Search Results

You searched for all publications:

with publication states 'Published (Approved)'

Search Again...

These results only include publications that have been reviewed and processed by Diamond Light Source. To also view papers that have not yet been processed click here.

You can use the folder icon under Actions to collate papers as required. You can then click on View Folder in the left-hand navigation to review and/or download your folder.

Exact matches
Related results

13 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2 [Next/Last]

Instruments / Technical Area	Publication Details	Published
	Synchrotron-based x-ray photoelectron microscopy of LMO/LAGP/Cu thin-film solid-state lithium metal batteries Majid Kazemian , Matteo Amati , Luca Gregoratti , Maya Kiskinova , Benedetto Bozzini Batteries 9 DOI: 10.3390/batteries9100506 Open Access Show Abstract ▼ Abstract: Solid-state batteries (SSB), characterized by solid-state electrolytes—in particular inorganic ones (ISSE)—are an ideal option for the safe implementation of metallic Li anodes. Even though SSBs with ISSEs have been extensively investigated over the last two decades, they still exhibit a series of technological drawbacks. In fact, mechano-chemical issues, mainly the stability of the electrolyte/anode interface, hinder their widespread application. The present investigation focusses on a thin-film LMO (Lithium-Manganese-Oxide)/LAGP (LiAlGe Phosphate)/Copper, anodeless Lithium-metal battery and explores the morphochemical evolution of the electrode/electrolyte interfaces with synchrotron-based Scanning Photoelectron Microscopy (SPEM) of intact pristine and cycled cells. Chemical images were acquired with submicrometer resolution, to highlight the coupled geometrical and chemical-state changes caused by electrochemical ageing. Geometrical changes of the electrolyte/cathode interface were induced by periodic volume changes, causing de-cohesion of the solid-solid contact, but no chemical-state changes accompany the cathodic damaging mode. Instead, shape changes of the electrolyte/anode region pinpoint the correlation between mechanical damaging with the decomposition of the LAGP ISSE, due to the reduction of Ge, triggered by the contact with elemental Li. The micro-spectroscopic approach adopted in this study enabled the assessment of the highly localized nature of the cathodic and anodic degradation modes in SSB devices and to single out the chemical and mechanical contributions.	Oct 2023
	Operando photoelectron spectromicroscopy of nanodevices: correlating the surface chemistry and transport in SnO2 nanowire chemiresistors Andrei Kolmakov , J. Trey Diulus , Kurt D. Benkstein , Steve Semancik , Majid Kazemian , Matteo Amati , Maya Kiskinova , Luca Gregoratti Journal Of Electron Spectroscopy And Related Phenomena 257 DOI: 10.1016/j.elspec.2023.147366 Show Abstract ▼ Abstract: With size reduction of active elements in microelectronics to tens of nanometers and below, the effect of surface and interface properties on overall device performance becomes crucial. High resolution spectroscopic and imaging techniques provide a metrological route for characterization of these properties relevant to device diagnostics and failure analysis. With its roughly 100 nm spatial resolution, superior surface sensitivity, and approximately 200 meV spectral resolution, scanning photoelectron microscopy (SPEM) stands out as a comprehensive tool to access the surface/interface composition of nanodevices, as well to provide chemical state designations and materials property evolutions upon treatment by thermal, electrical, chemical, radiative and other stimuli. Here we present a SPEM-on-device setup that combines X-ray spectromicroscopy with advanced NIST microhotplate technology to demonstrate new combined analytical and electrical measurements capabilities of this metrology platform for operando nanodevice characterization. Using model integrated SnO2 nanowire (NW) chemiresistor devices, the chemically induced alterations in the chemical state of the nanowire surface are correlated to the observed conductance changes, thus directly testing the receptor and transduction mechanisms for SnO2 NW conductometric chemical sensors.	Jun 2023
