Upscaling the urea method synthesis of CoAl layered double hydroxides

• Camilo Jaramillo-Hernández,
• Víctor Oestreicher,
• Martín Mizrahi and
• Gonzalo Abellán

Beilstein J. Nanotechnol. 2023, 14, 927–938, doi:10.3762/bjnano.14.76

• spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the

• process and aiming to quantify the amount of this Co-based α-LH impurity, X-ray absorption spectroscopy (XAS) measurements were performed at the CLÆSS BL22 beamline at the ALBA synchrotron. Figure 2A depicts the X-ray absorption near-edge structure (XANES) spectra for the Co K edge. In all samples, the

• combination of CoAl-LDH and α-CoII LH reference spectra. Figure 2B depicts the result of the fits, where excellent agreement is achieved using 57% of LDH and 43% of α-CoII LH. This analysis is an excellent example to show that XANES is a useful technique for LH structure quantification. A detailed description

Theoretical investigations of oxygen vacancy effects in nickel-doped zirconia from ab initio XANES spectroscopy at the oxygen K-edge

• Dick Hartmann Douma,
• Lodvert Tchibota Poaty,
• Alessio Lamperti,
• Stéphane Kenmoe,
• Abdulrafiu Tunde Raji,
• Alberto Debernardi and
• Bernard M’Passi-Mabiala

Beilstein J. Nanotechnol. 2022, 13, 975–985, doi:10.3762/bjnano.13.85

• Nanotechnologies, Institut National de Recherche en Sciences Exactes et Naturelles (IRSEN), Brazzaville, Congo 10.3762/bjnano.13.85 Abstract In this study, we present theoretical X-ray absorption near-edge structure (XANES) spectra at the K-edge of oxygen in zirconia containing Ni dopant atoms and O vacancies at

• vacancies. In this system, each Ni atom is surrounded by two shells of O with tetrahedral geometry, in a similar way as in bulk cubic zirconia. The oxygen K-edge XANES spectrum of this configuration shows a pre-edge peak, which is attributable to dipole transitions from O 1s to O 2p states that are

• one remains in a tetrahedral geometry. Furthermore, the introduction of two vacancies in the 2Ni-doped zirconia results in the two Ni atoms having distorted octahedral and trigonal bipyramidal geometries and being coupled antiferromagnetically in the ground state. Additionally, the oxygen K-edge XANES

Comparison of fresh and aged lithium iron phosphate cathodes using a tailored electrochemical strain microscopy technique

• Matthias Simolka,
• Hanno Kaess and
• Kaspar Andreas Friedrich

Beilstein J. Nanotechnol. 2020, 11, 583–596, doi:10.3762/bjnano.11.46

• (FIB) SEM and X-ray absorption near edge structure (XANES) [6][7][8][9][10][11][12][13]. Another technique for post-mortem analysis is atomic force microscopy (AFM). In its basic form, it provides information on the topography of the sample. More advanced AFM modes extract in addition to the topography

The influence of porosity on nanoparticle formation in hierarchical aluminophosphates

• Matthew E. Potter,
• Lauren N. Riley,
• Alice E. Oakley,
• Panashe M. Mhembere,
• June Callison and
• Robert Raja

Beilstein J. Nanotechnol. 2019, 10, 1952–1957, doi:10.3762/bjnano.10.191

• observed (Figure 3 and Figures S10–S15, Supporting Information File 1). There was good agreement with the Au foil, suggesting the gold has been successfully reduced to metallic gold particles. The Au/MP-SAPO-5 systems show a lower-energy X-ray absorption near edge structure (XANES), suggesting a higher

• required additional Au1 features to be accurately fit, in agreement with the Auδ+ species observed from XANES (Figure 4A). As XPS has a limited penetration depth, it will accentuate surface species, which are more likely to contain Au1 species, over the bulk [22]. In both cases the weak signal from the low

Gas sensing properties of individual SnO₂ nanowires and SnO₂ sol–gel nanocomposites

