Publications by authors named "Luca Gregoratti"

A Scanning Photoelectron Microscopy (SPEM) experiment has been applied to ZnO:N films deposited by Atomic Layer Deposition (ALD) under O-rich conditions and post-growth annealed in oxygen at 800 °C. spatial resolution (130 nm) allows for probing the electronic structure of single column of growth. The samples were cleaved under ultra-high vacuum (UHV) conditions to open atomically clean cross-sectional areas for SPEM experiment.

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Here a sealing-style x-ray photoelectron spectroscopy study of the surface of a 1.0 wt. %Ni/TiO2 nanoparticle catalyst in a flowing mixture of CO and O2 at 1 bar was performed with a graphene membrane-sealed Si3N4 window-based miniature cell.

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Bipolar plates, a critical component of proton exchange membrane fuel cell (PEMFC), are constructed out of alloys of Ti, Pt, Cr, or graphitic materials that have limitations. Electrical conductivity, cost, and corrosion resistance are among the critical considerations for bi-polar plate material. Graphene, which possesses impressive conductivity and toughness, is an attractive option as coating on metallic substrates of PEMFC bipolar plates.

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Graphene coatings developed by chemical vapor deposition (CVD) that possess extraordinary/unique characteristics as barrier against aggressive environment can improve the corrosion resistance of Ni and Cu by up to two orders of magnitude. However, because of some compelling technical reasons, it has thus far been a nontrivial challenge to develop graphene coatings on the most commonly used engineering alloy, mild steel (MS). To circumvent the challenge simply by first electroplating MS with a Ni layer is attempted, and then developing CVD graphene over the Ni layer.

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Article Synopsis
  • - The study examines how different materials (Rh, Au, and ZrO) affect the catalytic behavior of Rh particles during hydrogen (H) oxidation using advanced microscopy techniques (PEEM and SPEM).
  • - Researchers found that the catalytic activity varied based on the support material and the size of Rh particles, with unique oscillation behaviors observed: independent with Rh/Rh, dependent with Rh/ZrO, and fully inhibited with Rh/Au.
  • - Micro-kinetic simulations helped explain the results, showing how the local structure and composition influence catalytic performance, highlighting the importance of in situ surface microscopy.
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Improvements in sodium intercalation in sodium cathodes have been debated in recent years. In the present work, we delineate the significant effect of the carbon nanotubes (CNTs) and their weight percent in the intercalation capacity of the binder-free manganese vanadium oxide (MVO)-CNTs composite electrodes. The performance modification of the electrode is discussed taking into account the cathode electrolyte interphase (CEI) layer under optimal performance.

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Understanding the chemical and electronic properties of point defects in two-dimensional materials, as well as their generation and passivation, is essential for the development of functional systems, spanning from next-generation optoelectronic devices to advanced catalysis. Here, we use synchrotron-based X-ray photoelectron spectroscopy (XPS) with submicron spatial resolution to create sulfur vacancies (SVs) in monolayer MoS and monitor their chemical and electronic properties during the defect creation process. X-ray irradiation leads to the emergence of a distinct Mo 3d spectral feature associated with undercoordinated Mo atoms.

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Magnetic topological insulators (MTIs) have recently become a subject of poignant interest; among them, Z topological insulators with magnetic moment ordering caused by embedded magnetic atoms attract special attention. In such systems, the case of magnetic anisotropy perpendicular to the surface that holds a topologically nontrivial surface state is the most intriguing one. Such materials demonstrate the quantum anomalous Hall effect, which manifests itself as chiral edge conduction channels that can be manipulated by switching the polarization of magnetic domains.

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Herein, we report the microscopic and spectroscopic signatures of the hydrated VO phase, prepared from the α-VO powder, which was kept in deionized water inside an airtight glass container for approximately 2.5 years. The experimental results show an evolution of the V component in V 2p core energy level spectra, and a peak corresponding to σ-OH bond appeared in the valence band spectra in the hydrated VO powder sample due to the water intercalation.

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Article Synopsis
  • - GeTe, a semiconductor with ferroelectric properties, is attracting attention due to its unique giant Rashba splitting and diverse applications, including thermoelectric devices and data storage.
  • - The study investigates how the GeTe (111) surface reacts with oxygen, focusing on reaction kinetics using techniques like NAP XPS and exploring the resulting oxide layer's structure.
  • - Findings reveal nanoscale phase separation of GeO and Te in the oxide layer, which is atypical for semiconductors and may be linked to GeTe's ferroelectric behavior and domain structure.
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We investigate the oxidation mechanism of the layered model system GeAs. X-ray photoelectron spectroscopy experiments performed by irradiating an individual flake with synchrotron radiation in the presence of oxygen show that while As leaves the GeAs surface upon oxidation, a Ge-rich ultrathin oxide film is being formed in the topmost layer of the flake. We develop a theoretical model that supports the layer-by-layer oxidation of GeAs, with a logarithmic kinetics.

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Hybrid inorganic/organic heterointerfaces are promising systems for next-generation photocatalytic, photovoltaic, and chemical-sensing applications. Their performance relies strongly on the development of robust and reliable surface passivation and functionalization protocols with (sub)molecular control. The structure, stability, and chemistry of the semiconductor surface determine the functionality of the hybrid assembly.

