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1.
Monitoring chemical processes in (photo)catalysts and energy storage materials by operando X-ray absorption spectroscopy
Iztok Arčon, 2022, published scientific conference contribution abstract (invited lecture)

Abstract: X-ray absorption spectroscopy (XAS) is a powerful tool for characterisation of local structure and chemical state of selected elements in different new functional materials and biological or environmental samples. The XAS spectroscopy is based on extremely bright synchrotron radiation X-rays sources, which allow precise characterisation of bulk, nanostructured or highly diluted samples. The rapid development of extremely bright synchrotron sources of X-ray and ultraviolet light in recent years has opened new possibilities for research of matter at the atomic or molecular level, indispensable in the development of new functional nanostructured materials with desired properties. The talk will present the possibilities offered by X-ray absorption spectroscopy with synchrotron light for ex-situ or operando characterization of various functional porous and other nanomaterials, before, after and during their operation [1,2,3,4]. New generation of synchrotron light sources also opened the possibility of combining X-ray absorption with high-resolution emission [5] and inelastic scattering spectroscopy [6], and microscopy with sub-micron resolution [7]. Examples of operando XANES and EXAFS analysis to track changes in the valence states and local structures of selected elements in different energy storage materials and in various (photo)catalysts, during chemical reactions under controlled reaction conditions, will be presented, which provided insight into the dynamic functional properties and reaction mechanisms of these materials. Access to SR facilities of Petra III (beamlines P65, P64 and P01), ESRF (beamlines BM23, ID21, ID26) and Elettra (beamlines XAFS, XRF), for the presented research is kindly acknowledged.
Keywords: X-ray absorption spectroscopy, operando XANES, EXAFS, catalysts, batteries
Published in RUNG: 07.10.2022; Views: 998; Downloads: 0
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2.
Monitoring chemical processes on the atomic scale in catalysts by operando X-ray absorption spectrometry
Iztok Arčon, 2022, published scientific conference contribution abstract (invited lecture)

Abstract: X-ray absorption spectroscopy (XAS) is a powerful tool for characterisation of local structure and chemical state of selected elements in different new functional materials and biological or environmental samples. The rapid development of extremely bright synchrotron sources of X-ray and ultraviolet light in recent years has opened new possibilities for research of matter at the atomic or molecular level, indispensable in the development of new functional nanostructured materials with desired properties. The lecture will present the possibilities offered by X-ray absorption spectroscopy with synchrotron light for ex-situ and in-situ or operando characterization of various catalyst materials before, after and during their operation. With the operando XANES and EXAFS methods it is possible to track changes in the valence states and local structures of selected elements in various (photo)catalysts, during chemical reactions under controlled reaction conditions, thus gaining insight into the dynamic functional properties and reaction mechanisms of these materials. New synchrotron light sources also opened the possibility of combining X-ray absorption or emission spectroscopy and microscopy with a resolution of up to a few tens of nanometres, allowing micro-XAS analysis with high spatial resolution.
Keywords: XAS, operando XANES, EXAFS, catalysts
Published in RUNG: 01.06.2022; Views: 1305; Downloads: 0
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3.
Monitoring of chemical processes at the atomic level by X-ray absorption spectrometry using extremely bright synchrotron radiation sources
Iztok Arčon, invited lecture at foreign university

Abstract: X-ray absorption spectroscopy (XAS) is a powerful tool for characterisation of local structure and chemical state of selected elements in different new functional materials and biological or environmental samples. The XAS spectroscopy is based on extremely bright synchrotron radiation X-rays sources, which allow precise characterisation of bulk, nanostructured or highly diluted samples. The rapid development of extremely bright synchrotron sources of X-ray and ultraviolet light in recent years has opened new possibilities for research of matter at the atomic or molecular level, indispensable in the development of new functional nanostructured materials with desired properties. The lecture will present the possibilities offered by X-ray absorption spectroscopy with synchrotron light for ex-situ and in-situ or operando characterization of various functional porous and other nanomaterials before, after and during their operation.
Keywords: XAS, operando XANES, EXAFS, functional materials
Published in RUNG: 01.06.2022; Views: 1238; Downloads: 0
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4.
Monitoring of chemical processes at the atomic level by X-ray absorption spectrometry using extremely bright synchrotron radiation sources
Iztok Arčon, unpublished invited conference lecture

