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XAS and micro-XRF analysis of mono and bi-metallic exopolysaccharide (FePd-EPS) bio-generated by K. oxytoca
Franco Baldi, Katarina Vogel-Mikuš, Michele Gallo, Oreste Piccolo, Stefano Paganelli, Iztok Arčon, 2016, objavljeni povzetek znanstvenega prispevka na konferenci

Opis: Bacteria Klebsiella oxytoca (DSM 29614) secret a specific exopolysaccharide (EPS) in the presence of Fe(III)-citrate, as sole carbon and energy source, and produces after 7 days an iron gel precipitate (Fe-EPS) [1]. In the presence of palladium or other metal species, the culture of K. oxytoca can produce other mono or bimetal species (Pd-EPS, FePd-EPS) [2]. These bio-materials may be used as green biogenerated catalysts or for other biotechnological purposes. In this work we present the analysis of the morphology and the chemical state of the metals in mono and bi-metallic (Fe-EPS, Pd-EPS, FePd-EPS) complexes, by a combination of micro X-ray fluorescence, X-ray absorption spectroscopy methods (XANES and EXAFS), and transmission electron microscopy. The results show that iron in monometallic Fe-EPS and bimetalic FePd-EPS is in the mineralized form of iron oxides/hydroxides, predominantly in the form of Fe3+, with a small amount of Fe2+ in the structure, as a mixture of different nano-crystalline iron oxides and hydroxides. Palladium on the other hand is found as Pd(0) in the form of metallic nanoparticles with fcc structure in both, bi-metallic (FePd-EPS) and mono-metallic (Pd-EPS) species. In bi-metallic species Pd and Fe nanoparticles agglomerate in larger clusters, but they remain spatially separated. Access to the SR facilities at ESRF (beamline ID21, project LS-2225), DESY (beamline C) Hamburg (project I-20110511 EC) and ELETTRA (beamline XAFS, project 20115112) is acknowledged.
Najdeno v: osebi
Ključne besede: Klebsiella oxytoca, Fe, Pd, XANES, EXAFS, exopolysaccharide, FePd-EPS
Objavljeno: 28.06.2016; Ogledov: 2611; Prenosov: 0
.pdf Polno besedilo (388,27 KB)

Study of Li-S batteries by S K-edge RIXS spectroscopy
Robert Dominko, Iztok Arčon, Marko Petrič, Klemen Bučar, Matjaž Žitnik, Matjaž Kavčič, Alen Vižintin, 2016, objavljeni povzetek znanstvenega prispevka na konferenci

Opis: 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.
Najdeno v: osebi
Ključne besede: RIXS, RXES, Li-S battery, operando, Sulphur K-edge XANES, Lithium polysulphides, Li2S
Objavljeno: 28.06.2016; Ogledov: 2630; Prenosov: 0
.pdf Polno besedilo (60,50 KB)

Correlations between photocatalytic activity and chemical structure in copper doped TiO2-SiO2 with surface/incorporated Cu2+ sites
Tihana Čižmar, Iztok Arčon, Urška Lavrenčič Štangar, 2016, objavljeni povzetek znanstvenega prispevka na konferenci

Opis: Sol−gel method was used to synthesize copper doped TiO2-SiO2 with varied dopant concentrations using tetraisopropoxide (TTIP) and copper acetlyacetonate (CuAcAc) as titania and copper sources. Structural information of Cu cation incorporation and its chemical state in the coatings are determined with Cu K-edge EXAFS and XANES analysis. The correlations between chemical state of the Cu dopant and the photocatalytic properties of the new active coatings are discussed.
Najdeno v: osebi
Ključne besede: dip-coating, titanium dioxide, metal doping, Cu K-edge XANES, photocatalytic activity
Objavljeno: 07.07.2016; Ogledov: 2240; Prenosov: 0

Photocatalytic Activity of Zirconium- and Manganese- Codoped Titania in Aqueous Media: The Role of the Metal Dopant and its Incorporation Site
Nataša Novak Tušar, Iztok Arčon, O. L. Pliekhov, Urška Lavrenčič Štangar, 2016, izvirni znanstveni članek

