-dimer atoms, and the first subsurface layer behaves distinctly from the bulk by exhibiting surface core-level shifts in the Ge 3d core-level spectrum. The O2 molecules become dissociated upon reaching the epi Ge(001)-2 × 1 surface. One of the O atoms removes the up-dimer atom and the other bonds with the underneath Ge atom in the subsurface layer. Atomic oxygen preferentially adsorbed on the epi Ge(001)-2 ×1 in between the up-dimer atoms and the underneath subsurface atoms, without affecting the down-dimer atoms. The electronic environment of the O-affiliated Ge up-dimer atoms becomes similar to that of the down-dimer atoms. They both exhibit an enrichment in charge, where the subsurface of the Ge layer is maintained in a charge-deficient state. The dipole moment that was originally generated in the buckled reconstruction no longer exists, thereby resulting in a decrease in the ionization potential. The down-dimer Ge atoms and the back-bonded subsurface atoms remain inert to atomic O and molecular O2, which might account for the low reliability in the Ge-related metal-oxide-semiconductor (MOS) devices. Full article
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Open AccessArticle
On the Formation of Nanocrystalline Grains in Metallic Glasses by Means of In-Situ Nuclear Forward Scattering of Synchrotron Radiation
Nanomaterials 2019, 9(4), 544; https://doi.org/10.3390/nano9040544 - 04 Apr 2019
Cited by 1
Abstract
Application of the so-called nuclear forward scattering (NFS) of synchrotron radiation is presented for the study of crystallization of metallic glasses. In this process, nanocrystalline alloys are formed. Using NFS, the transformation process can be directly observed during in-situ temperature experiments not only [...] Read more.
Application of the so-called nuclear forward scattering (NFS) of synchrotron radiation is presented for the study of crystallization of metallic glasses. In this process, nanocrystalline alloys are formed. Using NFS, the transformation process can be directly observed during in-situ temperature experiments not only from the structural point of view, i.e., formation of nanocrystalline grains, but one can also observe evolution of the corresponding hyperfine interactions. In doing so, we have revealed the influence of external magnetic field on the crystallization process. The applied magnetic field is not only responsible for an increase of hyperfine magnetic fields within the newly formed nanograins but also the corresponding components in the NFS time spectra are better identified via occurrence of quantum beats with higher frequencies. In order to distinguish between these two effects, simulated and experimental NFS time spectra obtained during in-situ temperature measurements with and without external magnetic field are compared. Full article
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Open AccessArticle
Structural and Thermal Characterisation of Nanofilms by Time-Resolved X-ray Scattering
Nanomaterials 2019, 9(4), 501; https://doi.org/10.3390/nano9040501 - 01 Apr 2019
Cited by 2
Abstract
High time resolution in scattering analysis of thin films allows for determination of thermal conductivity by transient pump-probe detection of dissipation of laser-induced heating, TDXTS. We describe an approach that analyses the picosecond-resolved lattice parameter reaction of a gold transducer layer on pulsed [...] Read more.
High time resolution in scattering analysis of thin films allows for determination of thermal conductivity by transient pump-probe detection of dissipation of laser-induced heating, TDXTS. We describe an approach that analyses the picosecond-resolved lattice parameter reaction of a gold transducer layer on pulsed laser heating to determine the thermal conductivity of layered structures below the transducer. A detailed modeling of the cooling kinetics by a Laplace-domain approach allows for discerning effects of conductivity and thermal interface resistance as well as basic depth information. The thermal expansion of the clamped gold film can be calibrated to absolute temperature change and effects of plastic deformation are discriminated. The method is demonstrated on two extreme examples of phononic barriers, isotopically modulated silicon multilayers with very small acoustic impedance mismatch and silicon-molybdenum multilayers, which show a high resistivity. Full article
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Open AccessArticle
In Situ X-ray Photoelectron Spectroscopic and Electrochemical Studies of the Bromide Anions Dissolved in 1-Ethyl-3-Methyl Imidazolium Tetrafluoroborate
Nanomaterials 2019, 9(2), 304; https://doi.org/10.3390/nano9020304 - 22 Feb 2019
Cited by 3
Abstract
Influence of electrode potential on the electrochemical behavior of a 1-ethyl-3-methylimidazolium tetrafluoroborate (EMImBF4) solution containing 5 wt % 1-ethyl-3-methylimidazolium bromide (EMImBr) has been investigated using electrochemical and synchrotron-initiated high-resolution in situ X-ray photoelectron spectroscopy (XPS) methods. Observation of the Br 3d [...] Read more.