• Alexey V. Shaposhnik,
• Dmitry A. Shaposhnik,
• Sergey Yu. Turishchev,
• Olga A. Chuvenkova,
• Stanislav V. Ryabtsev,
• Alexey A. Vasiliev,
• Xavier Vilanova,
• Francisco Hernandez-Ramirez and
• Joan R. Morante

Beilstein J. Nanotechnol. 2019, 10, 1380–1390, doi:10.3762/bjnano.10.136

• ; gas transport method; nanowires; quasi-one-dimensional materials; sol–gel synthesis; tin dioxide; X-ray absorption near edge structure (XANES); X-ray photoelectron spectroscopy (XPS); Introduction Semiconductor sensor functionality relies on heterogeneous catalytic chemical processes, which makes the

• near edge structure (XANES), both employing the high-brilliance synchrotron radiation of the BESSY II storage ring at the Helmholtz Zentrum Berlin on the joint Russian–German beamline. The efficiency of XPS and XANES has previously been demonstrated in investigations of local atomic surroundings

• as a reference. The application of synchrotron radiation allowed the variation of X-ray quantum energies for the excitation of XANES spectra. These spectra represent local partial densities of free electronic states in the conduction band of the investigated materials [35][36][37][38][39][40][41

Integration of LaMnO_3+δ films on platinized silicon substrates for resistive switching applications by PI-MOCVD

• Raquel Rodriguez-Lamas,
• Dolors Pla,
• Odette Chaix-Pluchery,
• Benjamin Meunier,
• Fabrice Wilhelm,
• Andrei Rogalev,
• Laetitia Rapenne,
• Xavier Mescot,
• Quentin Rafhay,
• Hervé Roussel,
• Michel Boudard,
• Carmen Jiménez and
• Mónica Burriel

Beilstein J. Nanotechnol. 2019, 10, 389–398, doi:10.3762/bjnano.10.38

• nanostructure growth was further analyzed in cross section by transmission electron microscopy (TEM), a JEOL 2011 equipment operating at 200 kV with a 0.19 nm point-to-point resolution. X-ray absorption near-edge spectroscopy (XANES) spectra at the Mn K-edge of LMO thin films were collected at the ESRF ID12

• incident beam. The relative variation in the Mn formal valence was carried out from the experimental recorded inflection point after XANES spectra normalization, and using references found in the literature for other manganite perovskites [28]. The device fabrication for electrical measurements was

• a mixed valence state of the manganese cation (Mn3+/Mn4+). The variation of the Mn oxidation state for the same series of LMO films measured by Raman was confirmed by XANES (Figure 7). The local geometry of Mn was extracted from the pre-edge feature. For all the spectra, the absence of a sharp pre

Structural properties and thermal stability of cobalt- and chromium-doped α-MnO₂ nanorods

• Romana Cerc Korošec,
• Polona Umek,
• Alexandre Gloter,
• Jana Padežnik Gomilšek and
• Peter Bukovec

Beilstein J. Nanotechnol. 2017, 8, 1032–1042, doi:10.3762/bjnano.8.104

• that the content of the dopant ions decreases with increasing reaction temperature. The oxidation of Co2+ to Co3+ during the reaction was proved by an XANES study, while EXAFS results confirm that both dopant ions substitute Mn4+ in the center of an octahedron. The K/Mn ratio in the doped samples

• that of the undoped ones. Dopant ions do not preserve the MnO2 phase at higher temperatures nor do they destabilize the cryptomelane structure. Keywords: α-MnO2; doping; EXAFS; nanorods; XANES; Introduction The wide range of physical and chemical properties of manganese dioxide (MnO2), which exists

• with an energy dispersive X-ray spectrometer (SEM–EDS). Obtained results were correlated with XAFS and XANES (X-ray absorption fine structure; X-ray absorption near-edge structure) analysis, which helps to determine the position of dopant ions in the cryptomelane structure, as well as the oxidation

Microwave synthesis of high-quality and uniform 4 nm ZnFe₂O₄ nanocrystals for application in energy storage and nanomagnetics