I08-Scanning X-ray Microscopy beamline (SXM)	X-ray absorption spectromicroscopy gives access to Li1+xAlxGe2−x(PO4)3 (LAGP) local degradation at the anode-electrolyte interface Majid Kazemian , Maya Kiskinova , Benedetto Bozzini Journal Of Power Sources Advances 17-18 DOI: 10.1016/j.powera.2022.100106 Diamond Proposal Number(s): [26226] Open Access Show Abstract ▼ Abstract: Batteries with inorganic solid-state electrolytes (ISSE) are attracting notable interest for next-generation systems implementing Lithium (Li) metal anodes, in view of achieving higher energy densities combined with superior safety. Notwithstanding extensive research and development work, this technology is not yet ready for industrial implementation, one of the key challenges being the stability of ISSEs, chiefly at the anodic interface. This work attacks this issue for the specific case of the LAGP/Li (Lithium Aluminium Germanium Phosphate/Lithium) interface with a micro-spectroscopic approach centred on post mortem Scanning Transmission X-ray Microscopy (STXM) of intact LMO/LAGP/Li thin-film batteries, microfabricated in discharged state. Pristine and cycled cells were mapped to pinpoint morphochemical changes, induced by electrochemical ageing. The evidenced shape changes, corresponding to mechanical damaging of the solid/solid electrodic interfaces correlate with LAGP decomposition at the anode, leading to reduction of Ge, whereas the chemical state at the cathodic interface is preserved. Thanks to its submicron spacial resolution, the STXM at the Ge L-edge and O K-edge spectra allowed to assess the highly localized nature of the chemical transformation of LAGP and its correlation with the formation of Li outgrowth features.	Nov 2022
I08-1-Soft X-ray Ptychography I08-Scanning X-ray Microscopy beamline (SXM)	X-ray imaging and micro-spectroscopy unravel the role of zincate and zinc oxide in the cycling of zinc anodes in mildly acidic aqueous electrolytes Majid Kazemian , Francesca Rossi , Andrea Casaroli , Tommaso Caielli , Burkhard Kaulich , Maya Kiskinova , Ivonne Sgura , Benedetto Bozzini Journal Of Power Sources 524 DOI: 10.1016/j.jpowsour.2022.231063 Diamond Proposal Number(s): [22398] Open Access Show Abstract ▼ Abstract: Sustainability, environmental and safety concerns raised by the increasing demand of batteries are driving research towards post-lithium technologies. Rechargeable Zn batteries are strong candidates, but still not practically viable, owing to the extensively studied, but poorly understood unstable behavior of Zn metal upon discharge-charge cycling. This limiting factor warrants more fundamental investigations and the present report provides the lacking molecular-level information on the Zn-based compounds forming at the electrode/electrolyte interface as a result of electrochemical cyclic in weakly acidic aqueous electrolyte. The results are obtained using ex situ X-ray absorption spectromicroscopy maps, modelled mathematically and complemented with cyclic voltammetry, symmetric-cell tests and electron microscopy. We have identified the role of the zincate precipitation resulting from local alkalinization during recharge, combined with additional zincate formation and decomposition to zinc oxide during discharge. The mathematical model allowed a transparent interpretation of morphochemical changes observed. The synergy of these processes leads to electrochemical localization effects, resulting in the formation of a complexly structured and low conductive ZnO-based template, that might play a role in driving shape changes.	Mar 2022
	The role of chromium in the corrosion performance of cobalt- and cobalt-nickel based hardmetal binders: A study centred on X-ray absorption microspectroscopy Benedetto Bozzini , Alessandra Gianoncelli , Georgios Kourousias , Marco Boniardi , Andrea Casaroli , Simone Dal Zilio , Rafaqat Hussain , Majid Kazemian Abyaneh , Maya Kiskinova , Claudio Mele , Sandra Tedeschi , Gian Pietro De Gaudenzi International Journal Of Refractory Metals And Hard Materials DOI: 10.1016/j.ijrmhm.2020.105320 Show Abstract ▼ Abstract: The corrosion control of WC-Co type hardmetals is steadily gaining momentum for novel crucial applications in the Oil & Gas and food industries. The corrosion rate of the Co-based binder, and the extent to which coupling to WC speeds it up, are strongly influenced by alloying. In this paper, we investigate the impact of Cr on the corrosion-product film formation of Co- and CoNi based hardmetal binders in acidic, neutral and alkaline aqueous solutions. We centred our study on the role of Cr in driving the distribution of oxidized Co and Ni at the micrometre scale, thanks to synchrotron-based soft-X ray microspectroscopy. We have investigated morphochemical distributions for the following grades: Co96Cr4, Co48Ni48Cr4, Co50Cr50. Chemical-state mapping has been complemented by electrochemical measurements and metallographic observations. Amounts of Cr and Ni of ca. 50% notably increase the corrosion resistance in all ambients, with a stronger beneficial effect of the former element. 