Abstract: X-ray absorption spectroscopy (XAS) is a powerful tool for characterisation of local structure and chemical state of selected elements in different new functional materials and biological or environmental samples. The XAS spectroscopy is based on extremely bright synchrotron radiation X-rays sources, which allow precise characterisation of bulk, nanostructured or highly diluted samples. The rapid development of extremely bright synchrotron sources of X-ray and ultraviolet light in recent years has opened new possibilities for research of matter at the atomic or molecular level, indispensable in the development of new functional nanostructured materials with desired properties. The lecture will present the possibilities offered by X-ray absorption spectroscopy with synchrotron light for ex-situ and in-situ or operando characterization of various functional porous and other nanomaterials before, after and during their operation. With the operando micro-XANES and EXAFS methods it is possible to track changes in the valence states and local structures of selected elements in different energy storage materials or in various (photo)catalysts, during chemical reactions under controlled reaction conditions, thus gaining insight into the dynamic functional properties and reaction mechanisms of these materials. New synchrotron light sources also opened the possibility of combining X-ray absorption or emission spectroscopy and microscopy with a resolution of up to a few tens of nanometres, crucial for analysis of environmental and biological samples on sub-cellular level, to understand the mechanisms of uptake, transport, accumulation, and complexation of metal cations on subcellular level in various plant tissues or accumulation in environment, to develop effective remediation approaches.
Keywords: X-ray absorption spectroscopy, EXAFS, XANES, synchrotron radiation sources, operando
Published in RUNG: 15.12.2021; Views: 1701; Downloads: 0
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5.
Spremljanje kemijskih procesov na atomskem nivoju v živo z rentgensko absorpcijsko spektrometrijo
Iztok Arčon, 2021, published scientific conference contribution abstract

Abstract: Skokovit razvoj izjemno svetlih sinhrotronskih virov rentgenske in ultravijolične svetlobe v zadnjih letih je odprl nove možnosti za raziskave snovi na atomskem oziroma molekularnem nivoju, brez katerih si ne moremo predstavljati razvoja in sinteze novih funkcionalnih nanostrukturnih materialov z želenimi lastnostmi. V predavanju bodo predstavljene možnosti, ki jih nudi rentgenska absorpcijska spektroskopija s sinhrotronsko svetlobo pri karakterizacij različnih funkcionalnih nano-materialov v živo med njihovim delovanjem. Z metodama operando mikro-XANES in EXAFS lahko sledimo spremembam valenčnih stanj in lokalnih struktur izbranih elementov npr. v materialih za shranjevanje energije ali v različnih (foto)katalizatorjih, med kemičnimi reakcijami pri nadzorovanih reakcijskih pogojih, s čimer dobimo vpogled v dinamične funkcionalne lastnosti in mehanizme delovanja teh materialov. Novi sinhrotronski viri svetlobe odpirajo tudi možnosti kombinacije rentgenske spektroskopije in mikroskopije z ločljivostjo do nekaj deset nanometrov, s čimer lahko ključno prispevajo tudi k razumevanju mehanizmov zajemanja, transporta, akumulacije in kompleksacije kovinskih kationov na sub-celičnem nivoju v različnih tkivih rastlin, ki te polutante (hiper)akumulirajo in jih s tem prenašajo v prehranjevalno verigo.
Keywords: rentgenska absorpcijska spektroskopija, operando XAS, strukturna analiza materialov
Published in RUNG: 03.06.2021; Views: 1908; Downloads: 54
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6.
X-ray absorption spectroscopy analysis: in situ, operando, in vivo
Iztok Arčon, 2020, published scientific conference contribution abstract (invited lecture)

Abstract: X-ray absorption spectroscopy (XAS) is a powerful tool for characterisation of local structure and chemical state of selected elements in different new functional materials and biological or environmental samples. The XAS spectroscopy is based on extremely bright synchrotron radiation X-rays sources, which allow precise characterisation of bulk, nanostructured or highly diluted samples. With its two methods (XANES and EXAFS) it enables monitoring changes in valence states and local structures of constituent elements during chemical reactions under controlled reaction conditions, and it offers a possibility of a combination of X-ray spectroscopy and microscopy with sub-micron lateral resolution, crucial for analysis of biological samples on sub-cellular level. In this talk some typical examples of advanced XAS analysis will be presented.
Keywords: X-ray absorption spectroscopy, EXAFS, XANES, in-situ, operando
Published in RUNG: 17.10.2020; Views: 2961; Downloads: 0
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7.
Polysulfides formation in different electrolytes from the perspective of X-ray absorption spectroscopy
Robert Dominko, Alen Vižintin, Giuliana Aquilanti, Lorenzo Stievano, Maria Joseph Helen, Anji Reddy Munnangi, Maximilian Fichtner, Iztok Arčon, 2018, original scientific article