• Christian Suchomski,
• Ben Breitung,
• Ralf Witte,
• Michael Knapp,
• Sondes Bauer,
• Tilo Baumbach,
• Christian Reitz and
• Torsten Brezesinski

Beilstein J. Nanotechnol. 2016, 7, 1350–1360, doi:10.3762/bjnano.7.126

• based on a least-squares linear combination of reference spectra and was carried out by use of TXM-XANES Wizard after normalization [26]. The quality of fits was assessed by the misfit factor, R. Results and Discussion Highly crystalline ZFO nanoparticles were prepared by microwave-assisted nonaqueous

• further insight into both the electrochemical reactions of ZFO with Li and the oxidation state of Fe, combined full-field transmission X-ray microscopy (TXM) and X-ray absorption near edge structure (XANES) spectroscopy was conducted on “pristine” and pre-cycled nanoparticle electrodes at the NANO

• beamline at the ANKA Synchrotron Radiation Facility and the preliminary data are shown in Figure 10 [25]. For these measurements, Li half-cells were disassembled inside an argon-filled glovebox and the obtained electrodes sealed using Kapton tape to maintain airtight conditions. Since XANES imaging is

From lithium to sodium: cell chemistry of room temperature sodium–air and sodium–sulfur batteries

• Philipp Adelhelm,
• Pascal Hartmann,
• Conrad L. Bender,
• Martin Busche,
• Christine Eufinger and
• Juergen Janek

Beilstein J. Nanotechnol. 2015, 6, 1016–1055, doi:10.3762/bjnano.6.105

Overview about the localization of nanoparticles in tissue and cellular context by different imaging techniques

• Anja Ostrowski,
• Daniel Nordmeyer,
• Alexander Boreham,
• Cornelia Holzhausen,
• Lars Mundhenk,
• Christina Graf,
• Martina C. Meinke,
• Annika Vogt,
• Sabrina Hadam,
• Jürgen Lademann,
• Eckart Rühl,
• Ulrike Alexiev and
• Achim D. Gruber

Beilstein J. Nanotechnol. 2015, 6, 263–280, doi:10.3762/bjnano.6.25

• local distribution of zinc in the cells and micro-X-ray absorption near-edge structure (XANES) spectroscopy allowed for the identification of different zinc species present in the sample [144]. Others used STXM and compact source transmission X-ray microscopy for subcellular imaging of vascular smooth

Materials and characterization techniques for high-temperature polymer electrolyte membrane fuel cells

• Roswitha Zeis

Beilstein J. Nanotechnol. 2015, 6, 68–83, doi:10.3762/bjnano.6.8

• examining the X-ray near edge structure (XANES). For these analyses, the XANES measurements were taken from −20 to 50 eV relative to the Pt L3 edge at 11.564 eV. The Pt L3 absorption edge from a platinum foil was used as a reference. The Δμ signals were generated by using the subtractive method Δμ = μsample

• (XANES). They also applied the Δμ technique. The difference is that the measurements were carried out at room temperature while using perchloric acid as the base electrolyte with added small concentrations of phosphoric acid. Commercial carbon-supported Pt and Pt/Ni nanoparticle catalysts were used in

• experiments was found at a lower potential. Above 400 mV the phosphoric acid adsorption decreases. In their XANES data phosphoric acid is present on the platinum surface at all potentials, but this is not the case at elevated temperatures and higher acid concentrations as reported by Kaserer et al. [63

Artificial sunlight and ultraviolet light induced photo-epoxidation of propylene over V-Ti/MCM-41 photocatalyst

• Van-Huy Nguyen,
• Shawn D. Lin,
• Jeffrey Chi-Sheng Wu and
• Hsunling Bai

Beilstein J. Nanotechnol. 2014, 5, 566–576, doi:10.3762/bjnano.5.67

• distinctive feature of MCM-41. The pore diameters of catalyst estimated from TEM was approximately 3 nm. We previously proposed that the titanium in V-Ti/MCM-41 should be Ti4+ with a tetrahedral coordination [17]. The K-edge XANES of vanadium (Figure 4) suggests its oxidation state to be V5+. A possible local