4% addition of Cr results in slight positive effects, with the exception of the CoNi system in alkaline ambient, that, together with Co50Cr50, outperforms the other grades. In all investigated alloy-ambient combinations, a continuous oxidized metal film grows, onto which micrometric island form of shape and dimensions that depend on the specific grade and aggressive conditions. Quantitative descriptors of chemical-state maps and their theoretical interpretation in terms of electrochemical phase-formation by oxy-hydroxide precipitation, allow to correlate the island patterns with the degree of pseudopassivation.	Jun 2020
I08-Scanning X-ray Microscopy beamline (SXM)	Operando soft X-ray microscope study of rechargeable Zn-air battery anodes in deep eutectic solvent electrolyte Benedetto Bozzini , Majid Kazemian , Maya Kiskinova , Georgios Kourousias , Claudio Mele , Alessandra Gianoncelli X-Ray Spectrometry 15 DOI: 10.1002/xrs.3031 Diamond Proposal Number(s): [14027] Open Access Show Abstract ▼ Abstract: Zn–air batteries are very promising devices for energy storage at high energy density due to their intrinsic safety, environmental friendliness, and low cost, but still, there are key issues to be solved to get to the industrial scale. One of the unsolved problems is the poor cyclability of batteries based on aqueous solvents that urges to consider nonaqueous solvents. Among different possible options are deep eutectic solvents, which are cost‐effective and technologically relatively easy to implement. The present investigation reports for the first time an operando scanning soft X‐ray microscope analysis of the Zn behaviour in a choline–chloride/urea deep eutectic solvents electrolyte during the cathodic and anodic phase formation processes taking place in battery charge and discharge, providing a platform for in‐depth space–time dependent investigations of the chemistry of crystallites evolving during potential cycling. These operando measurements have been enabled by the construction of a novel wet cell, improving the design and filling protocol of earlier generation cells developed by authors. High‐resolution soft X‐ray microscope images were acquired in two modes: (a) dynamic mode at a fixed beam energy, allowing to follow morphology evolution under electrochemical control and (b) static mode for selected morphologies representative of characteristic Zn growth and dissolution steps.	Mar 2019
	Life science applications and research potential of the TwinMic spectromicroscopy station at ELETTRA A. Gianoncelli , G. Kourousias , L. Pascolo , C. Rizzardi , G. Ceccone , B. Kaulich , M. Kiskinova Journal Of Physics: Conference Series 463 11th International Conference on X-ray Microscopy (XRM2012) DOI: 10.1088/1742-6596/463/1/012004 Open Access Show Abstract ▼ Abstract: Since its opening to the users in late 2007, the TwinMic beamline at the Elettra synchrotron has been attracting the interest of a broad life science community. The recent development and implementation of a low energy x-ray fluorescence detection mode have increased the capability and the versatility of the scanning mode of the TwinMic microscope. Now using simultaneously the x-ray transmission and emission detection systems one can perform elemental, absorption and phase contrast imaging that provides complementary chemical and morphological information for the sample under investigation. The recent achievements in the performance of the instrument using combined acquisition modes for characterization of nano and micro-structured biomaterials will be illustrated with selected exemplary results.	Oct 2013