Opis: The development of efficient TiO2-based photocatalysts for water treatment is mainly performed by doping with transition metals or by establishing junctions between different phases, metal–semiconductor or semiconductor–semiconductor. We present, for the first time, the synthesis of Zr- and Mn-modified TiO2 by a redesigned sol–gel technique that allows the formation of heterometallic bridges on the TiO2 surface. Cations of the doping metals are located in the pores of mesoporous anatase and attached to the crystalline TiO2 walls. The presence of the Zr enhances the photoactivity of the TiO2 catalyst. However, the introduction of Mn decreases the photocatalytic efficiency in a nonadditive manner. The inhibition effect was assigned to the side reaction between hydroxyl radicals and Mn ions. The fact that Mn effectively scavenges the hydroxyl radicals and, consequently, inhibits the whole oxidation process is direct proof that hydroxyl radicals are the main reactive species in the photocatalytic oxidative processes on TiO2 surfaces in aqueous media and the process of COH generation is the rate-determining step, which was confirmed using a method based on the decolorization of a commercial dye Bezaktiv Blau in a reaction with Fenton’s reagent as a source of hydroxyl radicals.
Najdeno v: osebi
Ključne besede: doping, manganese, oxidation, X-ray absorption spectroscopy, zirconium
Objavljeno: 21.07.2016; Ogledov: 1411; Prenosov: 0
.pdf Polno besedilo (577,49 KB)

Arbuscular mycorrhizal fungi alter Hg root uptake and ligand environment as studied by X-ray absorption fine structure
Alojz Kodre, Iztok Arčon, Marta Debeljak, Mateja Potisek, Matevž Likar, Katarina Vogel-Mikuš, 2017, izvirni znanstveni članek

Opis: Mercury (Hg) – plant – fungal interactions are only poorly studied. Hg speciation and ligand environment in maize roots inoculated with arbuscular mycorrhizal (AM) fungi were investigated in order to better understand the role of AM in Hg soil to root transfer. The maize plants were grown in Hg polluted substrate (50 mg g1 as dissolved HgCl2) and inoculated with AM fungi originating from: a) highly Hg polluted environment of a former Hg smelting site in Idrija, Slovenia, (Glomus sp. – sample AmI), and b) non-polluted environment (commercial AM inoculum Symbivit1 – sample AmC). Hg speciation and ligand environment in maize roots was studied by Hg-L3 XANES and EXAFS with emphasis on XAS methodology – modelling and fitting the XAFS spectra to extract in a reliable way as much information on Hg coordination as possible. The AmI plants developed more arbuscules and less vesicles than the AmC plants, and also accumulated more Hg in the roots. A clear difference in Hg coordination between the AM (AmC & AmI) and the control (ConC & ConI) plants is recognized in Hg L3-edge EXAFS analysis: in the ConC & ConI maize roots 73–80% of Hg is attached between two sulphur atoms at the distance of 2.34 Å. The remaining ligand is nitrogen at 2.04 Å. In AmI & AmC roots another Hg-S attachment encompassing four thiol groups at the S-distance of 2.50 Å are identified, accounting for 21–26%. AM fungi can modify Hg ligand environment in plant roots, thus playing an important role in biogeochemical cycling of Hg in terrestrial ecosystems.
Najdeno v: osebi
Ključne besede: EXAFS XANES Arbuscular mycorrhiza Phytoremediation Toxicity Hg coordination Ligand environment
Objavljeno: 27.09.2016; Ogledov: 2530; Prenosov: 0
.pdf Polno besedilo (1,82 MB)

Atomically resolved dealloying of structurally ordered Pt nanoalloy as an oxygen reduction reaction electrocatalyst
Andraž Pavlišič, Primož Jovanovič, Vid Simon Šelih, Martin Šala, Marjan Bele, Goran Dražić, Iztok Arčon, Samo B. Hočevar, Anton Kokalj, Nejc Hodnik, Miran Gaberšček, izvirni znanstveni članek

Opis: The positive effect of intermetallic ordering of platinum alloy nanoparticles on oxygen reduction reaction (ORR) activity has been well established. What is still missing is an understanding of selective leaching of the less noble metal from the ordered structure and its correlation to longterm ORR performance. Using a combination of kinetic Monte Carlo simulations and advanced characterization techniques, we provide unprecedented insight into dealloying of intermetallic PtCu3 nanoparticles a well-known binary alloy. Comparison of ordered and disordered samples with identical initial compositions and particle size distributions reveals an unexpected correlation: whereas the copper dealloying rates in the ordered and disordered counterparts are almost the same, in the ordered structure Pt atoms are surrounded by 15−30% more Cu atoms throughout all the stages of acid leaching. This more convenient Pt−Cu coordination explains the statistically significant increase of 23−37% in ORR activity of the ordered structure at all stages of alloy degradation.
Najdeno v: osebi
Ključne besede: ORR activity, fuel cells, platinum alloy, nanoparticle stability, intermetallic ordering, kinetic Monte Carlo, dealloying, in situ ICP-MS
Objavljeno: 27.09.2016; Ogledov: 2046; Prenosov: 0
.pdf Polno besedilo (3,27 MB)