Abstract: Li-S batteries are promising energy storage technology for the future, however there two major problems remained which need to be solved before successful commercialization. Capacity fading due to polysulfide shuttle and corrosion of lithium metal are directly connected with the type and quantity of electrolyte used in the cells. Several recent works show dependence of the electrochemical behavior of Li-S batteries on type of the electrolyte. In this work we compare and discuss a discharge mechanism of sulfur conversion in three different electrolytes based on measurements with sulfur K-edge XAS. The sulfur conversion mechanism in the ether based electrolytes, the most studied type of solvents in the Li-S batteries, which are enabling high solubility of polysulfides are compared with the fluorinated ether based electrolytes with a reduced polysulfide solubility and in carbonate based electrolytes with the sulfur confined into a ultramicroporous carbon. In all three cases the sulfur reduction proceeds through polysulfide intermediate phases with a difference on the type polysulfides detected at different steps of discharge.
Keywords: Li-S batteries, operando sulphur K-edge XANES, EXAFS, Li-polysulphides
Published in RUNG: 01.06.2018; Views: 3486; Downloads: 0
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8.
Operando characterization of batteries using x-ray absorption spectroscopy: advances at the beamline XAFS at synchrotron Elettra
Giuliana Aquilanti, marco Giorgetti, Robert Dominko, Lorenzo Stievano, Iztok Arčon, Nicola Novello, Luca Ivanc Olivieri, 2017, original scientific article

Abstract: X-ray absorption spectroscopy is a synchrotron radiation based technique that is able to provide information on both local structure and electronic properties in a chemically selective manner. It can be used to characterize the dynamic processes that govern the electrochemical energy storage in batteries, and to shed light on the redox chemistry and changes in structure during galvanostatic cycling to design cathode materials with improved properties. Operando XAS studies have been performed at beamline XAFS at Elettra on different systems. For Li-ion batteries, a multiedge approach revealed the role of the different cathode components during the charge and discharge of the battery. In addition, Li-S batteries for automotive applications were studied. Operando sulfur K-edge XANES and EXAFS analysis was used to characterize the redox chemistry of sulfur, and to relate the electrochemical mechanism to its local structure.
Keywords: operando studies, x-ray absorption spectroscopy, Li-ion batteries, Li-S batteries
Published in RUNG: 03.03.2017; Views: 6055; Downloads: 0
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9.
Study of Li-S batteries by S K-edge RIXS spectroscopy
Matjaž Kavčič, Matjaž Žitnik, Klemen Bučar, Marko Petrič, Iztok Arčon, Robert Dominko, Alen Vižintin, 2016, published scientific conference contribution abstract

Abstract: Li-S batteries are considered as one of the most promising candidates for future batteries in applications where high energy density is required [1]. Despite that the general principle of operation is known for a long time [2], the lack of detailed understanding of relevant operation mechanisms has so far prevented their extensive use. A Li-S battery is composed of a lithium metal anode and a sulfur based cathode, separated by a porous separator wetted with electrolyte. During the battery cycle the reduction and oxidation of S to Li2S and back proceeds through a complicated equilibrium mixture of compounds that are typically dissolved in the electrolyte in the form of long and short chain polysulfides. In order to improve our understanding of polysulfide formation and its interactions within electrode, which are essential to achieve the long term cycling stability, development and application of new analytical tools is required. In this work sulfur K-edge resonant X-ray emission (RXES) measurements were performed on the Li-S battery in operando mode. The experiment was performed at the ID26 beamline at ESRF using the Johansson type tender x-ray emission spectrometer [3]. Full K-L RIXS maps were recorded on a set of chemically prepared Li2Sx sample standards characterized by different Li:S stoichiometric ratio, followed by the operando measurements on Li-S battery. Using the spectra recorded on Li2Sx standards two excitation energies were chosen and RXES spectra from the back of the battery cathode were sequentially acquired during one discharge cycle (C20). The relative amounts of each sulfur compound in the cathode during the discharge cycle were determined from the linear combination fit using measured reference standard spectra. Because of resonant excitation conditions the sensitivity for the polysulfide detection was significantly enhanced. Our work sets up S K-edge RIXS spectroscopy as an important analytical tool to study the mechanism of Li-polysulfide formation in the cathode and their interaction with the host matrix and electrolyte.
Keywords: RIXS, RXES, Li-S battery, operando, Sulphur K-edge XANES, Lithium polysulphides, Li2S
Published in RUNG: 28.06.2016; Views: 5560; Downloads: 0
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