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Graphene coating on the cobalt-chromium alloy was optimized and successfully carried out by a cold-wall chemical vapor deposition (CW-CVD) method. A uniform layer of graphene for a large area of the Co-Cr alloy (discs of 10 mm diameter) was confirmed by Raman mapping coated area and analyzing specific G and 2D bands; in particular, the intensity ratio and the number of layers were calculated. The effect of the CW-CVD process on the microstructure and the morphology of the Co-Cr surface was investigated by scanning X-ray photoelectron microscope (SPEM), atomic force microscopy (AFM), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS).

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Renewed interest in the ferroelectric semiconductor germanium telluride was recently triggered by the direct observation of a giant Rashba effect and a 30-year-old dream about a functional spin field-effect transistor. In this respect, all-electrical control of the spin texture in this material in combination with ferroelectric properties at the nanoscale would create advanced functionalities in spintronics and data information processing. Here, we investigate the atomic and electronic properties of GeTe bulk single crystals and their (111) surfaces.

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We combine spatially resolved scanning photoelectron spectroscopy with confocal Raman and optical microscopy to reveal how the oxidation of the buried graphene-Cu interface relates to the Cu crystallographic orientation. We analyze over 100 different graphene covered Cu (high and low index) orientations exposed to air for 2 years. Four general oxidation modes are observed that can be mapped as regions onto the polar plot of Cu surface orientations.

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Multiphoton polymer cross-linking evolves as the core process behind high-resolution additive microfabrication with soft materials for implantable/wearable electronics, tissue engineering, microrobotics, biosensing, drug delivery, Electrons and soft X-rays, in principle, can offer even higher resolution and printing rates. However, these powerful lithographic tools are difficult to apply to vacuum incompatible liquid precursor solutions used in continuous additive fabrication. In this work, using biocompatible hydrogel as a model soft material, we demonstrate high-resolution in-liquid polymer cross-linking using scanning electron and X-ray microscopes.

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How a catalyst behaves microscopically under reaction conditions, and what kinds of active sites transiently exist on its surface, is still very much a mystery to the scientific community. Here we present an in situ study on the red-ox behaviour of copper in the model reaction of hydrogen oxidation. Direct imaging combined with on-line mass spectroscopy shows that activity emerges near a phase boundary, where complex spatio-temporal dynamics are induced by the competing action of simultaneously present oxidizing and reducing agents.

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We present an in-depth analysis of the surface band alignment and local potential distribution of InP nanowires containing a p-n junction using scanning probe and photoelectron microscopy techniques. The depletion region is localized to a 15 nm thin surface region by scanning tunneling spectroscopy and an electronic shift of up to 0.5 eV between the n- and p-doped nanowire segments was observed and confirmed by Kelvin probe force microscopy.

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Element clustering and structural features of liquid lead-bismuth eutectic (LBE) alloy have been investigated up to 720 °C by means of high temperature X-ray diffraction (HT-XRD), X-ray Photoemission Spectroscopy (XPS) and Scanning Photoemission Microscopy (SPEM) at the Elettra synchrotron in Trieste. The short-range order in liquid metal after melting corresponds to the cuboctahedral atomic arrangement and progressively evolves towards the icosahedral one as temperature increases. Such process, that involve a negative expansion of the alloy, is mainly connected to the reduction of atom distance in Pb-Pb pairs which takes place from 350 °C to 520 °C.

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We performed spatially resolved near-ambient-pressure photoemission spectromicroscopy on graphene-coated copper in operando under oxidation conditions in an oxygen atmosphere (0.1 mbar). We investigated regions with bare copper and areas covered with mono- and bi-layer graphene flakes, in isobaric and isothermal experiments.

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Studying surface of catalyst nanoparticles in a flowing liquid is important for understanding the underlying mechanism of a reaction performed in liquid. We report the design of a reaction cell system of Si3N4 window covering the flowing liquid with an electron-transmissible membrane. By using metal nanoparticles as a catalyst dispersed in a solvent, examination of the surface of catalyst nanoparticles in a flowing liquid was demonstrated by observation of Ag 3d photoemission feature when a liquid containing Ag nanoparticles was flowing through this system.

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For nanoparticles active for chemical and energy transformations in static liquid environment, chemistries of surface or near-surface regions of these catalyst nanoparticles in liquid are crucial for fundamentally understanding their catalytic performances at a molecular level. Compared to catalysis at a solid-gas interface, there is very limited information on the surface of these catalyst nanoparticles under a working condition or during catalysis in liquid. Photoelectron spectroscopy is a surface-sensitive technique; however, it is challenging to study the surfaces of catalyst nanoparticles dispersed in static liquid because of the short inelastic mean free path of photoelectrons traveling in liquid.

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Chemical waves in the H + O reaction on a Rh(111) surface alloyed with Ni [Θ < 1.5 monolayers (ML)] have been investigated in the 10 and 10 mbar range at T = 773 K using scanning photoelectron microscopy and x-ray photoelectron spectroscopy as in situ methods. The local intensity variations of the O 1s and the Ni 2p signal display an anticorrelated behavior.

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