Donor doping of K0.5Na0.5NbO3 ceramics with strontium and its implications to grain size, phase composition and crystal structure
Jitka Hreščak, Goran Dražić, Marco Deluca, Iztok Arčon, Alojz Kodre, M. Dapiaggi, Tadej Rojac, Barbara Malič, Andreja Benčan, 2017, izvirni znanstveni članek

Opis: In this study, the particular effects of A-site donor doping in a lead-free piezoceramic material K0.5Na0.5NbO3 (KNN) doped with Sr2+, i.e., the crystal-structure change, the secondary-phase formation and the grain-size decrease, were investigated. The already-reported causes of these effects upon doping KNN were critically discussed and a mechanism of the effects’ formation was suggested and experimentally supported with advanced analytical methods. Extended X-ray absorption fine structure (EXAFS) analyses proved that the Sr occupies the perovskite A-sublattice, and locally modifies the KNN monoclinic structure to cubic. With the help of Sr K-edge EXAFS and wavelength-dispersive X-ray spectroscopy, the Sr was found to be homogenously distributed in the KNN perovskite lattice with 0.5, 1 and 2% Sr and no Sr segregation on the nano level was found in any of the studied samples with transmission electron microscopy. Introducing Sr into the A-sublattice, as well as accounting for the charge-compensating A-site vacancies in the starting composition, causes increasing lattice disorder and microstrain, as determined from a Rietveld refinement of the synchrotron X-ray diffraction data. Above 2% Sr the system segregates the A-site vacancies in a secondary phase in order to release the chemical pressure, as revealed by Raman spectroscopy. All these effects result in an increasing number of low-angle grain boundaries that limit the grain growth and finally lead to a significant grain-size decrease.
Najdeno v: osebi
Ključne besede: perovskite, potassium sodium niobate, donor doping, cation vacancies
Objavljeno: 17.01.2017; Ogledov: 1885; Prenosov: 186
.pdf Polno besedilo (2,11 MB)

Correlations between photocatalytic activity and chemical structure of Cu-modified TiO2–SiO2 nanoparticle composites
Iztok Arčon, Urška Lavrenčič Štangar, T. Čižmar, 2016, izvirni znanstveni članek

Opis: Copper-modified TiO2–SiO2photocatalysts were prepared by sol–gel method based on organic copper,silicon and titanium precursors. Copper concentration varied from 0.1 to 3.0 mol%. A widely appliedmodel reaction of photocatalytic oxidation of terephtalic acid (TPA) in water solution was used in order toevaluate the catalytic activities of elaborated samples. The crystal structures of the titania components ofall tested titania–silica species were studied using XRD analysis. The influence of Cu2+cation incorporationon the crystal structure of titania, as well as the chemical states and the neighbouring structures of coppercations, have been examined by means of Cu K-edge EXAFS and XANES analysis. The experimental datashow that there is a ten times increase in photocatalytic activity when TiO2–SiO2matrix is modified with0.1 mol% of Cu. It can be supposed that an enhancement of photocatalytic activity of low-concentratedcopper-modified titania–silica nanocomposites is probably due to a close attachment of Cu2+cationsto the surfaces of photocatalytically active TiO2nanoparticles. In this case, Cu2+cations may possiblyact as free electron traps reducing the intensity of recombination between opposite free charge carriers(electrons, holes) available at the photocatalyst’s surface.
Najdeno v: osebi
Ključne besede: Cu-modified TiO2–SiO2photocatalysts, Titanium dioxide, Metal doping, Cu K-edge XANES, EXAFS, Photocatalytic activitya
Objavljeno: 17.01.2017; Ogledov: 2063; Prenosov: 0
.pdf Polno besedilo (580,62 KB)

Correlations between photocatalytic activity and chemical structure of Cu-modified TiO [sub] 2-SiO [sub] 2 nanoparticle composites
T. Čižmar, Iztok Arčon, Urška Lavrenčič Štangar, 2016, objavljeni povzetek znanstvenega prispevka na konferenci

Najdeno v: osebi
Ključne besede: Cu-modified TiO2-SiO2, sol-gel, XANES, EXAFS
Objavljeno: 06.02.2017; Ogledov: 1420; Prenosov: 0
.pdf Polno besedilo (378,67 KB)

Operando characterization of batteries using x-ray absorption spectroscopy: advances at the beamline XAFS at synchrotron Elettra
Nicola Novello, Iztok Arčon, Lorenzo Stievano, Robert Dominko, marco Giorgetti, Giuliana Aquilanti, Luca Ivanc Olivieri, 2017, izvirni znanstveni članek

Opis: 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.
Najdeno v: osebi
Ključne besede: operando studies, x-ray absorption spectroscopy, Li-ion batteries, Li-S batteries
Objavljeno: 03.03.2017; Ogledov: 3049; Prenosov: 0
.pdf Polno besedilo (1,59 MB)

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