	New energy sources: in-situ characterisation of fuel cell and supercapacitor components. complementary studies using transmission, fluorescence and photoelectron microscopy and imaging B. Bozzini , M. Amati , A. Gianoncelli , L. Gregoratti , B. Kaulich , M. Kiskinova Journal Of Physics: Conference Series 463 11th International Conference on X-ray Microscopy (XRM2012) DOI: 10.1088/1742-6596/463/1/012018 Open Access Show Abstract ▼ Abstract: Fuel cells and supercapacitors are electrochemical devices providing efficient and pollution-free production and transformation of electricity. Notwithstanding their environmental appeal, a host of materials-science problems – chiefly related to the limited durability of crucial functional components – are hindering their widespread application. The present knowledge of the relevant materials-science notion is mostly at the macroscopic and empirical trial-and-error level and the answers to many questions require much deeper scientific understanding of the origin of degradation processes. In this regard, the development and the implementation of appropriate methods for in-situ characterization of cell components at the functionally relevant length scales is highly required. Soft X-ray spectroscopies, such as X-ray absorption spectroscopy, X-ray emission (fluorescence) spectroscopy, resonant inelastic X-ray spectroscopy and X-ray photoelectron spectroscopy have been extensively employed for ex-situ characterization of materials used in electrochemical systems. Furthermore, adding spatial resolution capabilities by implementing proper optical solutions has opened unique opportunities for monitoring material changes and mass transport events occurring at submicron length scales. The input from these methods is providing correlative information about the status of the electrode surface and of the electrode/electrolyte interface and also of the processes occurring under operation conditions.	Oct 2013
	Direct mapping of 19F in 19FDG-6P in brain tissue at subcellular resolution using soft X-ray fluorescence C. Poitry-Yamate , A. Gianoncelli , G. Kourousias , B. Kaulich , M. Lepore , R. Gruetter , M. Kiskinova Journal Of Physics: Conference Series 463 (1) 11th International Conference on X-ray Microscopy (XRM2012) DOI: 10.1088/1742-6596/463/1/012003 Open Access Show Abstract ▼ Abstract: Low energy x-ray fluorescence (LEXRF) detection was optimized for imaging cerebral glucose metabolism by mapping the fluorine LEXRF signal of 19F in 19FDG, trapped as intracellular 19F-deoxyglucose-6-phosphate (19FDG-6P) at 1μm spatial resolution from 3μm thick brain slices. 19FDG metabolism was evaluated in brain structures closely resembling the general cerebral cytoarchitecture following formalin fixation of brain slices and their inclusion in an epon matrix. 2-dimensional distribution maps of 19FDG-6P were placed in a cytoarchitectural and morphological context by simultaneous LEXRF mapping of N and O, and scanning transmission x-ray (STXM) imaging. A disproportionately high uptake and metabolism of glucose was found in neuropil relative to intracellular domains of the cell body of hypothalamic neurons, showing directly that neurons, like glial cells, also metabolize glucose. As 19F-deoxyglucose-6P is structurally identical to 18F-deoxyglucose-6P, LEXRF of subcellular 19F provides a link to in vivo 18FDG PET, forming a novel basis for understanding the physiological mechanisms underlying the 18FDG PET image, and the contribution of neurons and glia to the PET signal.	Oct 2013
	Interaction of magnetic nanoparticles with U87MG cells studied by synchrotron radiation X-ray fluorescence techniques A. Gianoncelli , P. Marmorato , J. Ponti , L. Pascolo , B. Kaulich , C. Uboldi , F. Rossi , D. Makovec , M. Kiskinova , Giacomo Ceccone X-Ray Spectrometry 42 (4), 316 - 320 European Conference on X-Ray Spectrometry (2012) DOI: 10.1002/xrs.2475 Show Abstract ▼ Abstract: Synchrotron radiation (SR) X-ray microscopy combined with X-ray fluorescence (XRF) microspectroscopy provides unique information that have pushed the frontiers of biological research, particularly when investigating intracellular mechanisms. This work reports an SR-XRF microspectroscopy investigation on the distribution and the potential toxicity of Fe2O3 and CoFe2O4 nanoparticles (NPs) in U87MG glioblastoma-astrocytoma cells. The U87MG cells exposed to NPs concentrations ranging from 5 to 250 µg/ml for 24 h were analyzed in order to monitor both morphological and chemical changes. The SR-XRF maps complemented with XRM absorption and phase contrast images have revealed different intracellular distribution patterns for the two nanoparticles types allowing different mechanism of toxicity to be deduced	Jul 2013

Publications Database

Search Results

You searched for all publications:

Search Again...

Subject Areas (check all that apply) select all

Instruments used to collect data (check all that apply) select all

Collaborations involved (check all that apply) select all

Diamond Offline Facilities used

Relevant Technical Areas (check all that apply) select all

Menu for Anonymous User