Influence of electrode potential on the electrochemical behavior of a 1-ethyl-3-methylimidazolium tetrafluoroborate (EMImBF4) solution containing 5 wt % 1-ethyl-3-methylimidazolium bromide (EMImBr) has been investigated using electrochemical and synchrotron-initiated high-resolution in situ X-ray photoelectron spectroscopy (XPS) methods. Observation of the Br 3d5/2 in situ XPS signal, collected in a 5 wt % EMImBr solution at an EMImBF4–vacuum interface, enabled the detection of the start of the electrooxidation process of the Br anion to Br3 anion and thereafter to the Br2 at the micro-mesoporous carbon electrode, polarized continuously at the high fixed positive potentials. A new photoelectron peak, corresponding to B–O bond formation in the B 1s in situ XPS spectra at E ≤ −1.17 V, parallel to the start of the electroreduction of the residual water at the micro-mesoporous carbon electrode, was observed and is discussed. The electroreduction of the residual water caused a reduction in the absolute value of binding energy vs. potential plot slope twice to ca. dBE dE−1 = −0.5 eV V−1 at E ≤ −1.17 V for C 1s, N 1s, B 1s, F 1s, and Br 3d5/2 photoelectrons. Full article
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Open AccessFeature PaperArticle
Biocompatible Materials Based on Self-Assembling Peptides on Ti25Nb10Zr Alloy: Molecular Structure and Organization Investigated by Synchrotron Radiation Induced Techniques
Nanomaterials 2018, 8(3), 148; https://doi.org/10.3390/nano8030148 - 07 Mar 2018
Cited by 5
Abstract
In this work, we applied advanced Synchrotron Radiation (SR) induced techniques to the study of the chemisorption of the Self Assembling Peptide EAbuK16, i.e., H-Abu-Glu-Abu-Glu-Abu-Lys-Abu-Lys-Abu-Glu-Abu-Glu-Abu-Lys-Abu-Lys-NH2 that is able to spontaneously aggregate in anti-parallel β-sheet conformation, onto annealed Ti25Nb10Zr alloy surfaces. This synthetic [...] Read more.
In this work, we applied advanced Synchrotron Radiation (SR) induced techniques to the study of the chemisorption of the Self Assembling Peptide EAbuK16, i.e., H-Abu-Glu-Abu-Glu-Abu-Lys-Abu-Lys-Abu-Glu-Abu-Glu-Abu-Lys-Abu-Lys-NH2 that is able to spontaneously aggregate in anti-parallel β-sheet conformation, onto annealed Ti25Nb10Zr alloy surfaces. This synthetic amphiphilic oligopeptide is a good candidate to mimic extracellular matrix for bone prosthesis, since its β-sheets stack onto each other in a multilayer oriented nanostructure with internal pores of 5–200 nm size. To prepare the biomimetic material, Ti25Nb10Zr discs were treated with aqueous solutions of EAbuK16 at different pH values. Here we present the results achieved by performing SR-induced X-ray Photoelectron Spectroscopy (SR-XPS), angle-dependent Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy, FESEM and AFM imaging on Ti25Nb10Zr discs after incubation with self-assembling peptide solution at five different pH values, selected deliberately to investigate the best conditions for peptide immobilization. Full article
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