• (XANES) of the vanadium K-edge was carried out with synchrotron radiation at the beam line 16A, National Synchrotron Radiation Research Center, Taiwan. The standard metal foil and V oxides (V2O5 and V2O3) powders were used as references. High resolution transmission electron microscope (HRTEM) was

• references by XANES and proposed structures of V-Ti/MCM-41 (inset). Time course of the photo-epoxidation of propylene with molecular oxygen under UV–visible light irradiation (without an AM1.5G filter; 18.5 mW·cm−2): (a) C3H6 consumption rate and PO formation rate, (b) Selectivity to products. Lines are

Extended X-ray absorption fine structure of bimetallic nanoparticles

• Carolin Antoniak

Beilstein J. Nanotechnol. 2011, 2, 237–251, doi:10.3762/bjnano.2.28

• structure (XANES). In the energy range above the XANES region – typically from 100 eV to 1000 eV above the absorption edge – the extended X-ray absorption fine structure (EXAFS) contains information about the type and distance of atoms in the local environment of the absorbing atom. In the literature

• is organised as follows: In the next few subsections, the basics of XANES and EXAFS are shortly summarised. The second section focuses on the EXAFS analysis either on the basis of standard Fourier transform (FT) methods or by using a wavelet transform (WT). As an example, recent results on FePt

• structure (XANES) The XANES includes information about the density of states (DOS) of the absorbing atoms. More precisely, the XANES is connected to the unoccupied electronic DOS of the excited atom in the presence of a core-hole. In this section, the description of the XANES by the standard one-electron

Zirconium nanoparticles prepared by the reduction of zirconium oxide using the RAPET method

• Michal Eshed,
• Swati Pol,
• Aharon Gedanken and
• Mahalingam Balasubramanian

Beilstein J. Nanotechnol. 2011, 2, 198–203, doi:10.3762/bjnano.2.23

• employed to confirm the formation of metallic Zr synthesized (Zr-syn) by RAPET of ZrO2. The techniques of XAS, namely X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), are used to probe local structural details [13] around specific metal atoms and to discern

• the oxidation states of the metal, here the zirconium atom. The Zr K-edge XAS of Zr-syn is compared with the standards, ZrO2 (also used as a starting material) and metallic hexagonal close packed (hcp) Zr as shown in Figure 2. The normalized XANES spectrum (Figure 2a) shows a comparison of the

• starting ZrO2 material and Zr-syn with the metallic hcp Zr standard. The general appearance of the XANES of starting material is very similar to the spectra reported [14] by Li et al. for the monoclinic polymorph of ZrO2. This observation confirms that the monoclinic phase is the major component in the

Ultrafine metallic Fe nanoparticles: synthesis, structure and magnetism

• Olivier Margeat,
• Marc Respaud,
• Catherine Amiens,
• Pierre Lecante and
• Bruno Chaudret

Beilstein J. Nanotechnol. 2010, 1, 108–118, doi:10.3762/bjnano.1.13

• synthesis of well-isolated Fe NPs embedded in a polymer, with diameters of less than 2 nm. The structural and chemical properties have been investigated by transmission electron microscopy, wide angle X-ray scattering (WAXS), and X-ray absorption near-edge structure (XANES). Preliminary results of this work

• oxidation. The particles were characterized by transmission electron microscopy (TEM), wide angle X-ray scattering (WAXS) [22], and X-ray absorption near-edge structure (XANES). TEM micrographs show the presence of well-dispersed small particles of ca. 1.8 nm mean size with a narrow size distribution (15

• ., lower than that of bulk iron. XANES and EXAFS are other powerful tools for the study of short range order [29]. We therefore carried out these measurements at the iron K-edge at room temperature. Figure 3 shows the data obtained for the iron NPs and an iron foil used as a reference, and the first